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Message from Chairman, ISRS 2008

Dated: 2-12-2008
The ISRS 2008 being held between 10th and 12th December 2008, in Chennai is a well
established conference for research scholars working in the broad areas of the science,
engineering, and technology and is recognized as such by the fraternity associated with Materials
Science and Technology. This conference brings together research scholars from around the
world and offers a great opportunity for the participants to learn from each other’s experience.
Thanks to the efforts of the organizers, ISRS 2008 will provide a platform for showcasing some
of the latest advancements in the field of Materials Science and Technology.

This year’s conference is of special significance being the golden jubilee year of IIT Madras and
that of the Department of Metallurgical and Materials Engineering. I am happy to note that the
institute has recognised this event as one of the Golden Jubilee Events. I am convinced that this
effort by the organizers will greatly assist young researchers for enhanced mutual engagement
and interaction, both social and professional. Such interactions are essential in the modern
context where compartmentalization has proven to be counterproductive and even detrimental to
the overall scientific and technological progress. I am sure with such wide participation and keen
enthusiasm this symposium will turn out to be a memorable one.

I am also particularly happy to note that the organisers have taken care to invite eminent plenary
speakers engaged in different aspects of the broad theme of the conference. Undoubtedly it will
be of great benefit to the participants and will strengthen their understanding of Materials
Science and Technology.

I congratulate the organizers of ISRS 2008 for the enthusiasm with which they have gone about
organizing this conference and wish the conference all success.

(Dr. P.K. Nair)

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ISRS 2008 Patrons
Prof. M S Ananth, Director, IIT Madras
Dr. Baldev Raj, Director, IGCAR
Shri B Muthuraman, Managing Director, TATA Steel
Shri M M Murugappan, Chairman, Carborundum Universal Ltd

ISRS 2008 International Advisory Committee


Prof. K Krishnaiah, IITM
Prof. S Santhakumar, IITM
Prof. V G Idichandy, IITM
Prof. T T Narendran, IITM
Prof. M Singaperumal, IITM
Prof. R Ramamurthi, IITM
Prof. P Kesavan Nair, IITM
Prof. N Chakraborti, IIT Kharagpur
Prof. S K Nath, IIT Roorkee
Prof. Rajiv O Dusane, IIT Bombay
Prof. R Shekhar, IIT Kanpur
Prof. K Chattopadhyay, IISc Bangalore
Prof. S B Abdullah, Universiti Teknologi MARA, Malaysia
Prof. William A. Baeslack III, Ohio State University, USA
Dr. D Banerjee, DRDO
Dr. S Banerjee, BARC
Dr. S Best, University of Cambridge
Dr. K Bhanu Sankara Rao, IGCAR, Kalpakkam
Dr. D Bhattacharjee, TATA Steel, Jamshedpur
Prof. R K Bordia, University of Washington, USA
Prof. T Chandra, University of Wollongong, Australia
Prof. C Dong, Dallan University of Technology, China
Prof. H Hahn, INT, FZK, Germany
Prof. K Hono, NIMS Japan
Prof. H S Kim, Chungnam National University, S. Korea
Prof. D H Kim, University of Yonsel, S. Korea
Prof. H G Lee, POSTECH, S. Korea
Prof. C G Levi, UCSB
Dr. G Malakondaiah, DMRL, Hyderabad
Prof. B Matovic VINS, Serbia
Prof. S P Mehrotra, NML, Jamshedpur
Dr. J Mukhopadhyay, JNARDDC, Nagpur
3URI.0OOHU8QLYHUVLW\RI6WXWWJDUW*HUPDQ\
Prof. K L Murty, NC State University, USA
Dr. J Narayana Das, NMRL, Ambarnath
Prof. K A Padmanabhan, Anna University, Chennai
Prof. S Ramakrishna, NUS, Singapore
Prof. S Ranganathan, IISc Bangalore
Prof. C Ravi Ravindran, Ryerson University, Canada
Prof. P Rodriguez, IITM
Prof. Schneider, Technical University of Darmstadt, Germany
Dr. G Sundararajan, ARCI, Hyderabad
Prof. S Suresh, MIT, USA
Dr. T Webster, Brown University, USA
Prof. P Wollants, Catholic University, Belgium
Prof. Y Zeng, Shangai Institute of Ceramics, China

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ISRS 2008 Local Organising Committee
Chairperson
Prof. P Kesavan Nair, Head, Dept. of MME, IITM
Convener
Dr. Prathap Haridoss, MME, IITM
Co-Convener
Dr. Uday Chakkingal, MME, IITM
Treasurer
Dr. K C Hari Kumar, MME, IITM
Secretaries
Mr. R Vijay, MME, IITM
Mr. P Gerald Tennyson, MME, IITM
Members
Prof. D R G Achar, IITM
Prof. B Guha, IITM
Prof. B S Murty, IITM
Prof. Paramanand Singh, IITM
Prof. S D Pathak, IITM
Prof. K Prasad Rao, IITM
Prof. T S Prasanna Kumar, IITM
Prof. S Raghavan, IITM
Prof. P Rodriguez, IITM
Prof. S K Seshadri, IITM
Prof. P Venugopal, IITM
Dr. M Balasubramanian, IITM
Dr. S S Bhattacharya, IITM
Dr. S Ganesh Sundara Raman, IITM
Dr. M Kamaraj, IITM
Dr. V Sampath, IITM
Dr. T S Sampath Kumar, IITM
Dr. Ashutosh S Gandhi, IITM
Dr. G Phanikumar, IITM
Dr. Ranjit Bauri, IITM
Dr. N V Ravi Kumar, IITM
Dr. Ravi Shankar Kottada, IITM
Dr. S Sankaran, IITM
Dr. V Subramanya Sarma, IITM
Mr. Devinder Yadav, IITM
Ms. P Susila, IITM
Ms. R Sangeetha, IITM
Mr. Manjith, IITM
Mr. Ganesh Niranjan, IITM
Mr. N R Rajasekaran, IITM
Mr. T V K Kidao, MMSPL, Chennai
Dr. R Mahadevan, India Pistons, Chennai
Dr. T V L Narasimha Rao, Sundaram Clayton, Chennai
Mr. R Natarajan, TII Group, Chennai
Mr. V Parthasarathy, Wave Current Automotive. Chennai
Mr. N Sampath Kumar, Ambattur Metal Treators, Chennai
Dr. P Sivaprasad, IGCAR, Kalpakkam
Dr. S Srikanth, NML, Chennai
Mr. B K Venkatesh, Techmat Enterprises, Chennai
Dr. S Venugopal, IGCAR, Kalpakkam

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About the Organizing Bodies
Department of Metallurgical and Materials Engineering

The Department of Metallurgical Engineering was established in 1959. President of India in his
capacity as the Visitor of IIT Madras approved the change of name of the Department of
Metallurgical Engineering as Department of Metallurgical & Materials Engineering with effect
from 12th March 2003. The Department offers B.Tech., Dual Degree, M.Tech., M.S. and Ph.D.
programmes. The Department has excellent research infrastructure in the broad areas of
materials processing (forming, joining, casting, particulate processing, nanostructured
materials), characterisation (X-ray diffraction, electron microscopy, thermal analysis, scanning
probe microscopy), mechanical testing, environmental degradation, surface engineering, and
computational materials science.

The Department has 29 faculty members: 10 Professors, 8 Associate Professors and 9 Assistant
Professors. In addition, one Emeritus Professor and one Distinguished Visiting Faculty Member
are also hosted by the Department.

Contact Details
Department of Metallurgical and Materials Engineering
Indian Institute of Technology Madras
Chennai - 600 036
INDIA
Phone: +91 44 2257-4750 (Office)
Phone: +91 44 2257-4751 (HoD)
Fax: +91 44 2257-4752 (Dept.)
Fax: +91 44 2257-0509 (Institute)
e-mail: mtoffice@iitm.ac.in
http://mme.iitm.ac.in/

Indian Institute of Metals Chennai Chapter

Indian Institute of Metals (IIM) is a premier organization representing materials and


metallurgical engineers in India. Founded in 1946 by a group of metallurgists, today IIM is the
largest professional organization for metallurgists and materials scientists in India with over
8000 members from R&D laboratories, academia and industry. The two primary objectives of
IIM are: promoting and advancing the science and technology of metals, alloys and materials and
protecting the interests of metallurgists, material scientists and metallurgical industry. The
Institute has been honored by the Ministry of Steel and Mines, Govt. of India, by naming 14th of
November as National Metallurgists Day (NMD) and instituting awards for distinguished
metallurgists to be conferred on that day every year. The institute organizes various meetings,
seminars, conferences, workshops and courses through its three Divisions namely, Ferrous,

iv
Nonferrous and Metal Sciences and 52 Chapters at different places regularly, providing
opportunities for researchers and industry to come together and exchange ideas of mutual
interest. It also organizes an Annual Technical Meeting (ATM) and immediately following NMD
celebrations, where in 400-500 metallurgists and material scientists from academia, R&D
institutes and industry share their recent research work in various fields. IIM Chennai Chapter
functions from the Department of Metallurgical and Materials Engineering of Indian Institute of
Technology Madras. The main objective of the Chapter is to disseminate knowledge in the field
of Metals, Materials and Metallurgy in this part of the country. This is achieved by arranging
lectures by eminent metallurgists, conducting workshops, organizing seminars, courses, etc. The
Chapter has arranged a large number of lecture talks by eminent scientists, industrialists and
experts from India and abroad. The Chapter has also conducted many workshops /courses /
seminars by national and international experts. The Chapter is also a Centre for conducting
examinations leading to Associate Membership of IIM. IIM Chennai Chapter has been
conducting preliminaries of Prof. Brahm Prakash Memorial Materials Quiz every year for Class
XI and XII students of various schools in Chennai. Two teams are selected and they represent
IIM Chennai Chapter in the National Level Prof. Brahm Prakash Memorial Materials Quiz at
Kalpakkam.

Office Bearers
Chairman - Prof. Kesavan Nair
Vice Chairmen - Dr. S. S.Bhattacharya
Hon. Secretary - Dr. S. Sankaran
Hon. Treasurer - Dr. R. Bauri

Contact Details
The Indian Institute of Metals Chennai Chapter
C/o Dept. of Metallurgical and Materials Engg.
IIT Madras, Chennai – 600 036
Phone: 044 – 2257 4750
E-mail: mtoffice@iitm.ac.in
Fax: 044 – 2257 0509 / 2257 4752

METSA

METSA is the Metallurgical and Materials Engineering Students’ Association of the Department
of Metallurgical and Materials Engineering IIT Madras. A wide range of activities are organized
under the banner of METSA and these activities serve to enhance interaction between students
and faculty of the Department of Metallurgical and Materials Engineering, IITM.

METSA has organized several contests with joint student-faculty teams participating. These
include quiz, dumb charades and pictionary contest, and a cricket match. A welcome dinner for
all the incoming students of the Department was organized.

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METSA organizes an annual technical festival “Amalgam” for B.Tech / M.Tech students from
Materials and Metallurgy Departments of the country. Events include paper presentation, guest
lectures, lecture-demonstrations and quiz.

METSA also releases an annual magazine called 'Etch' with articles contributed by the students
and faculty members of the Department.

Activities of METSA provide platform for student-faculty interactions and members of METSA
and the faculty of the Department share fond memories of the games, dinner and joint student-
faculty variety entertainment programme conducted at a beach.

Office bearers

Chairman : Prof. P. Kesavan Nair

Treasurer and Faculty Advisor : Dr. N.V. Ravi Kumar

Secretaries : Mr. Rahul Ladhania & Mr. T. Ragesh

URL: http://metsa.iitm.ac.in/

Material Advantage Student Chapter at IIT Madras

A career in materials can bring you in contact with an amazing and almost endless
journey of discovery and creation

About the Chapter


The Material Advantage Student Chapter at IIT Madras was formed as the IIT Madras Student
Chapter of ASM International in November 2002. In 2005, ASM International, in collaboration
with
the other professional societies viz., The Minerals and Materials Society (TMS), Association for
Iron
and Steel Technology (AIST) and The American Ceramic Society (ACerS) launched the
Material Advantage
Program to promote materials science & engineering among students. The members of this
program have the benefits of membership of the ASM, TMS, AIST, and ACerS. The Material
Advantage
Student Chapter at IIT Madras is being managed entirely by the students, with guidance from the
Faculty Advisor. The Chapter was founded with 22 members and has now grown to a strength of
72.

Chapter Activities
Activities are focussed on professional development of student members and promote interest in
materials science & engineering among school children. The Chapter has been very active in
arranging lectures by

vi
eminent personalities, organising industrial visits, conducting conferences and innovative
workshops, and school outreach programmes for motivating the students to take up careers in the
field of materials science and engineering. The All India Material Quiz is organised by the
Material Advantage Chapter every year.

Chapter Achievements

x Chapter Excellence Award for 2004-2005


x Chapter Excellence Award for 2005-2006
x Highest Membership Award for 2005-2006
x Award for the Most Number of New Members Recruited, 2007-08
x Chapter of Excellence Award for 2007-08
x Special grant for conducting school outreach programme

Chapter Office Bearers


Faulty Advisor: Dr. Ashutosh S. Gandhi (a.s.gandhi@iitm.ac.in)
Chairman: P. Gerald Tennyson (geraldtennyson@gmail.com)
Vice-Chairman: P. John Felix Kumar (felix1976@gmail.com)
Secretary: Alaparti H.V. Pavan (pavanahv@gmail.com)
Treasurer: H. Khalid Rafi (khalidrafi@gmail.com)

Material Advantage Student Chapter at IIT Madras


Department of Metallurgical and Materials Engineering
Indian Institute of Technology Madras
Chennai-600036, INDIA
E-mail: asm_chennaistudent@yahoo.com
Material Advantage Program: www.materialadvantage.com
IIT Madras Chapter: http://mme.iitm.ac.in/matadv/

vii
Invited speakers

10th December 2008

Dr. Amol Gokhale

Scientist G, DMRL
Hyderabad

Cellular aluminum and other metals

11th December 2008

Shri. Pugazhenthy

President, IIM and Executive Director, India


Lead Zinc Development Association

Non-ferrous metals industry in India – The


unfolding scenario

12th December

Prof. K.A. Padmanabhan

Mercator Professor
University of Muenster, Germany

Ultrafine grain size through mechanical


processing
ISRS 2008 Programme Schedule
Wednesday, December 10th Thursday, December 11th Friday, December 12th
0800-0900 BREAKFAST
0900-0915
REGISTRATION PLENARY TALK II PLENARY TALK III
0915-0930
0930-0945
INAUGURATION
0945-1000
1000-1015 Nanoscience & Tech I Nanoscience & Tech II
PLENARY TALK I
1015-1030
1030-1045
HIGH TEA
1045-1100 TEA
1100-1115
1115-1130
Mechanical Behaviour I + Mechanical Behaviour II + Nanoscience & Tech III +
1130-1145
Carbon Nanotubes Synthesis & Processing Joining
1145-1200
1200-1215
1215-1230
1230-1245
1245-1300
LUNCH
1300-1315
1315-1330
1330-1345
POSTERS I POSTERS II POSTERS III
1345-1400
1400-1415
1415-1430
1430-1445
Electronic materials + Surface Bio & Functional Materials + Optical Materials + Materials
1445-1500
Engg. Energy Technology Degradation
1500-1515
1515-1530
1530-1545 TEA
1545-1600
1600-1615
Composites + Modeling & VALEDICTORY
1615-1630 Magnetic Materials + Forming
Phase stability
1630-1645
1645-1700 HIGH TEA
1900 Dinner Dinner
ABSTRACTS
ISRS-2008 1

18>5D=2C8>=0;<0C4A80;B

BF-O1
PRESSURE DEPENDENCE OF ELECTRONIC STRUCTURE OF SmSe
Gupta D.C., Subhra Kulshrestha, Gajendra Raipuriya, Singh K.C., and Sushil Auluck*,
Condensed Matter Theory Group, School of Studies in Physics, Jiwaji University, Gwalior, India
* Department of Physics, Indian Institute of Technology, Kanpur,India

The present paper is an attempt to study various crystal properties viz. structural, electronic and optical
properties of SmSe as a function of pressure has been computed by the ab-initio pseudo-potential approach
using the density functional theory under the generalized gradient approximation (GGA). It is found that this
compound undergoes a structural phase transformation from B1 (NaCl structure) to B2 (CsCl structure) at
high pressures. We have investigated the structural phase transformation, electronic band structure and density
of states (DOS) in parent as well as at high pressures. The calculated lattice constant, bulk modulus and its
pressure derivative under ambient conditions are in good agreement with their corresponding experimental
data. The band structure of SmSe shows X). The value of energy gap is in good agreement_ indirect band
gap (with the experimental one. The upper valence bands in SmSe are characterized by Se-5p states and
Sm-5d states. Beside this, we have also computed the real and imaginary part of dielectric function. We have
analyzed the interband contribution to the optical properties of SmSe.

BF-O2
BIOACTIVITY ENHANCEMENT OF COMMERCIAL PURE TITANIUM
THROUGH EQUAL CHANNEL ANGULAR PRESSING
Thirugnanam A., Sampath Kumar T.S., Uday Chakkingal
Dept.of Metallurgical & materials Engg, Indian Institute of Technology, Madras, India

Commercial pure titanium (CP Ti) has been the material of choice for medical implants. There is great
interest in the formation of nanosize/submicron grains due to their unusual properties as the morphology of
the biomaterial is critical to its success as an implant material i.e. cells live in a nano-featured environment
of a complex mixture of pores, ridges, and fibers of extracellular matrix (ECM). This information eventually
leads to the concept of nano biomaterials with advantages over conventional biomaterials. Equal channel
angular pressing (ECAP) is one of the severe plastic deformation (SPD) processes used to obtain
submicron/nano sized grains in bulk metals. Plastic deformation of titanium is difficult at room temperature
due to limited active slip systems. However, ECAP was done successfully at room temperature up to two
passes. The objective of the present work is to study the bioactivity of ultra fine grain refined CP Ti processed
by ECAP in simulated body fluid (SBF). ECAP at room temperature was done using route BC in 120 degree
die angle. Drastic grain refinement (~300nm) was observed in Transmission Electron Microscopy (TEM).
Chemical treatment (acid+alkali) was done on the processed specimen to enhance bioactivity. The processed
specimen was immersed in SBF for 2, 4 weeks to access its bioactivity. The immersed specimen were
characterized using SEM-EDAX and XRD to study the formation of hydroxyapatite(HA). It was observed
that 2nd pass specimen exhibited dense and homogenous hydroxyapatite coating when compared to
unprocessed and 1st pass condition. This is due to increase in surface area as a result of chemical treatment
which favors more HA to nucleate and grow. The mechanism for enhancement of HA formation will be
discussed in detail in this study.
2 ISRS-2008

BF-O3
EVALUATION OF HEXAVALENT CHROMIUM REDUCTION
BY BACILLUS SP
Mary Mangaiyarkarasi M.S.1,2, Vincent S.2, Janarthanam S.3, Tata B.V.R1
1
Materials Science Division, IGCAR, Kalpakkam, India
2
PG and Research Department of Zoology, Loyola college, Chennai, India
3
Department of Zoology, University of Madras, Chennai, India

Bioremediation of heavy metals is studied widely using various microorganisms. But the subcellular
localization of the heavy metal reducing ability, in these organisms is less studied. Three of the bacteria (G1,
G2, G7) isolated from soil exposed to tannery effluent were found to have a minimum inhibitory concentration
(MIC) of 500ppm of Cr (VI). One of the isolates G7 was found to take up high concentration of Cr (VI) and
hence selected as the test organism. G7 was identified as Bacillus sp. through the biochemical tests and 16S
rRNA sequencing. The sequencing results show that it has close homology (100%) with Bacillus subtilis.
This organism was studied for its Cr (VI) uptake ability at various initial concentrations of 50 to 150ppm.
Experiments using whole cells and permeabilized cells of G7 confirmed that a protein, present either in the
soluble or membrane fraction, carries out the reduction process. Further the Cr (VI) reduction assays using
the cell free extract and the membrane fraction of the cells revealed the role of membrane bound proteins in
chromium reduction. In order to investigate the nature of the enzyme involved in chromium reduction, assays
were carried out using the intracellular extract and the membrane fraction of cells exposed and unexposed
to Cr (VI). The results of intracellular extract assay demonstrated that the chromium reducing enzyme is
constitutive in nature and not inducible. The difference in reduction of chromium was very negligible (5%).
And the membrane fraction of exposed cells showed less reduction ability compared to membrane fraction
of cells unexposed to Cr (VI). Thus the association of the protein to the membrane fraction and its constitutive
nature are confirmed in the Bacillus sp. through these assays.

BF-O4
EXPERIMENTAL AND NUMERICAL STUDIES ON MECHANICAL
BEHAVIOUR OF BOVINE CORTICAL BONE USING MINIATURE
SPECIMEN TECHNIQUE
Chitti babu V., Sehgal D.K., and Pandey R.K.
Indian Institute of Technology, Delhi, India

Measurement of mechanical properties of biological materials often sets important constraints such
as the limited size or the irregular geometry etc. These constraints may be overcome by employing miniature
specimens for mechanical testing. The advantage of such miniature specimens includes the possibility of
sampling very small volume of material within a heterogeneous structure such as cortical bone. Though the
miniature specimen test technique has been used by a number of investigators to predict mechanical properties
in metallic alloys the work reported in case of bones is practically non-existent. This paper describes the
miniature specimen test technique for the study of mechanical behavior of Haversian (matured) bovine
cortical bone. The matured bovine cortical bone has been described as a transversely isotropic material. For
the present investigation rectangular shaped miniature specimens of sizes 10mm (length) u 2mm (width) u
1mm (thickness) were carefully prepared from the middle third portion of the Bovine tibia in longitudinal
and transverse (circumferential) directions. The samples were machined by low speed Buehler Isomet linear
ISRS-2008 3

precision diamond saw under continuous water spray to minimize the thermal damage. Specimens were
subjected to Small Punch Testing at room temperature in wet condition using an MTS (810 model) machine.
A specially designed fixture was used to hold the specimens in the MTS machine and the load vs load point
deflection measurements were taken during the test. The experimental data obtained from miniature specimen
tests were further analyzed to obtain the standard mechanical properties of the cortical bone such as the yield
strength, fracture strain and fracture toughness. The results obtained from miniature specimen tests were
validated by conducting tensile tests and fracture toughness tests on large size specimens from mid diaphysis
of bovine cortical bone in both longitudinal and transverse directions. A good agreement was found between
the results of miniature test and standard specimen tests. Further, finite element simulation was employed to
obtain load-load point deflection diagrams in the miniature specimens by using the elastic-plastic deformation
data from the standard tensile tests conducted in the longitudinal as well as the transverse direction of the
specimens from the cortical bone. The simulation results were found to be in good agreement with
experimental results from miniature tests. The results have been discussed and the main findings have been
outlined.

BF-O5
POLYMER-MnO2-MWNTs BASED BIOSENSOR
FOR THE DETECTION OF ORGANOPHOSPHORUS NERVE AGENTS
Neetu Jha and Ramaprabhu S.
Department of Physics, Indian Institute of Technology Madras, India

The development of a disposable Acetylcholinesterase (AChE) based biosensor is described. The


process of multi walled carbon nanotubes (MWNT) by chemical vapor deposition technique has been
detailed. The as-grown MWNT have been purified by acid treatment and air oxidation methods. MWNT are
further functionalized by hydrophilic functional groups. Nanocrystalline MnO2 particles have been attached
on the surface of MWNT by chemical reduction method. Further, the conducting polymer polypyrrole has
been uniformly coated over the MnO 2MWNT surface using chemical oxidative technique and used for the
electrode preparation over GC electrode. The nanocomposite was characterized by scanning electron
microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). The high catalytic
activity of MWNT composite towards the electroxidation of thiocholine has been utilized for the detection
of nerve agent paraoxon. Due to high porosity of polymer and high electrical conductivity of CNT based
composite, an excellent detection level for paraoxon could be achieved. The details of fabrication of the sensor
and the dependence of the sensitivity have been discussed.

BF-P1
PIEZOELECTRIC AND DIELECTRIC PROPERTIES OF PURE AND
DOPED PZT WAFERS
Sudipta Goswami* #, Soumen Mandal, Dhruba Pal, Anshuman Seal and Sen A.
Central Glass & Ceramic Reasearch Institute, Kolkata, India

PZT near its MPB (morphotropic phase boundary) has got tremendous technological importance in
the field of transducers, sensors, actuators, mechanical filters etc. Dielectric and piezoelectric properties of
PZT ceramics are strongly dependent on domain wall motion. Incorporating lead or oxygen vacancies into
the original perovskite structure can alter this domain mobility. ‘Donor’ doping induces lead- vacancies
4 ISRS-2008

whereas ‘acceptor’ doping induces oxygen vacancies to maintain the charge neutrality. Hence by
manipulating the composition via doping it is possible to tailor the properties for various technical
applications. The current trend of miniaturization demands scaling down of the size of the electronic
components. Thus high-density PZT wafers are desired for the development of piezoelectric transducers,
micro sensors, pyroelectric detectors and embedded surface mounted sensors and actuators for structural
health monitoring. It is therefore very challenging to produce high quality doped and pure PZT wafers instead
of bulk samples. Morphotropic, ‘donor’ doped and ‘acceptor’ doped PZT powders were prepared via citrate
nitrate combustion method. The powders formed were calcined at a relatively low temperature (550qC) to
get high quality phase pure material. The wafers were fabricated using tape-casting method followed by
sintering. The dielectric and piezoelectric properties of the wafers were compared with those of the
corresponding bulk samples and the possible reasons behind the discrepancies have been discussed.

BF-P2
DIELECTRIC AND FERROELECTRIC PROPERTIES OF PLD
GROWN BiFeO3 THIN FILMS
Ramachandran B., and Ramachandra Rao M.S.
Dept of Physics, Indian Institute of Technology, Madras, India

Multiferroics are materials which exhibit one or more of ferroic properties, namely ferroelectric,
ferromagnetic and ferrotoric. The coupling between two order parameters, called the magnetoelectric effect,
is very interesting from the point of view of fundamental Physics and could also lead to applications in
spintronics and other fields. In order to use the magnetoelectrics in devices, a preliminary step is to grow thin
films of magnetoelectrics. Among the possible candidates, BiFeO3 (BFO) has attracted much attention
because it has order temperatures far beyond 300 K [the ferroelectric Curie temperature is 1043 K and the
magnetic Néel temperature 647 K], which is essential for applications. In this work, we have grown BFO
thin films on Si(001) substrate with different substrate temperature (Ts 500  600qC) and oxygen partial
pressure (O2pp 6 u 10 4 to 0.6 mbar) by pulsed laser deposition (PLD). We have studied dielectric and
ferroelectric properties of BFO thin films grown on Pt (used as bottom electrode) coated Si (001) at optimized
conditions using impedance analyzer and ferroelectric loop tracer respectively. Details will be presented and
discussed.

BF-P3
IS TITANIUM A SUITABLE BIO-IMPLANT MATERIAL???
FRETTING CORROSION APPROACH
Satendra Kumar1, Sankara Narayanan T.S.N.1, Ganesh Sundara Raman S.2, Seshadri S.K.2
1
National Metallurgical Laboratory, CSIR Madras Complex, Chennai
2
Dept. of Metallurgical and Materials Engg. Indian Institute of Technology, Madras

Titanium and titanium alloys are widely used for many biomedical applications due to their low density,
excellent biocompatibility, corrosion resistance and mechanical properties. High strength Ti alloys are
particularly susceptible to damage caused by repeated small amplitude reciprocating sliding, typically at
attachment locations by a process known as fretting or fretting fatigue. However, these small amplitude
movements become more dangerous if they occur in an environment that is rich in chlorides. The combined
action of small movements between the contacting parts and the corrosivity of the environment leads to the
ISRS-2008 5

degradation of materials which is known as fretting corrosion. The fretting corrosion is produced by a
relatively small-scale (< 100 Pm) motion between the components. This motion increases the corrosion rate
because it causes a continuous fracture and re-passivation of the oxide layers of the metallic surfaces.
Orthopaedic implants, particularly the hip and knee joints, exposed to a physiological medium suffer due to
fretting corrosion. Fretting corrosion leads to a reduction in life-time of the prosthesis. Each year, about
800,000 hip joint prostheses are implanted in the world. However, within 9 years of use, 6 % have been
replaced because of an aseptic loosening of the femoral stem. The mechanical damage combined with the
corrosive action could cause the release of metallic ions and fine debris that could induce deleterious effects
on the surrounding tissues. In many instances, the wear debris triggers the liberation of macrophages inducing
bone resorption and osteolysis responsible for prostheses failure. The performance of titanium as an implant
material under fretting corrosion conditions was assessed using a fretting-corrosion test assembly in Ringer’s
solution (simulated body fluid). During the fretting corrosion tests, load and frequency were set at 3 N and
10 Hz respectively, while the on-time and off-time of the fretting motion were varied. The change in open
circuit potential (OCP) was measured as a function of fretting cycles/time. The extent of cathodic shift in
OCP caused by the rupture of the passive film due to fretting motion and the time taken for the OCP to
re-establish the steady state potential after the fretting motion is stopped indicate the performance of Ti under
fretting corrosion conditions. Electrochemical impedance spectroscopy study was also performed to get a
better understanding of the corrosion behaviour of Ti under static and fretting conditions.

BF-P4
DNA FUNCTIONALIZED GOLD-GRAPHENE BIOSENSOR FOR
DOPAMINE DETECTION
Jyothirmayee Aravind S.S., Tessy Theres Baby, Rakhi R.B., Arockiadoss T.
Dept of Physics, Indian Institute of Technology, Madras, India
The two dimensional one carbon atom thick graphene has excellent electronic properties due to the
ability of the electrons in graphene to conduct electrical current greater than one dimensional carbon
nanotubes. In addition, the increase in the surface area in graphene due to the availability of both surfaces
makes it a very promising candidate for sensing and biosensing applications. The present work demonstrates
the detection of dopamine using DNA Functionalized Gold-graphene biosensor. Single strand DNA based
Dopamine biosensor has been constructed using Au-graphene and its electrochemical detecting behavior has
been reported. Graphene have been synthesized by exfoliation of graphitic oxide, followed by
functionalization using concentrated acid. It is then treated with aquaregia for better dispersion and to improve
its combining capacity with DNA. Functionalized graphene is then decorated with nanocrystalline Au metal
clusters using a simple chemical reduction method. Special machine grade DNA[AC] 15 was used for
functionalization of graphene by a sonication process. Structural and morphological characterizations have
been carried out using SEM, TEM, HRTEM and FT-IR spectroscopy. Electrochemical characterizations have
been carried out using potassium ferro cyanide as the redox electrolyte. The detailed cyclic voltammetry
studies indicate the quick electron transfer showing that DNA-Au/graphene film is a good electrochemical
sensor.
6 ISRS-2008

BF-P5

FABRICATION OF AMPEROMETRIC GLUCOSE BIOSENSOR USING


TWO DIMENSIONAL GRAPHENE
Tessy Theres Baby, Jyothirmayee Aravind S.S., Rakhi R.B., Arockiadoss T., and Ramaprabhu S.
Dept of Physics, Indian Institute of Technology, Madras, India

Graphene, a single layer of carbon atoms arranged in a honeycombed lattice in a 2 D, has unusual
electronic properties which arise from the hybridization of unbound fourth electrons in orbitals extending
vertically above and below the plane spreading across the whole graphene sheet. As a result, the ability of
the electrons in graphene to conduct electrical current is 10 to 100 times greater than those in a normal
semiconductor like silicon at room temperature. This makes graphene a very promising candidate for future
electronic and biosensing applications. In the present work, graphene has been prepared by exfoliation of
graphitic oxide and characterized by powder X-ray diffraction (XRD), High resolution transmission electron
microscopy (HRTEM), atomic force microscopy (AFM), thermal gravimetric analysis (TGA) and Raman
spectroscopy. Amperometric biosensor has been fabricated by the deposition of glucose oxidase (GOD) over
Nafion-solubilized graphene electrode. The electrode used was glassy carbon electrode. The resultant
bioelectrode retains its biocatalytic activity and offers fast and sensitive glucose quantification. The
performance of the sensor was investigated by electrochemical methods at an optimum potential of  0.80
V and pH 7.0. The fabricated glucose biosensor exhibits a linear response up to about favorable glucose
content and an excellent detection limit and the results have been discussed.

BF-P6

PHOSPHORIC ACID GRAFTED MCM-41 IS A NOVEL BRONSTED ACID


CATALYST FOR TRANSESTERIFICATION REACTION OF DIETHYL
OXALATE WITH n-BUTY
Nedumaran D. and Pandurangan A.
ICPT, A. C. Tech, Anna University, Chennai, India

The focus towards healthy solid acid catalysts associated with recyclability laying road to the
preparation of Orthophosphoric acid grafted MCM-41 mesoporous molecular sieves. The various
concentration of Orthophosphoric acid was grafted on siliceous MCM-41 by wet impregnation method. The
material was dried and Calcined The prepared H3PO4/MCM-41 materials were characterized by X-ray
Diffraction analysis (XRD), BET surface area method, Pyridine adsorption FT-IR measurements, NH3-TPD,
XPES and31P NMR. The information about the acid sites, state and structure of grafted phosphorus species
were obtained from the physicochemical investigations. The morphology of mesoporous materials was
studied by TEM technique. The catalytic activity of the above materials was tested over single step organic
transformation reactions. The transesterification reaction of Diethyl oxalate with n-Butanol was studied to
check the catalytic activity of the synthesized mesoporous material. The pyridine adsorption FT-IR
investigations show the generation of Bronsted acid sites on mesoporous material. It enhances the selectivity
of the product. To get better yield the reaction parameters such as time, temperature and various concentrations
loading of catalyst were optimized. The leaching out of Phosphoric acid from MCM-41 and the reusability
were investigated.
ISRS-2008 7

2><?>B8C4B

CM-O1

INNOVATIVE PRODUCTION OF POROUS COPPER COMPOSITE


BY CHEMICAL REACTION
Ahmad Moloodi, Ramin Raiszadeh, Jalil Vahdati Khaki, Abolfazl Babakhani
Shahid Bahonar University of Kerman

Metal foams are a new, as yet imperfectly characterized, class of materials with low densities and novel
physical, mechanical, thermal, electrical and acoustic properties. Copper foams are popular metal foams that
are used in thermal conductors. This article describes a method named Self-propagating High-temperature
Synthesis (SHS) process to produce open cell copper composite foams. Porous Cu composite was fabricated
by reactions between CuO, Al and C powders. Gas released during these reactions and also the initial porosity
of the green powder compact were the source of the produced pores. The relative densities of the copper
composite foams have been investigated for different metal weight fractions. Optical microscopy and
scanning electron microscopy (SEM) were utilized to characterize the porous samples. Analyzing the
properties of the metal foams showed that the optimum weight fraction for blending initial powders was %84
CuO, %9.5 Al and %6.5 C. In addition, if the initial compacting pressure of the powders was decreased to
below 150MPa, the SHS reaction did not take place properly.

CM-O2

SHEAR BEHAVIOR OF REINFORCED CONCRETE T-BEAMS


WITH EXTERNALLY SIDE BONDED GLASS FIBER REINFORCED
POLYMER COMPOSITES
Bhattacharyya S.K. and Barai S.V.
Indian Institute of Technology, Kharagpur, India

Rehabilitation of structures becomes the new challenge for structural engineers today. Fiber Reinforced
Polymer (FRP) composite systems may be used for rehabilitation of reinforced concrete (RC) structures.
These materials are an excellent option for use as external reinforcing because of their light weight, high
strength, and high corrosion resistance. This paper presents an experimental study on the performance of
2500 mm long reinforced concrete (RC) T-beams strengthened in shear using epoxy bonded glass fiber fabric.
Experiments are conducted on nine simply supported RC T-beams, out of which six beams are used as control
beam with and without transverse steel reinforcements and rest three beams are strengthened in shear with
one, two, and three layers of glass fiber reinforced polymer (GFRP) in side of the web of the T-beams. The
6 mm dia. stirrups are provided at 200 mm spacing. All the beams are tested at the structural engineering
laboratory of IIT, Kharagpur by using 300 Ton hydraulic testing machine. It is observed that the magnitude
of the increased shear capacity is dependent not only on the type of GFRP but also on the internal transverse
steel reinforcement. The study also shows that the combination of GFRP layers and transverse steel is an
important factor to gain the ductility.
8 ISRS-2008

CM-O3
STRUCTURE AND PROPERTIES OF TRANSITION METAL NITRIDE
BASED SUPERHARD NANOCOMPOSITE COATINGS
Deepthi C., Harish, Barshilia C. and Rajam K. S.
Surface Engineering Division, National Aerospace Laboratory, Bangalore, India
The role of coatings as a surface modification technique has grown significantly for applications in
automobile, aerospace, electronic, biomedical, cutting tool and other sectors since they can impart specific
properties such as hardness, toughness, wear resistance, etc. to a surface. Transition metal nitride coatings
have been widely used as protective hard coatings to increase the lifetime of cutting and forming tools. The
use of hard coatings has spread well beyond tools; they are now being used for many tribological applications
and also for decorative purposes. Among the significant developments in the area of hard coatings has been
the synthesis of nanostructured coatings like nano-scale multilayers and nanocomposites. Highly
sophisticated surface related properties like mechanical, optical, magnetic, electronic and tribological
properties can be obtained using nanostructured coatings. Transition metal nitride based nanocomposite
coatings are the emerging class of superhard materials (hardness 40 GPa) and apart from high hardness they
also exhibit high oxidation resistance, toughness, corrosion and wear resistance and even retain their high
hardness at elevated temperatures. As these nanocomposite coatings display a combination of extreme
properties, they are expected to have a wide range of technological applications apart from the basic science
involved in the development of such coatings. We have developed a variety of superhard nanocomposite
coatings such as TiN/a-C, TiN/a-Si3N4, TiAlN/a-Si3N4, CrN/a-Si3N4 and CrAlN/a-Si3N4. This
presentation will address issues related to the growth and characterization of these coatings. In particular, we
have used ion beam assisted reactive direct current unbalanced magnetron sputtering process to deposit these
coatings. Characterization techniques such as X-ray diffraction, X-ray photoelectron spectroscopy,
transmission electron microscopy, nanoindentation, scanning electron microscopy, atomic force microscopy,
energy dispersive X-ray analysis, micro-Raman spectroscopy, tribometer and potentiodynamic polarization
have been used. Correlation between the microstructure and various properties of the superhard
nanocomposite coatings will be presented.

CM-O4
FORMING AND ANLYSIS IN METAL MATRIX COMPOSITES Al/SiC
Vijayananth S., Kalaiselvan K., Ravi Subramanian
Madras Institute of Technology, Chennai, India
Superplastic forming analysis of Aluminium 6063 alloy which is reinforced with Silicon Carbide
particles. The presence of the reinforcement phase in a continuous Aluminium alloy Metal Matrix Composite
results in properties not attainable by other means, thereby enhancing the potential range of possible
applications. Aluminium metal matrix composite has wide range of applications in the field of Automobile
and Aeronautical structures. In this project the superplastic analysis of composite material will be done for
various particle size and volume fractions of Silicon Carbide. The Al/SiC can be formed by Stir casting
process and Compare the strength of the materials. Cavitational behavior of the material has been studied.
ISRS-2008 9

CM-O5
EVALUATION OF COMPRESSIVE PROPERTIES OF EPOXY RESIN
FILLED WITH FLY ASH POLYMER MATRIX COMPOSITE MATERIALS
Arun Kumar M.B. and Swamy R.P.
University BDT College of Engineering

This paper summarizes attempts to incorporate fly ash into epoxy matrix to evaluate the compressive
properties of fly ash epoxy composite materials. It is shown that fly ash can be incorporated effectively into
an epoxy matrix to build fly ash epoxy composite material. With the purpose of characterizing the compressive
properties of the promising low density epoxy/fly ash composites, a series of epoxy composites filled with
different volume fractions of fly ash content are prepared in this work. Compression tests on the cured fly
ash epoxy composites are performed using computerized universal testing machine and the results are
discussed.

CM-P1
PREPARATION AND CHIP ANALYSIS OF ALUMINIUM
MATRIX COMPOSITES (AMC)
Arunachalam R.M., Sasikumar R. and Karthikvenkatesh G.
Dept of Mechanical Engg. Sona College of Technology, Salem, India

In the recent years, the nanostructured materials have been identified as a new wave towards
millennium innovations in the materials science engineering. With reduction of a characteristic length such
as the grain size or the cluster or molecular size, the normal properties of materials are drastically changed.
By large strain plastic deformation of materials the grain sizes are refined in the range of submicron level.
In this research Aluminium Metal Matrix composites (AMC) casting of 15% silicon carbide (SiC) particle
and 85% Aluminium alloy (LM25) is prepared by stir casting method. Aluminium is melted in a composite
furnace and preheated SiC particles are added and stirred. The molten mixture was then poured into a metal
die of diameters 50mm and length 100mm. The casted AMC was machined using tungsten carbide coated
cutting tools. Newly designed mechanical Quick Stop Device (QSD) was fabricated for the chip root study.
AMC chip root samples were obtained using the fabricated QSD. The chip sample was mounted and prepared
for microstructure analysis.
Key words: Stir casting, Machining, Aluminium Metal Matrix Composites.

CM-P2
FABRICATION AND TESTING OF GLASS FIBER EPOXY RESIN
COMPOSITE LAMINATE
Komuraiah A.*, Srikath Rao D.**, Suvarna Raju L.*, Devender V.**
*
Asst Prof, KITS(S) huzrabad, Asst prof, KITS(S) huzrabad Dist., Karimnagar
**
Asst Prof., Asst Prof. S R, Engineering college

A composite material is a combination of two or more materials having compositional variations and
depicting properties distinctly different from those of individual materials of the composites. The composite
material in general better than the individual components regarding their strength, heat resistant and stiffness.
The composite materials are widely used in aerospace industry, underwater exploration and other so many
10 ISRS-2008

industries. In this paper we want to explain how to fabricate the laminate (specimen) of glass/ epoxy composite
and test it. Than the results are compared with the conventional materials i e mild steel. We have found the
modulus of rigidity of the composite material is 1.54 u 10e5 N/sq mm where as mild steel is 8.9 N/sq mm
and Young’s modulus of elasticity is for composite specimen is 0.73 u 10 e 4 N/sq mm and mild steel is 2.01
u 10 e5 N/sqmm . We conducted tests to find brinels hardnes test, Impact test. The beauty of this
experimentation is that the specimens are prepared by commonly available materials and testing done on the
machines in our collages.

CM-P3
HYGROTHERMIC BEHAVIOR OF CARBON / GLASS REINFORCED
COMPOSITES
Sreejith M., Narasimha Murthy H.N., Krishna M., Rai K.S., Sharma S.C.
R.V.College of Engineering, Bangalore, India
Moisture absorption and Hygrothermic aging of 2-D woven mat glass / carbon reinforced epoxy / vinyl
ester composites were thoroughly studied for their suitability to marine applications. The laminates (250 u
250 u 3 mm) were fabricated using hand lay-up process maintaining a fibre / matrix ratio of 65: 35 by wt %
and were naturally cured as post curing is not recommended for marine applications. The test coupons were
exposed to 50oC 60oC, 70oC and 95 % RH for a maximum duration of 196 days in a programmable
environmental chamber supplied by M/s CM Equipment. The specimens were periodically withdrawn and
weighed for moisture absorption and tested for mechanical property (UTS, FS and ILSS) degradation. The
maximum moisture absorption under the test conditions was found to be in case of Epoxy / glass specimens,
i.e. 0.95 % at 700oC, 95 % RH and 0.87 % at 500oC. The least moisture absorption was in the case of vinyl
ester/carbon specimens being 0.55% at 700oC, 95 % RH and 0.5% at 500oC. Diffusion mechanism was
studied based on the Fick’s law of diffusion. Diffusion coefficient (D) was found to be the highest (5.52 u
E-6) in case of epoxy/glass specimens and the lowest (3.65 u E-6) for Vinyl ester / Carbon at 50oC, 95 %. D
increased with increase in temperature for all the specimens. Between Vinyl ester / Carbon and Epoxy / carbon
specimens the former showed lesser drop in ILSS, UTS and FS. Vinyl ester / glass specimens proved superior
to Epoxy / glass specimens with respect to degradation in the mechanical properties. Though the degradation
in the mechanical properties increased with increase in temperature from 50oC to 70oC, the degradation was
higher when the temperature was increased from 50 and 60o C than from 60 to 70oC. The overall observation
was that Vinyl ester proved superior to epoxy and carbon to glass. These experimental observations are
confirmed by scanning electron micrographs which showed better adhesion of the fibre to the matrix and
lesser plasticization effect of the matrix in case of vinylester/carbon specimens. The better performance of
vinyl ester was attributed to the gel coat which minimizes the voids and decreases water permeation. The
number of days to attain maximum moisture absorption increased with respect to increase in temperature in
all the four types of specimens. The duration was the least (39 days at 50oC and 48 days at 70oC) in case of
vinylester / carbon specimens. Vinylester based specimens showed stability with respect to degradation unlike
the epoxy based specimens which showed continuous drop in the mechanical properties.
ISRS-2008 11

CM-P4
MORPHOLOGY AND DYNAMIC MECHANICAL PROPERTIES OF
PP/MMT/OMMT HYBRID NANOCOMPOSITES
Selvakumar V., Palanikumar K., Palanivelu K.,
Dept of Mechanical & Production Engineering, Sathyabama University, Chennai, India

This article addresses the effect of nanoclays montmorillonite (MMT) and organo-montmorillonite
(OMMT) on morphology and dynamic mechanical properties of polypropylene (PP). The preparation of
polymer hybrid nanocomposites by melt compounding PP with MMT and OMMT using polypropylene
grafted maleic anhydride (PP-g-mA) as compotibilizer is described. First stage compositions with MMT
content 1%, 3%, 5% and 7%by weight ratio PP/MMT nanocomposites were prepared and tested. Second
stage compositions with OMMT content 1%, 3%, 5% and 7% by weight ratio PP/OMMT nanocomposites
were prepared and tested. Third stage both combined MMT and OMMT equally mixed content 1%, 3%, 5%
and 7% by weight ratio PP/MMT/OMMT hybrid nanocomposites were prepared and tested. The influence
of nanoclays on the impact fracture morphology of the nanocomposites was studied by scanning electron
microscopy (SEM). Dynamic mechanical properties (DMA) indicated significant improvement in the storage
modulus and loss modulus compared with neat PP. The tan peak signifying the glass transition temperature
of nanocomposites shifted to higher temperature.

CM-P5
SOME STUDY ON MECHANICAL PROPERTIES
OF POLYESTER HYBRID COMPOSITES
Sudha G.S. and Arun kumar M.B.
University BDT College of Engineering

The paper presents the results of experimental investigation on mechanical properties of polyester
hybrid composites. Mechanical properties such as compression, shear and hardness for varied volume
fractions of polyester, glass-fiber, silica and polyester, glass-fiber emery were conducted for both solid and
drilled specimens with varied wall thickness. Compressive strengths for solid and drilled specimens were
compared and their results were tabulated. It was observed that as the wall thickness varies from 2mm to
6mm in step of 2mm the compressive strength increases with increase in wall thickness and also percentage
increase in area and reduction in length for both solid and drilled specimen were noted and graphs were
plotted for percentage increase in area v/s specimen type. Hardness test was conducted and it was studied
that specimen codePGS4 and PGE2 had the highest RHN-B number.

CM-P6
HIGHER ORDER COMPUTATIONAL MODEL FOR THE STRESS
ANALYSIS OF ANTISYMMETRIC ANGLE PLY COMPOSITE PLATES
Swaminathan K. and Sangwai G.R.
National Institute of Technology, Surathkal, India

Fibre reinforced composite materials are increasingly used in industrial sectors due to their high
strength-to weight ratio, high stiffness-to-weight ratio, excellent corrosion resistance and satisfactory fatigue
durability. For composite plate structures, the elastic modulus to shear modulus ratio is relatively large as
12 ISRS-2008

compared to isotropic plates. The special properties exhibited by composite materials such as high degree of
anisotropy and weak rigidities in transverse shear make the method of analysis using computational models
based on Classical Laminated Plate Theory (CLPT) and the First Order Shear Deformation Theory (FSDT)
inadequate. Hence the mathematical modeling of the effects of transverse shear deformation and the cross
sectional warping has become an important area of research in the analysis and design of various structural
elements viz., plates and shells made up of fibre reinforced composite materials used in aerospace
applications. Developing accurate and efficient analysis methods for composite structures have consistently
been an important area to predict accurate failure patterns which consequently can be used for economical
and durable designs.
In the present investigation one such higher order displacement model with nine degrees-of-freedom
is used for the computation of transverse stresses which reduces the mathematical complexity in analyzing
the plates with 3 D elasticity solution. This computational model is based on Taylor’s series expansion of the
displacements in the thickness coordinate and incorporates the laminate deformations which account for the
effects of transverse shear deformation and a non-linear variation of in-plane displacements. A simply
supported plate subjected to sinusoidal transverse load is considered for the analysis. The equations of
equilibrium are obtained using Principle of Minimum Potential Energy (PMPE). Solutions are obtained in
closed form using Navier’s technique by solving the boundary value problem. Plates with varying aspect
ratios, degrees of anisotropy, fibre orientations and material properties are considered for the analysis.
Extensive numerical results are obtained and presented for the transverse deflection, inplane and transverse
stresses.
ISRS-2008 13

20A1>==0=>CD14B

CN-O1
MWCNT/CARBON BLACK DISPERSED INTO STRUCTURAL
ADHESIVE (EPOXY) USING TWIN SCREW EXTRUDER FOR
IMPROVED ELECTRICAL CONDUCTIVITY
Jeena J.K., Narasimha Murthy H.N., Krishna M., Rai K.S.
R.V. College of Engineering, Bangalore, India

Structural adhesives are used extensively in space and aerospace industries for adhesive bonding of
both metallic and composite materials. Conductivity is required across the joints to prevent static charge
build-up. Research efforts are concentrated on improving the conductivity of structural adhesives and one
potential method is to disperse nanofillers into the adhesive systems. Though several methods of dispersion
of nanofillers such as MWCNT and carbon black (CNP) into Epoxy systems are reported achieving uniform
dispersion of the conductive fillers is still a challenge especially in case of adhesive grades. This paper presents
adoption of co-rotating twin screw extrusion for dispersing MWCNT / CNP into AV138M a structural
adhesive which is widely used in space structural applications. The process of dispersion was evolved based
on a patent on the twin screw extrusion for thermoplastics. Preliminary experiments were conducted to arrive
at the temperature, speed, residence time and the screw elements of the extruder. Nanocomposite samples
with up to 15 wt % MWCNT/ CNP were fabricated. Volume and surface resistivities of the nanocomposites
were measured as per ASTM D257using Keithley Model 6517 High resistance meter. Both CNP and
MWCNT showed drop in electrical resistivity of the neat resin; a drop to the extent of 1010 ohm-cm, which
was achieved with 10 wt % MWCNT loading and the same was with 15 wt % in case of CNP. With the
corresponding values of volume resistivity the structural - cm) to:adhesive (AV138M) transitioned from
totally insulative (E 15 - cm). The experimental values were compared:dissipative range (E 5 with analytical
computations using Power law equation. SEM and AFM were used to examine the dispersion. The effect of
nanofillers on the glass transition temperature was studied using DSC. Tg improved by 10q in case of
MWCNT and by 4qC in CNP composites compared with that of neat resin.

CN-O2
FABRICATION OF CARBON NANOTUBE BASED
ELECTRODES FOR WATER PURIFICATION
Ashish Kumar Mishra and Ramaprabhu S.
Indian Institute of Technology, Madras, India

Carbon nanotubes (CNTs) are currently the focus of intense research interest due to their exceptional
physical, chemical and electronic properties that could impact broad areas of science and technology, ranging
from super strong nanocomposites to nanoelectronics. Water purification is one of the most important areas
of research in the present era,since natural water has different metal ions which cause different diseases. High
aspect ratio of CNT makes it a suitable candidate for water purification due to the fact that its large surface
area provides enough adsorption sites for harmful metallic ions present in some natural sources of water.
Although sodium (Na) is an essential element for human beings, excess of Na cause health problem and
hence there is need for a mechanism which can reduce the excessive amount of Na from natural water.
14 ISRS-2008

Therefore in the present study, the reduction of Na metal ion in water is being focused by the ion exchange
mechanism with CNT based electrodes. CNTs have been synthesized by chemical vapor deposition technique
and the appropriate CNT based nanocomposites have been prepared by chemical methods. CNT based
electrodes have been fabricated over a flexible carbon fabric substrate using appropriate binder with a special
treatment to regain the porosity of the CNT. The performance of these electrodes for the removal of Na ion
in water has been discussed.

CN-O3
SYNTHESIS OF CNTs OVER MESOPOROUS MCM-41
MOLECULAR SIEVES
Malarvizhi A. and Pandurangan A.*
ICPT, A. C. Tech, Anna University, Chennai, India

Carbon nanotubes-based bio-nano-systems, which are formed by functionalizing nanostructures with


biological/biochemical molecules, utilize unique properties of nanostructures in conjunction with remarkable
biological/chemical species recognition capabilities, exhibiting great potential for biological and biochemical
applications. Carbon nanotubes were synthesized by CVD method using acetylene as carbon source at
700-900 $C. Mesoporous Fe, Co and Mg-MCM-41 molecular sieves synthesized by hydrothermal method
in various ratios (25, 50, 75 and 100) were used as catalysts support for the growth of CNTs. The catalysts
were characterized by XRD, FT-IR and DRS-UV spectrum. The synthesized carbon nanotubes were purified
with acid treatment in order to remove the metal particles and other carbonaceous products. The purified
CNTs were characterized by SEM, TEM and Raman spectroscopy to know its surface morphology and
vibrational properties. These single walled carbon nanotubes were produced in high selectivity and the carbon
deposition was found to be more than 90 %. For cholestrol molecules, the most commonly used scheme is
to covalently link the CNT carboxylic acid groups.

CN-O4
WATER ASSISTED CHEMICAL VAPOR DEPOSITION FOR
MILLIMETER LONG GROWTH OF 2D ALIGNED CARBON
NANOTUBES
Ravi Joshi, Hermann Tempel, Jörg Engstler, Jörg J. Schneider
(Technische Universität Darmstadt Germany.)

Water assisted chemical vapor deposition is a unique route to grow millimeter long ultra pure carbon
nanotubes (CNTs). A small amount of water vapor and not the hydrogen gas plays a vital role as catalyst life
enhancer to keep catalyst clean from amorphous carbon, by which CNT growth rate as high as 20-30 %m
per minute can be achieved.

Here we present our work towards an understanding of the vital role of hydrogen gas and aluminum
metal as substrate for the typology of the CNTs grown. The type of CNTs grown essentially depends not on
the amount of water vapor supplied but on the quantity of hydrogen gas in the total gas flow as well as the
quality of aluminum used as a buffer layer. Our results confirm that hydrogen gas controls the number of
walls of CNTs grown while type and quantity of aluminum controls the catalyst particle size and thereby
controlling diameter of CNTs grown.
ISRS-2008 15

CN-O5

EFFICIENT PREPARATION OF CARBON NANOTUBES BY FLUIDIZED


FLOATING CATALYST METHOD USING Fe/Ni/Mg
Azira A.A.1*, Zainal N.F.A.1, Nik S.F.1, Soga T.2, Abdullah1S., Rusop M.1
1
Faculty of Applied Sciences
Universiti Teknologi MARA, 40450 Shah Alam, Malaysia
2
Nagoya Institute of Technology, Nagoya 466-8555, Showa-ku, Gokiso-cho, Japan

Fluidized floating catalyst method has been modified for preparing carbon nanotubes (CNTs) which
yielded high yield even at low temperature; 650qC. Optimum concentration for Fe/Ni/Mg (molar ratio of
Fe:Ni:Mg 1:1:1) has been found to be around 2.133% for the best yield. CNTs are produced from the
evaporation of part of the precursor (camphor oil) which decomposes in situ and aggregates on the metal
alloy catalyst particles present in the evaporating boat. Since the metallic alloy was obtained by calcining the
respective nitrates, it is expected to have residual entrapped nitrogen which may bond with the depositing
CNT. This result demonstrates that modified fluidized floating catalyst method is suitable for effective
formation of CNTs with average size ~11 nm. The morphological studies support ‘tip growth mechanism’
for the growth of the CNT’s in our case. The as-grown CNTs were characterized by FESEM and FTIR
spectroscopy. FTIR showed that nitrogen does go in the process and C-N is formed by accessing to the surface
carbon and instead of intercalating within the CNT.

CN-P1

ELECTRON FIELD EMISSION FROM CONDUCTING POLYMER


COATED METAL ENCAPSULATED AND METAL OXIDE LOADED
MULTI WALLED NANOTUBE COMPOSITE
Rakhi R.B., Sethupathi K. and Ramaprabhu S.
Indian Institute of Technology, Madras, India

Due to their natural geometry with high aspect ratio, chemical stability, high mechanical strength, high
electrical conductivity and the possibility of large scale production, carbon nanotubes (CNTs) have been
reported as excellent field emitters at low operating voltages. The realization of CNT based vacuum
microelectronics has been limited due to the absence of a stable film fabrication process over a suitable
substrate. The weak adhesion of CNTs to the substrate leads to catastrophic vacuum breakdown. In addition,
the electronic resistance between the CNTs and the substrate results in joule heating of the interface, reducing
the electrical contact between the emitters and the substrate. In order to overcome such undesirable effects,
we have fabricated a fully carbon based field emitter by spin coating a solution of surface modified multi
walled carbon nanotubes (MWNT) over a graphitized carbon cloth. MWNT have been synthesized by
chemical vapor deposition technique. Polymer/metal/metal-oxide dispersed MWNT have been prepared by
in-situ polymerization and chemical methods and field emitters have been prepared by spin coating the
composite material on suitable substrates. Field emission properties have been studied using an indigenously
made facility. The use of graphitized carbon woven as substrate has brought in flexibility in the fabrication
of carbon nanotube field emitters with reduced contact resistance and opens several new possibilities for
CNT field emitters.
16 ISRS-2008

CN-P2
CARBON NANOTUBE FILLED POLYMER NANOCOMPOSITES FOR
ELECTROMAGNETIC INTERFERENCE SHIELDING
Eswaraiah V., Sankaranarayan V. and Ramaprabhu S.
Indian Institute of Technology, Madras, India
With the rapid advances and broad implementation of telecommunication technologies, there is an
interest in shielding of electromagnetic interference in the radio and microwave frequency ranges. The use
of metals and their composites as effective shielding materials has disadvantage due to limited mechanical
flexibility, heavy weight and corrosion. Conducting polymers are promising materials for shielding
electromagnetic radiation because of their relatively high conductivity and flexibility. Due to their natural
geometry with high aspect ratio, chemical stability, high mechanical strength, high electrical conductivity
and the possibility of large scale production, carbon nanotubes (CNTs) can be used together with the
conductive polymers for possible electro magnetic shielding applications. In the present investigation, multi
walled Carbon nanotubes (MWNT) coated conducting polymer composites are fabricated by using
solution-casting method. Multi walled carbon nanotubes are prepared by catalyst supported Chemical Vapor
Deposition (CVD). Composites with different wt % of MWNT and MWNT have been characterized by
HRTEM, SEM, XRD, TGA and Raman spectra measurements. DC electrical conductivity at room
temperature for these composites has been measured and the transformation from insulator to conductor at
particular percolation threshold value of CNTs has been investigated. The effective use of MWNT filled
polymer composites as Electromagnetic Interference (EMI) shielding material has been discussed.

CN-P3
MULTI-WALLED CARBON NANOTUBES SYNTHESIS BY
MECHANO-THERMAL METHOD
Kesava Pandian, S. Karthik K. and Victor Jaya N.
Department of Physics, Anna University, Chennai, India
Mechano-Thermal method is a completely new method for carbon tube preparation, multi-walled
nanotubes (MWCNT) contain multiple graphite cylinders nesting within each other. The changes in the
crystallinity of graphite during milling have been examined on several occasions and the general conclusion
was that graphite passes through a nanocrystalline phase prior to amorphization. The mechano-thermal
method, consisting of a pre-ball milling and a subsequent thermal annealing process, can produce much larger
quantities of nanotubes due to a solid-state process without any vapor phase and the large milling capability.
In this present work graphite powder milled by ball-milling for 150 hours then annealed at 1200qC/6hrs in
nitrogen atmosphere. The prepared MWCNT’s were characterized by X-ray powder diffraction (XRD),
scanning electron microscopy (SEM) and Fourier Transform infrared spectroscopy (FTIR). Subsequent
annealing activates the growth of the (0 0 2) basal planes which shows that the prepared sample contains
CNT along with the amorphous carbon.
ISRS-2008 17

CN-P4
SYNTHESIS AND CHARACTERIZATION OF CARBON
NANOTUBES BY MECHANOTHERMAL PROCESS
Josephine Therasa J.
National Institute of Technology, Rourkela, India

This work is intended to study the characteristic nature of carbon nanotubes prepared by Mechano
thermal process. CNTs have been produced by first ball milling of graphite at room temperature and then by
annealing in the temperature range 1000  1200qC in the N2 atmosphere. Ball milling creates the nuclei for
nano tubes and the subsequent annealing is responsible for the formation of carbon nanotube growth. The
structure and morphology of as-prepared carbon nanotubes are characterized by XRD and SEM. Attachment
of impurities or functional groups with grown nanotubes were characterized by using FTIR spectroscopy.
The thermal behavior of the material is studied by using TGA and DTA measurement.

CN-P5
STUDIES ON CARBON NANOTUBE EMBEDDED
IN A SILICON DIOXIDE
ChandraKishore S. and Pandurangan A.
ICPT, A.C. Tech, Anna University, Chennai, India

In this work we use carbon nanotube (CNT) synthesized at low temperature using chemical vapor
deposition method. The above prepared CNT was purified by various acid treatment method .Carbon
nanotubes (CNTs) were investigated by Scanning electron microscopy (SEM), Transmission electron
microscopy (TEM) and Raman spectroscopy. A monolayer of CNT embedded in a dielectric film was
fabricated by sandwiching CNT between two silicon dioxide layers. Capacitance–voltage measurements at
300 K were studied to show CNT function as a floating gate in the above CNT/insulator /semiconductor
memory structure. The memory effect will be utilized in next generation flash memories.

CN-P6
STUDIES ON THE BROMINATED MULTI-WALLED
CARBON NANOTUBES
Zainal N.F.A.1*, Azira A.A.1, Nik S.F.1, Zain Ahmed A.2, Abdullah S.1 and Rusop3 M.
1
Faculty of Applied Sciences, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor, Malaysia
2
Research Management Institute (RMI) Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor, Malaysia
3
Institute of Sciences, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor, Malaysia

The multi-walled carbon nanotubes (MWCNTs) were brominated at room temperature by immersing
the MWCNTs in bromine solution. The MWCNTs were purified prior to the bromination process. The
intercalation of Br between graphene layers of MWCNTs was confirmed by the X-ray diffraction result,
showing an increase in the interlayer spacing compared to the MWCNTs without bromination sample.
Thermo-gravimetric analysis (TGA) was used to determine the content of the Br2 in the sample in which the
analyzer characterized the weight loss performed at a heating rate of 10q/min heating from room temperature
to 900qC in air flow.
18 ISRS-2008

4;42CA>=82<0C4A80;B

EM-O1
DIELECTRIC STUDIES OF Ca1-x Lax Cu3 Ti4-x Cox O12
SYNTHESIZED BY SEMI-WET ROUTE
Alok Kumar Rai, Mandal K.D. and Om Parkash,
Department of Applied Chemistry, Department of Ceramic Engineering,
Institute of Technology, B HU Varanasi, India

The calcium copper titanate Ca Cu3 Ti4 O12 (CCTO) is a distorted perovskite exhibiting a giant
dielectric constant with non-ferroelectric temperature behavior. The very large value of the dielectric constant
(k>10,000) and its near constancy over a wide temperature (100  600 K) and frequency (10 1MHz) range
make it a suitable material for memory and radio frequency applications in semiconductor technology. The
dielectric properties of CCTO that can be used in many commercial applications but it is only the loss factor,
which is restricting this material for variety of applications. It is well known that dielectric and electrical
properties of CCTO are strongly dependent upon the microstructure such as grain size and processing
conditions (such as oxygen partial pressure, sintering temperature and cooling rate) as well as doping. For
the doping effects, there are many examples in the literature such as substitution of Mn for Cu, La for Ca and
Zr for Ti. First time in this paper we have doped lanthanum and cobalt simultaneously in CCTO by semi-wet
route using solid TiO2 powder and metal nitrate solutions. TGA/DTA curves of the powder precursor shows
1073 K was considered as an appropriate annealing temperature for the gels. X-ray powder diffraction
analysis confirms the formation of single-phase at 1173 K. Energy dispersive X-ray analysis confirms the
high purity of the synthesized materials. The average grain size was determined by using Scanning electron
microscopy. Particle size was also confirmed by Transmission electron microscopy. The high permittivity
could be associated Maxwell-Wagner model, which was result from semiconducting grains and insulating
grain boundaries. The dissipation loss in the giant-dielectric constant materials CCTO was reduced to a level
of practical applications by the lanthanum doping.

EM-O2
INTERPLAY OF THE SINGLE PARTICLE AND JOSEPHSON
COOPER PAIR TUNNELING ON THE SUPERCONDUCTING
QUANTUM DOT JUNCTION
Archana Dhyani*, Tewari B.S. and Ajay
G.B. Pant University of Agriculture and Technology, Pantnagar, India

In the present paper we have investigated the interplay of the single particle and Josephson Cooper
pair tunneling on the Josephson supercurrent across the Superconducting Quantum dot junction having
s-wave symmetry order parameter and a single level uncorrelated dot. For this purpose we have used a
renormalized Anderson model that includes the single particle coupling of the superconducting lead, attractive
BCS effective interaction in the superconducting leads responsible for pairing and Josephson Cooper pair
tunneling responsible for the Cooper pair tunneling through such Superconducting Quantum dot junction.
We employed the Green’s function and Ambegaokar-Baratoff formalism to analyze the Josephson
supercurrent across such junction. We have pointed out that the Josephson supercurrent across
ISRS-2008 19

Superconducting Quantum dot junction is dominated by a competitive role of attractive pairing interaction
in the lead, energy of the dot level and also on the Josephson Cooper pair tunneling in an essential way.

EM-O3
NON-DESTRUCTIVE EVALUATION OF THERMAL AND ELECTRONIC
TRANSPORT PROPERTIES OF SEMICONDUCTOR THIN FILMS
Anita R Warrier, Sreekumar R., Sudha Kartha C., Vijayakumar* K.P.
Cochin University of Science and Technology, Kochi, India

Photothermal beam deflection technique is a non-destructive means of measuring the carrier mobility
and thermal diffusivity of semiconductor thinfilms. These properties are of major importance in determining
the device efficiency. Semiconductor materials when excited using a periodically chopped laser beam with
energy greater than the band gap of the material, causes emission of thermal waves due to intraband transitions
and carrier recombinations. Photothermal deflection (PTBD) technique was successfully employed for
characterization of indium selenide thin films. The chopping frequency was varied from 4 Hz to 2 kHz. The
refractive index gradient produced in the medium surrounding the sample is detected using a low power (0.5
mW) probe laser beam. The deflection of probe beam path is measured using bicell and lock in amplifier (SR
830). Indium selenide thin films were prepared by annealing In/Se bilayer systems. Thin films of selenium
(150 nm thick) were first deposited on glass substrate using chemical bath deposition technique, over which
30 nm of indium was deposited with the help of resistive heating technique (using molybdenum boat).
Thickness of the films was measured employing a stylus thickness profiler (Model – Dektak 6M). These
samples were later irradiated using 80 MeV Ni ions (from 15UD Pelletron accelerator) with a fluence of
ranging from 1-tera to 10-tera ions/cm2 at room temperature by using an electromagnetic scanner. Range of
80 MeV Ni in Indium selenide is about 15 Pm (calculated using TRIM code 95), so that it passes through
the film and gets embedded in the substrate. The minority carrier mobility of the film was found to increase
from 10 to 21 (cm) 2/Vs with increase in irradiation energy (1 tera to 3 tera ions/sq. cm) and decreases (3.6
(cm) 2/Vs) at higher energy irradiation (10 tera ions/sq. cm). This is because irradiation upto certain fluence
can anneal defects in the material but beyond that irradiation can cause creation of defects. We also observe
that the irradiation can cause increase in non-radiative thermal emission in the material. Hence we find the
increase in mobility upto 3 tera ions/sq. cm and decreases for higher fluence.

EM-O4
PREPARATION AND ELECTRICAL PROPERTIES
OF Sm28Fe72, Sm32Fe68 FILMS
Kamala Bharathi K. and Markandeyulu G.
Magnetism and Magnetic Materials Laboratory, Department of Physics, Indian Institute of Technology Madras, India

The electrical resistivity of Tb-Fe and Sm-Fe thin films are reported to increase with decreasing
temperature for certain composition range. This could be due the strain induced anisotropy that dominates
at low temperatures and lead to the development of in-plane anisotropy. Also the spin orbit interaction involves
in the scattering process. In the present case, preparation and the results of electrical resistance measurements
of Sm28Fe72, Sm32Fe68 films are reported. Sm28Fe72, Sm32Fe68 films were prepared by DC magnetron
sputtering on glass substrates. A composite target consisting of Fe disc and Sm chips was used. The number
of Sm chips was varied to get different compositions of Sm and Fe. The sputtering conditions used were the
20 ISRS-2008

following: The base pressure was 5 u 10 6 Torr; Ar was used as a sputtering gas and the sputtering was
carried out at 4 u 10 3 Torr with a DC input power of 300 W. The XRD patterns of both the films revealed
that they were amorphous. Compositional analysis was carried out by taking spot EDAX at different places
on the film. Electrical resistivity measurements were carried out from 300 K to 20 K using Van der paw
method. Resistance value was found to increase from 47.5 ohm (300 K) to 55.3 ohm (20 K) for Sm28Fe72
film and for Sm30Fe70 film the value was found to increase from 22.6 ohm (300 K) to 27.9 ohm (20 K).

EM-O5
CHANGE IN ELECTRIC POLARIZATION WITH
APPLIED MAGNETIC FIELD AT ROOM TEMPERATURE
IN DY MODIFIED BiFeO3 THIN FILMS
Mandal M., Prashanthi K., Duttagupta S.P. and Palkar V.R.
Centre for Excellence in Nanoelectronics, Indian Institute of Technology Bombay, India

Multiferroic systems, which exhibit coexistence of both ferroelectric and ferromagnetic ordering at
room temperature, are of great importance for a variety of device application. At the same time it is also
important to have presence of coupling between two order parameters since it gives additional degree of
freedom in device designing.
In this paper, we present the change in ferroelectric polarization with varying magnetic field in pulsed
laser deposited multiferroic Bi0.7Dy0.3FeO3 (BDFO) thin films grown on Pt/Si substrate. Experimental
results clearly show that as the magnetic field increases there is an improvement in ferroelectric hysteresis
loops. This trend is identical to what is normally obtained with applied electric field. The observed change
in ferroelectric polarization with applied magnetic field indicates that we have been able to orient ferroelectric
domains by means of applied magnetic field. It thus proves the coupling between magnetic and ferroelectric
order parameters in this system.

EM-P1
PREPARATION AND CHARACTERIZATION OF Nd2–xSrxCuO4
(WHERE x 0 to 0.2) CERAMIC COMPOUNDS
Anbarasu V., Sathiyakumar S., Manigandan A., Kaliyaperumal L.K. and Jayabalan K.
Anna University, Chennai, India

The search of higher transition temperature on inorganic compounds introduces the newer research
area “Ceramic Superconductors”. The search of newer ceramic superconducting compounds resulting with
the most productive research with TC around 40 K on La–(Ba/Sr)–Cu–O system. When substituting Cerium
and Strontium on the Nd2CuO4 system the compound Nd–(Ce/Sr)–Cu–O exhibits peculiar character of
n–type superconductivity and crystallize in two different crystal structures. Hence in the present work,
Strontium substituted Nd2–xSrxCuO4 (where x 0 to 2) system have been synthesized through solid state
reaction technique. Powder X – Ray Diffraction studies was carried out for the analysis of single phase
formation of the compound and it was revealed that variation on lattice parameters was linear with respect
to the substitution element. The possibility of n – type superconductivity was observed at x 0.15 because
of increase in lattice parameters causing increase in volume of the unit cell. Because of substitution of Sr
element on Nd site induces a variation on crystal system from parent tetragonal to orthorhombic and the
ISRS-2008 21

lattice parameters were calculated as: a 3.945(3) Å to 3.987(6) Å, b 3.927(6) Å to 3.946(2) Å and c
12.16(1) Å to 12.09(1) Å. From the vibrating sample magnetometer studies it was found that all the
compounds exhibit paramagnetic nature. A peculiar case of getting saturation magnetization on the lower
magnetic field was observed for Nd1.85Sr0.15CuO4 and Nd1.8Sr0.2CuO4 compounds which shows the weak
ferromagnetic nature at room temperature condition. Electron Spin Resonance (ESR) and Diffused
Reflectance Spectroscopy (DRS) studies were involved for the analysis of electronic structure and energy
gap values of the prepared compounds and results were discussed.

EM-P2
EFFECT OF UNI AXIAL PRESSURE ON Sm0.52Sr0.48MnO3
SINGLE CRYSTAL
Murugeswari A., Arumugam1 S. and Mandal P.
Bharathidhasan University, Thiruchirapalli, India

Doped manganite perovskites have been extensively studied because of their strong interactions
between spin, charge and orbital degrees of freedom. Single crystals of Sm0.52Sr0.48MnO3 were grown
using an optical floating zone surface. The quality of the crystal is checked by X-ray diffraction, electron
dispersive X-ray analysis etc. Effect of uniaxial pressure upto 120MPa on the electrical resistivity along both
c axis and ab plane of Sm0.52Sr0.48MnO3 was investigated for a wide c(T,P) rapidly increases withUab(T,P),
Urange of temperature. Both decreasing temperature until the metal insulator transition temperature (TMI)
is reached. The value of TMI is found to be 113K and it is extremely sharp and the sharpness does not
appreciably decrease upto c,Uhigher pressure range (P 120MPa). With increasing pressure along TMI shifts
towards lower temperature. The TMI decreases almost linearly with pressure. In contrast, TMI shifts towards
higher temperature with ab. The effect of pressureUthe application of uniaxial pressure along on electrical
resistivity is strongest near TMI and it indicates that the FM to PM phase transition is first order in nature.

EM-P3
EFFECT OF ANNEALING AND THICKNESS ON STRUCTURAL AND
ELECTRICAL RESISTIVITY OF FLASH EVAPORATED PBTE THIN FILMS
Kungumadevi L. and Sathyamoorthy R.
Kongunadu Arts & Science College,Coimbatore, India

PbTe thin films of different thickness were prepared onto cleaned glass substrates under a pressure of
6
9 u 10 Torr by flash evaporation method. The deposited films were annealed at different temperatures in
the range 373  573 K in vacuum. The X-ray diffraction analysis revealed that the as-grown films of lower
thickness grow with the stable phase NaCl-type structure whereas films at higher thickness unpredictably
exhibits all phases of PbTe (fcc NaCl, bcc CsCl and orthorhombic GeS). Interestingly, upon annealing all the
films exhibited hetero-phase of PbTe irrespective of film thickness. Growth mechanism of the prepared PbTe
films has been analyzed. The structural and lattice parameters of the films were calculated and they were
found to depend on thickness and annealing. Electrical resistivity was measured as a function of temperature
in the range 300-483 K and the energy gap was calculated from the Arrhenius plot. Both resistivity and band
gap have shown strong dependence on film thickness and annealing temperature. From the negative values
of TCR, it is inferred that PbTe films have semiconducting behavior.
22 ISRS-2008

EM-P4
FABRICATION AND TEMPERATURE DEPENDENT I-V
CHARACTERISTIC STUDIES OF n-ZnO / p-Si HETERO JUNCTION
Senthil Kumar E. and Ramachandra Rao M.S.
Dept.of Physics, Indian Institute of Technology, Madras, India
ZnO is ideally suited for blue-ultraviolet (UV) optoelectronics and transparent electronics due to its
direct and wide band gap (3.35 eV) and its ability to tailor electronic, magnetic and optical properties through
doping, alloying and nano engineering. ZnO exhibits intrinsically n-type conductivity and achieving high
quality, reproducible p-ZnO with sufficiently high mobility and hole concentration is difficult because of self
compensation effects due to its native defects. Thus, realization of high quality ZnO based homojunction
light emitting diode is still la challenging problem. In an alternate approach, ZnO based heterojunctions have
been focused for short wavelength optoelectronics. As a result a number of heterojunctions such as
n-ZnO/p-GaN, n-ZnO/p-SiC, n-ZnO/p-AlGaN, n-ZnO/p-NiO, n-ZnO/p-Si etc. have been fabricated to
successfully realize the UV electroluminescence (EL) and photo detection of ZnO.
n-ZnO thinfilm was fabricated on p-Si (100) substrate by pulsed laser deposition method at a substrate
temperature of 400qC and at pressure of 6 u 10 6 mbar. Al was deposited on back side of p-Si and top of
n-ZnO for top and bottom electrode. The junction area is defined as 500 u 500 Pm2 by UV-Lithography
technique. I-V characteristic of the junction was measured at different temperatures (from 77 K to 300K).
The junction shows very good rectifying characteristics at all temperatures. Turn-on voltage decreases from
9.6 V to 2.5 V and the saturation current increases from 5.7 u 10 5 A to 1.1 u 10 4 A as the temperature
increases from 77 K to 300 K. There is a four order decrease in reverse leakage current at a reverse bias
voltage of – 7.5 V as the temperature increases from 77 K to 300 K. These results will be presented and
discussed in detail.

EM-P5
DC CONDUCTIVITY OF ACTIVATED CARBON
FILLED EPOXY GRADIENT COMPOSITES
Navin Chand and Archana Nigrawal
Advanced Materials and Processes Research Institute (AMPRI),
(CSIR) (formerly RRL Bhopal) Hoshangabad Road, Bhopal, India
This paper reports the dc conductivity behavior of activated carbon powder filled epoxy gradient
composites. Activated carbon powder filled epoxy composites having 3 wt. % of activated carbon powder
and epoxy resin have been developed. dc conductivity measurements are conducted on the graded composites
by using an Electro-meter in the temperature range from 28qC to 150qC. dc conductivity increases with the
increase of distance in the direction of centrifugal force, which shows the formation of graded structure with
the composites. dc conductivity increases on increase in activated carbon powder content. Activation energy
was calculated and showed ionic conduction in the composites.
ISRS-2008 23

EM-P6
COMBUSTION SYNTHESIS AND DIELECTRIC PROPERTIES
OF Bi0.5Na0.5TiO3 - ZrO2 COMPOSITE
Kanagesan S., Velmurugan R., Jesurani S. and Kumar C.
SRM University, Chennai, India
Bismuth sodium zirconium titanate, a new class of ceramic composite powder was prepared by
combustion technique. Reactive metal nitrate and organic solvent are used as fuel. A yellow color precipitation
was obtained by slow evaporation of precursor solution at 90qC for 2 h. The final composition of powder is
Bi0.5Na0.5TiO3/ZrO2. The X-ray diffraction pattern BNZT composite calcined at 700qC shows the formation
of mixed phases. The characteristic peaks for BiTi3O12, Bi0.5Na0.5TiO3, m-ZrO2 and BiTiO3 were recorded.
The FTIR spectrum shows the absorption bands corresponding to N-H, NO2 and Zr-O)  (O-C O). The DSC
shows the crystallization of zirconium oxalate gel into zirconia at 470qC and Sodium bismuth titanate phase
between 625qC to 700qC. From TGA analysis, the major weight loss of 29 % was predicted and the overall
yield was calculated about 38 % of starting materials. The width and length of BNZT particle was measured
170 nm and 550 nm by atomic force microscope. At higher frequency side (1 kHz to 100 kHz), the dielectric
constant (varies from 75 to 211) is more or less temperature independent and not much increase until 400qC.
But, at lower frequencies (50 Hz to 100 Hz), the variation of dielectric constant is significant and attains the
maximum value of 2200 at 400qC. The X-ray diffraction analysis of calcined powder indicated that the
addition of zirconia suppress the predominant reflection peak at 32.48q corresponding to pure bismuth sodium
titanate (BNT) phase. For equal molar mixing of ZrO2 and BNT, zirconium exceeds the stabilization limits
and reduces the polarization contributed by Ti 4  ion and hence the dielectric constant is reduced to a low
value as compared to pure BNT. The relaxation temperature was not predicted in the present composite until
400qC. Therefore, the heavily zirconia doping suppress the formation of BNT phase and reduce the dielectric
permittivity value and increase the relaxation temperature.
24 ISRS-2008

4=4A6HC427=>;>6H
ET-O1
H OCCUPATION EFFECTS TO HYDROGEN STORAGE PROPERTIES
IN BOTH AB5 AND AB2-TYPES HYDROGEN STORAGE ALLOYS
Liang Yuan, Qing Wang, Hai-bin Wang, Chuang Dong
Dalian University of Technology

This paper investigates H occupations in both AB5 and AB2-type hydrogen storage materials, and also
analyses how different occupations effect hydrogen storage properties. H exists in both octahedron and
tetrahedron interstitial sites in hydrids of LaNi5(AB5), but only occupies tetrahedron interstitial sites in
hydrids of ZrV2. The enthalpy changes and lattice deformations of the cells are much different while H
occupies various interstitial sites. The hydrogen storage properties are determined by both enthalpy changes
and lattice deformations.

ET-O2
UNCONVENTIONAL LITHIUM INTERCALATION IN ACTIVE: INACTIVE
COMPOSITE CATHODE FOR LI RECHARGEABLE BATTERIES
Sivaprakash S. and Majumder S.B.
Indian Institute of Technology, Kharagpur, India

Intensive effort has been devoted to the synthesis of high energy density and stable positive cathode
materials for Li rechargeable batteries. For convention cathode such as lithium cobalt oxide, only about fifty
percent of theoretical capacity could be utilized due to the structural and chemical instability problem in deep
discharge. Capacity close to theoretical value could be achieved using unconventional lithium intercalation
in layered composite cathode. With aim to study unconventional lithium intercalation along with conventional
lithium intercalation in cathode material, layered composite cathode between two layered end members
Li2MnO3 and Li[Ni0.8Co0.15Zr0.05]O2 have been prepared by wet chemical route. The structural and
electrochemical properties of samples were investigated using XRD and galvanostic charge discharge
measurement respectively. X-Ray photoelectron spectroscopy has been used to investigate valance change
of transitional metal ion during extraction and insertion of Li+ to the cathode. The analyses indicate that Mn4+
ion in the novel cathode (with unconventional lithium intercalation) does not change its valance state even
after charging above > 4.6 V. further oxygen evolution during overcharging only meet the requirements of
excess lithium intercalation in this type of layered composite cathode.

ET-O3
COMPARATIVE STUDIES OF WATER UPTAKE AND PROTON
CONDUCTIVITY OF SPEEK AND SPEEK/PES BLENDS
Mahesh Arigonda, Abhijit P. Deshpande, Susy Varughese
Department of Chemical Engineering, Indian Institute of Technology Madras,India

Water uptake and proton conductivity are the important parameters to characterize a polymer
electrolytic membrane (PEM) for fuel cell applications. Membranes are prepared by blending sulfonated
poly (etheretherktone) (SPEEK) and poly (ether sulfone) (PES) using N-methyl-2-pyrrolidone (NMP) and
ISRS-2008 25

Dimethylacetamide (DMAc) as solvents. PES is added in the blend to decrease the water upake and optimize
the mechanical stability of the membrane. SPEEK membranes of different degree of sulfonation (DS) were
prepared. Blend membranes were prepared by using SPEEK of DS 71% with varying weight percentage of
SPEEK/PES (50/50 to 100/0). Water uptake, Ion Exchange capacity (IEC) and proton conductivity of the
blend membranes are characterized and a comparative study has been done with SPEEK.

ET-O4

STUDY OF TI-FE-V HYDROGEN STORAGE ALLOYS AND AN IDEAL


BCC SOLID SOLUTION STRUCTURE BASED ON
CLUSTER-PLUS-GLUE-ATOM MODEL
Hai-bin Wang, Qing Wang, Liang Yuan, Chuang Dong
Dalian University of Technology

This paper investigates the hydrogen-storage properties of (Fe4/13Ti9/13)100-xVx (x 10-50 at. %)


alloys which are designed by using our cluster line approach. These alloys are prepared by arc melting by
copper mould suction-casting (suction-cast) method. The hydrogen absorption and desorption measurements
indicate that the suction-cast BCC alloy (Fe4/13Ti9/13)50V50 possesses the optimum hydrogen absorption
capacity with the maximum hydrogen content of 3.46 wt. %. Furthermore, an ideal BCC solid solution
structure based on cluster-plus-glue-atom model is given.

ET-O5

DETERMINATION OF SAG IN GAS DIFFUSION


LAYER USED IN PEM FUEL CELL
Vijay R. and Prathap Haridoss
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

Gas Diffusion Layer (GDL) along with flow field plays the role of distributing the reactants uniformly
in the active area of the fuel cell. Carbon paper and cloth are the two different media that are commonly in
use as a GDL. These diffusion media sag in the fuel cell flow channels. Quantifying the sag becomes important
as affects the performance of the cell. This paper determines the sag in a diffusion medium quantitatively.

For sag measurement experiments flow field templates with channel width ranging from 1 mm, 2mm
and 3mm were machined. Experiments were conducted for both carbon paper and carbon cloth. The samples
were aged for 300 hours in two different environments. One in a humidity chamber at 60qC, 95% relative
humidity and other was in water at 60qC. Sag measurements were made by recording the micrographs of the
samples along with the template which gives the sag profile.

The results show that GDL sag occurs in the samples aged in liquid water, indicating that presence of
liquid water in the cell favors sag of diffusion medium. In comparison with carbon paper, carbon cloth exhibits
more sag. Increase in channel width increases in sag in all the cases tested.

The experimental procedure used to quantify the sag, and the implications of the results for fuel cell
technology development are discussed.
26 ISRS-2008

ET-P1
PREPARATION AND CHARACTERIZATION OF InTe
THIN FILMS FOR SOLAR CELL APPLICATIONS
Matheswaran P. and Sathyamoorthy R.
Kongunadu Arts & Science College, Coimbatore, India

III-VI semiconductor compounds have more attention due to its optoelectronic properties and finds
applications in solar cells, gas sensors, pressure transducers and IR detectors. InTe thin films were prepared
by sequential thermal evaporation of pure material at a pressure of 2 u 10 6m.bar. Structural, optical, surface
morphology and elemental composition of prepared films were analyzed by XRD, UV-Visible Spectra,
scanning electron microscopy and energy dispersive X-ray Spectroscopy respectively. Variation of band gap
energy with different film thickness and substrate temperature were discussed on the basis of phase transition
and defect formation. Optical studies reveals that the absorption co-efficient is very high and is effective in
visible region. Hence it is suitable for preparation of absorber layer in solar cells.

ET-P2
NOVEL GOLD-MANGANESE DIOXIDE-MULTI WALLED CARBON
NANOTUBE ELECTROCATALYST FOR PROTON EXCHANGE
MEMBRANE FUEL CELL
Imran Jafri R. and Ramaprabhu S.
Dept.of Physics, Indian Institute of Technology, Madras, India

Recently polymer electrolyte membrane fuel cells (PEMFC) have drawn considerable attention as a clean
energy conversion device due to its high energy conversion efficiency. The major challenge in the
commercialization of PEMFC is the cost of Platinum electrocatalyst and the effective utilization of the Pt. The
focus is the development of Pt-free electrocatalysts for the oxygen reduction reaction in PEMFC. In the present
paper, we report the synthesis of the gold-manganese dioxide nanocrystals supported on multi walled carbon
nanotubes (Au-MnO2/MWNT) and use of the same as electrocatalyst for oxygen reduction reaction in PEMFC.
MWNT have been prepared by the catalytic chemical vapor deposition technique and functionalized (f-MWNT)
using acid treatment. Au-MnO2 was dispersed on the surface of the f-MWNT by chemical method. The
as-prepared catalyst was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and
Transmission electron microscopy (TEM). Electrodes and membrane electrode assembly were prepared and
polarization measurements for single cell have been performed. The results indicate that Au-MnO2/f-MWNT
show good catalytic activity and stability for oxygen reduction reaction (ORR) in PEMFC.

ET-P3
PHOTOCATALYTIC HYDROGEN PRODUCTION FROM WATER USING
NOBLE METAL DOPED NANO TiO2
Kumaresan A., Prabhu L., Palanichamy M. and Murugesan V.
Anna University, Chennai, India

Photocatalytic water splitting into H2 and O2 using semiconductors as a photocatalyst has received
much attention, especially for its potential application to direct production of H2 for clean energy from water
utilizing solar energy. The photoelectrochemical effect of the semiconductor originates from the creation of
electrons and holes after absorption of light. Since the discovery of photocatalytic splitting of water in a cell
ISRS-2008 27

consisting of Pt and TiO2 electrodes under a small electric bias [1], the photoassisted production of hydrogen
and oxygen from water offers an extremely promising method for clean, low-cost and environmentally
friendly conversion of solar into chemical energy. Numerous efforts have been made for the construction of
efficient and practical systems in the production of hydrogen from water splitting reaction [2,3].Silver, Gold
and Platinum metal doped nano TiO2 were synthesised under sol-gel method. The presence of 100% anatase
phase was confirmed from XRD analysis. The synthesised materials are characterized by SEM, BET surface
area analysis, UV-vis DR spectra analysis. The presence of highly porous spherical like sphere was captured
from FESEM analysis. All the synthesised materials were tested for photocatalytic water splitting to generate
hydrogen under ultra violet and visible light irradiation.

ET-P4
CARBON NANOSTRUCTURES AS COUNTER ELECTRODE
MATERIAL FOR DYE SENSITIZED SOLAR CELL
Adarsh K., Arockiadoss T. and Ramaprabhu S.
Dept.of Physics, Indian Institute of Technology, Madras, India

Dye-sensitized solar cells (DSSC) are considered to be low cost alternatives for the conventional Silicon
solar cells. However, their efficiencies and long term stability still need to be improved upon, if they are to become
commercially viable. In DSSC, a thin film of Platinum coated on conductive glass substrate (ITO) is used as a
counter electrode material. However considering the cost and scarcity, Pt must be well utilized for the improvement
of performance. Recently, Carbon based materials such as carbon black have been employed as alternatives to Pt
with comparable efficiencies. Carbon nanotubes (CNT) and Graphene have excellent electrical conductivity and
are also excellent catalyst support materials. Hence, these materials seem to be good alternatives for Pt. However
better performance can be expected if we combine the properties of Pt and carbon based nanostructures. The
present work focuses on the investigation of increase in the efficiencies by the use of Pt nanocrystalline decorated
CNTs and graphene. MWNT have been synthesized by chemical vapor deposition technique and Graphene have
been synthesized by exfoliation of graphitic oxide, followed by functionalization using concentrated acid.
Pt-MWNT and Pt-f-graphene have been prepared by chemical method. DSSC have been fabricated and the
performances have been investigated. The results have been discussed and the role of Pt-MWNT and Pt-Graphene
as efficient counter electrode materials has been explored.

ET-P5
EFFECT OF CROSSLINKING DENSITY ON RHEOLOGY OF
CROSSLINKED POLY VINYL ALCOHOL/SSA
Kanakasabai P.
Indian Institute of Technology, Madras, India

Sol gel transitions are very important in materials processing. Gelation of crosslinking polymers is of
interest during polymer processing. The gelation reactions of poly vinyl alcohol (PVA) in the presence of
cross-linker sulfosuccinic acid (SSA) have been monitored through dynamic mechanical experiments.
Concentration of crosslinker (SSA) was varied from 0-30 wt %. The gel point (tg) for these chemically gelling
systems was determined. The dynamic storage modulus (G1) and loss modulus (G11) have been measured
for different cross-linker concentration. Stress relaxation measurements on gelling PVA systems were also
carried out. The structure of the network and the gel strength will depend on factors such as concentrations
and temperature. The frequency dependence of the viscoelastic properties at the gel point is an important
consideration. The gelation of PVA-SSA, which is an ionic polymer, will be compared with non-ionic polymer
such as PVA-glutaraldehyde.
28 ISRS-2008

5>A<8=6
FO-O1
TEXTURE AND MICRO STRUCTURAL EVOLUTION
OF PURE MAGNESIUM DURING ECAE
Somjeet Biswas, Satyaveer Singh D., Satyam Suwas
Indian Institute of Science, Bangalore, India

Initially hot rolled commercially Pure Magnesium having a basal texture was deformed by Equal
Channel Angular Extrusion (ECAE) in a 90q die following routes A and Bc. Texture and microstructure
evolution were studied using electron back scatter diffraction (EBSD) technique in a field emission gun (FEG)
scanning electron microscope (SEM). In addition to significant reduction in grain size, strong <0002> fiber
texture inclined at an angle ~ 45q from the extrusion axis formed in the material. Texture was also analyzed
by orientation distribution function (ODF) and compared vis-à-vis ideal shear texture. A slightly rotated B
and C2 fibers were observed after each ECAE pass. A significant amount of dynamic recrystallization
occurred during ECAE, which apparently did not influence the deformation texture.

FO-O2
STRETCH BENDING STUDIES OF SHEET METAL
– A NEW ATTEMPT USING RUBBER
Ganesh Niranjan G., Sri Harsha and Venugopal P.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

Bending of sheets assumes significant role in Sheet Metal Working besides deep drawing and cutting.
Bending is classified according to tool motion among which press brake bending is very popular. In V and
U bending of sheets in press brake, bending originates by moment and thus one finds what is called as “Free
bending force”. Free bending force is of academic interest only since, a major problem of spring back is
encountered. To correct the spring back, a simple die bending (of industrial importance) which applies a load
(varying in the range of 10 to 100 times the free bending force) is recommended. This die bending force has
its own attendant demerits – to cite a few, over stressing of the tools, possible breakage of “C” type press
brake, defeating the deformation efficiency (since losses vary as the square of the force) etc. Engineering
bending strain (under plane strain condition) is given as the ratio of thickness of sheet to twice the radius of
the tool. Thus, for a thin sheet bent over a large radius (such as aerofoil) the strain will be so small that, after
bending is done, large spring back is likely to be encountered. Stretch bending involves gripping the end
portions of the sheet by giving an initial small percentile load so that, the entire sheet is already in the plastic
stage. A form tool then plunges to generate the necessary shape. As the neutral axis is shifted away from the
plane of the sheet, the spring back is thus minimized or eliminated. This being the reason for evolution of
stretch bending, various designs for initial stretching the sheet followed. Such clamping tools and machines
involving many actions are very expensive.
The present work which is a preliminary attempt in nature, employs rubber of 85 shore hardness for
clamping to ensure initial stretching and then V bending is done up to the termination of the free bending.
By varying the layers of rubber (to ensure different initial stretching forces) and varying the V bending tools
(to ensure different bending strains) the bent aluminium samples are examined for their spring back. Spring
back with conventional conditions (without stretching) is compared with those obtained through stretch
ISRS-2008 29

bending. The optimal conditions for minimal spring back by stretch bending with rubber are examined. The
simplicity of the tooling using rubber for initial stretching and its host of advantages for industrial application
are contained in this paper.

FO-O3

ANALYSIS OF STRESSES IN HYDRODYNAMIC


DEEP DRAWING PROCESS
Uday kumar R.*, Ravinder Reddy P**. and Sitaramaraju A.V.
*
Dept.of Mechanical Engg. Mahatma Gandhi Institute of TechnologyGandipet Hyderabad, India
Dept.of Mechanical Engg. Chaitanya Bharathi Institute of Technology ,Gandipet Hyderabad, India
Dept.of Mechanical Engg. JNTU College of Engineering, Kakinada, India

A new method, named hydrodynamic deep drawing assisted by radial pressure is suggested in place
of the conventional hydrodynamic deep drawing process (HDD); where in the radial pressure is loaded along
the blank rim to reduce the drawing force. The radial pressure which is generated in the fluid due to punch
penetration in the fluid chamber is directed to the circumference of the blank to reduce the tensile stress
acting on the wall of the semi drawn blank. As a result of the combined effect of counter pressure and radial
pressure. High pressure fluid is directed to the peripheral surface of the blank through bypass holes. This
high pressure leaks out the blank and both the blank holder and the die. This creates a thin film of fluid on
both the upper and lower surfaces of the flange and subsequently reduces the frictional resistance. In this
phenomenon the shear stress of the fluid and viscosity is to be considered for evaluation of various parameters.
The optimum parameters were studied so that the flange wrinkling and fracture can be predicted and
controlled effectively. In this analysis radial stresses, hoop stresses and shear stresses along with the viscosity
are investigated and also these parameters effects with the geometry of blank and process parameters. These
investigations are obtained through theoretical analysis.

FO-O4

RING COMPRESSION TEST AND PLASTIC POISSONS


RATIO ON WARM EXTRUSION OF SINTERED POWDER
METALLURGICAL (P/M) PERFORMS OF STEEL
Chakravarthy P., Uday Chakkingal, Venugopal P.
Dept.of Metallurgival & Materials Engg, Indian Institute of Technology, Madras, India

A simple ring compression test had been carried out on sintered performs of steel at various resident
densities to assess the coefficient of friction. These tests were carried out at different temperatures and the
values of coefficient of friction were used for theoretical estimation of extrusion forces. The sintered preforms
were subjected to extrusion at different temperatures and the experimental forces required were recorded. A
comparison of the experimental values and theoretical values showed that the actual forces were greater than
calculated forces. The preforms were also subjected to compression test to analyze the plastic poissons ratio
at various resident densities at different temperatures. Some useful inferences with coefficient of friction and
plastic poissons ratios are discussed. The poissons ratios of resident preform densities and extrudes at different
temperatures were compared to characterize the enhancement in densities due to deformation and temperature
assisted sintering at warm working conditions.
30 ISRS-2008

FO-O5
COMPUTER AIDED MODELLING OF METAL FLOW
INVESTIGATION OF SQUARE BILLET TO SQUARE SHAPE
THROUGH BEZIER SHAPED CURVED DIES
Rout A.K. and Maity K.P.
National Institute of Technology, Rourkela, India
Extrusion plays a predominant role in the metal forming industry because of its improved mechanical
properties and higher productivity. It is usually noted that the extrusion is conventionally carried out with the
help of the shear faced dies. In these die metal is forced to go through a sudden change in cross-section
causing some practical problems such as formation of dead metal zone, non-uniformity in metal flow and
more redundant work, etc. To overcome these problems, extrusion dies are modified as streamlined extrusion
dies for smooth flow of material die. The present investigation has been done for the streamlined extrusion
dies designed based on a Bezier die profile. The velocity components and strain rates along x, y, and z
directions are determined by upper bound method using dual stream function. The velocity components and
strain rate of metal flow along x, y and z directions are determined in the dead metal zone. It is observed that
the velocity components Vx, Vy and Vz as well as strain rate components (both direct and shear) vary along
the die length. The variations are plotted with respect to non-dimensional die length for different reductions
and friction factors.

FO-O6
CHANGES IN DEFORMATION TEXTURE AND PLASTIC
ANISOTROPY WITH TEMPERATURE FOR AA6016
Manojit Ghosh1,2, Alexis Miroux1, Jurij Sidor1, Leo Kestens2
1
Materials Innovation Institute, Delft, Netherlands
2
Delft University of Technology, Delft, Netherlands
The use of aluminium alloys in automotive industry is restricted because of poor room temperature
formability in spite of their high strength to weight ratio and corrosion resistance. Tensile, plane strain
compression and deep drawing tests have been performed to investigate the forming behaviour of AA6016
alloy at room temperature and 250qC. It has been observed that temperature significantly influences the
plastic anisotropy of the sheets apart from expected reduction of yield strength. The earing profile of drawn
cups show a four-fold symmetry after drawing at room temperature and the r-value is minimum along a
direction at 45q from RD. At higher temperature the earing profile changes to 2-fold symmetry and the r-value
is minimum along RD. It has been noticed that texture changes after plane strain compression and deep
drawing compared to as-received texture but the effect of temperature is negligible on textural changes. The
experimental R-value and textures are well predicted by the VPSC model using {111}<110> slip system at
room temperature and {111}<111>, {110}<110> and {100}<110> slip systems at 250qC.
ISRS-2008 31

FO-P1
ANALYSIS OF ROUGHNESS AND FLANK WEAR IN TURNING GRAY
CAST IRON USING CRYOGENICALLY TREATED CUTTING TOOLS
Ramji B.R., Narasimha Murthy H.N. and Krishna M.
R.V. College of Engineering, Bangalore, India

The purpose of this research was to examine the surface roughness, flank wear in turning gray cast
iron using cryogenically treated inserts. Turning experiments were conducted with cutting velocities: 53, 85,
99, 149 m/sec, feeds: 0.12, 0.16, 0.2, 0.24 mm/rev and a constant depth: 1.5 mm. The specimens were turned
using cryogenically treated and non-treated carbide inserts. The cryogenic treatment cycle consisted of
cooling the test samples from room temperature to cryogenic temperature(–178.9oC) in three hours, soaking
at cryogenic temperature around 24 hours and warming to room temperature in about five hours. The surface
roughness (Ra, Rz, Rq and Rt Pm) of the cast iron surface was measured using talysurf and flank wear of the tool
was measured using toolmakers microscope. The experimental lay-out was designed based on Taguchi’s
Orthogonal Array technique and ANOVA was performed to identify the effect of the parameters on the response
variables. Cryogenically treated inserts proved superior to the non-treated in all the test conditions in terms of
lesser flank wear of the inserts and reduced surface roughness of the specimens. The after turned inserts were
examined using Scanning Electron Microscopy for studying the flank wear mechanism.

FO-P2
TEXTURE AND MICROSTRUCTURE EVOLUTION IN
INTERSTITIAL-FREE STEEL WIRES PROCESSED
THROUGH EQUAL CHANNEL ANGULAR EXTRUSION
Suresh K.S, Fundenberger J.-J. and Satyam Suwas
Indian Institute of Science, Bangalore, India

Interstitial Free Steel (IF Steel) wires were drawn at room temperature from samples annealed at 1023 K for
3Hr as well as from Equal Channel Angular Extruded (ECAE) material at 573 K. Texture evolution was analysed
both by X-ray diffraction as well as Electron Back Scattered Diffraction (EBSD). Further, the changes in Grain
Boundary Character Distribution (GBCD) of the samples during different routes are also reported. Significance of
Strain Path Changes (SPC) during wire drawing from different routes on grain refinement and texture was examined.
Torsion properties of the processed wires with different numbers of ECAE passes were compared.

FO-P3
FAILURE ANALYSIS OF SUPERPLASTIC FORMING / DIFFUSION
BONDING PROCESS (SPF/DB) ON ALUMINIUM ALLOYS DURING
EXPERIMENTATION
Ganesh P., Senthil Kumar V.S., Natarajan S., Kalaichelvan K.K.
Madras Institute of Technolgy, Anna University,Chennai, India

Superplastic forming is a high temperature deformation process where neck free elongations of over
400% at low applied stress, half the melting point and low strain rate of about 10 5 to 10 3 s-1are formed.
Diffusion bonding is a solid state bonding process capable of joining wide range of metals. During recent
32 ISRS-2008

years SPF/DB is applied in fabricating complex parts has increased in the automobile and aircraft industry.
The purpose of this research work is to analyze the formability of hemispherical bonded shaped part, reduce
cost, weight and tooling. This work focuses on Chronological change in dome height of the formed
component, thickness distribution and bonding two sheets of different thickness using SPF/DB process for
a hemispherical shape under controlled conditions. The controlled parameters were forming time,
temperature and applied pressure. The experiment was carried out for different combinations of pressure,
temperature and time and the forming height and bonding thickness were observed. A continuous trial by
varying the parameters, uniform bonding and complete hemispherical forming was achieved by appropriate
pressure, temperature and time. The responses such as forming height and bonding thickness were analyzed
using ABAQUS.

FO-P4
EXPERIMENTAL STUDIES ON THE SUPERPLASTIC FORMING OF
Ti-6Al-4V SHEET METAL INTO SQUARE SHAPED CUPS
Rayudu R.K., Bhattacharya S.S., Deepkumar V.P.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

Superplasticity is the ability of a polycrystalline material to exhibit, in a relatively isotropic manner, large
elongations when deformed in tension. This property is exploited during superplastic forming in the fabrication
of complex-shaped components which are otherwise technically difficult or economically costly to form by
conventional methods. The ability of some titanium alloys to undergo superplastic deformation coupled with their
diffusion bonding capability provides excellent opportunities to fabricate intricate parts in one operation resulting
in significant cost and weight savings, particularly in the manufacture of aerospace structures.
In the present work, experimental studies to characterize the superplastic behavior of an as-received
titanium Ti-6Al-4V alloy sheet metal commonly used in aerospace structural applications are reported. The
raw material sheet metal stock was characterized for the chemical composition and room temperature
mechanical properties. The raw material was also subjected to tensile tests under superplastic conditions to
confirm its ability to undergo superplasic deformations. Suitable dies, for superplastic forming of 80 mm u
80 mm square and 50 mm deep cup specimens, were designed and fabricated including die inserts which
facilitated the forming of square cup specimens of different depths. Alloy sheet specimens were
superplastically formed at a temperature of 1200qK (927qC) and 0.7 MPa constant pressure to different
depths. The superplastic forming rates were monitored throughout the process. The superplastically formed
components were characterized for their thickness distribution, mechanical and metallurgical properties.

FO-P5
EFFECT OF PROCESSING ROUTES ON MATERIAL FLOW AND STRAIN
INHOMOGENIETY IN EQUAL CHANNEL ANGULAR PRESSING
Patil Basavaraj V., Uday Chakkingal and Prasanna Kumar T.S.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

Investigations are currently focused on Equal Channel Angular Pressing (ECAP) because of its
potential to produce ultra fine-grained microstructures in metals and alloys. Ultra-fine materials exhibit
superior mechanical properties such as high strength and ductility. Many parameters contribute to the
inhomogeneity in the resulting work-piece. Among other process parameters the processing route has great
ISRS-2008 33

influence on the distribution of strain and resulting inhomogeneity in the work-piece. This influence can be studied
by Finite Element Modelling. In the present work 3D Finite Element Modelling of ECAP process was carried
out using the ABAQUS / Standard software for four passes in routes A, B and C.A cylindrical work-piece of
diameter 20 mm and length 105 mm was considered. Channel intersection angle was 105 degree. Strain hardening
behaviour of Aluminium alloy AA 6101 was used. Strain obtained from the previous pass was given as initial
condition for the subsequent pass. The results presented are useful for understanding the effect of processing
routes on the material flow and the strain distribution. It is also useful for selection of the best route.

FO-P6
STRAIN HARDENING BEHAVIOUR OF WARM ECAP PROCESSED Cp-Ti
Preetham Kumar G. V. and Uday Chakkingal
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India
Superior properties for structural applications of CP-Ti can be attained through multiple passes of equal
channel angular pressing (ECAP). ECAP is a procedure which involves large simple shear plastic deformation
without a resultant change in cross sectional area. In the present study, the specimens of CP Ti were extruded to
three passes through an ECAP die with 17mm diameter and an angle of 120o between the two intersecting
channels. All the equal channel angular pressings were carried out at 400oC. Compression and tensile tests were
conducted on the specimens subjected to different passes. The strain hardening behaviour of the CP-Ti material
was evaluated as a function of the number of passes from the compression test data. Significant strengthening and
grain refinement were observed. The variation of strain hardening rates were calculated as a function of the applied
strain and this was correlated to the microstructure developed during ECAP.

FO-P7
EFFECT OF MICROSTRUCTUAL AND MECHANICAL PROPERTIES
OF Al 2014 ALLOY PROCESSED THROUGH ROUTE A AND BA
Venkatachalam P., Ravisankar B., Thamos Paul*V., Vijayalakshmi*M. and Kumaran S.
Department of Metallurgical and Materials Engineering, National Institute of Technology, Tiruchirappalli, India
An Al 2014 alloy has been subjected to equal-channel angular pressing up to five passes by routes A,
and BA in a die with channel angle I 90q and corner angle \ 20q. Microstructural and mechanical
properties were compared for three different conditions namely (i) as received, (ii) solutionized at 768 K for
1 hr and (iii) solutionised at 768 K for 1 hr  aged at 468 K for 5 hr. Microstructural characterization was
done using TEM and mechanical properties were evaluated by micro hardness and micro tensile test. The
improved strength and hardness of ECAPed 2014 Al solutionised at 768 K for 1 hr  aged at 468 K for 5 hr
alloy was due to the precipitation hardening, grain refining and higher dislocation density. However, no
significant differences in tensile strength and hardness were found between the samples processed through
route A and BA.
34 ISRS-2008

9>8=8=6B>;8385820C8>=

JS-O1

OPTIMIZATION OF ZONE REFINING IN PREPARING


GALLIUM EXCEEDING 7N PURITY
Ghosh K., Mani V.N., Dhar S. and Balaraju K.
Dept of Electronic Science, University of Calcutta, India

Computer simulation was carried out to optimize zone refining process parameters such as zone length
and zone travel rate on the impurity concentration profile in the zone refined material ingot. Simulation study
was also used to ascertain the number of passes required to reach the ultimate distribution, which is the
attainment of steady state at which no more reduction in impurity concentration takes place. It was also
studied that stirring of the molten zone produced in the material undergoing the refining process will cause
improvement in impurity segregation enabling higher material purity. Based upon the optimization carried
out through simulation, experiment was conducted to purify gallium by a laboratory scale two-heater vertical
zone refiner and a three-zone (hot, gradient and cold zone) Directional Freezing system. After conducting
50 zone refining passes on the starting 5N2 (99.9992% pure) gallium, the refined metal was placed in the
Directional Freezing system where it is rotated at 20-35 rpm for effective stirring of the gallium melt. Gallium
was purified up to 7N2 (99.999992%) purity as analyzed by Glow Discharge Mass Spectrometry (GDMS).
The total impurity concentration with respect to 24 impurities in gallium namely, Al, Cu, Ca, In, Ni, Si, As,
Cd, Fe, Mg, P, Sn, Au, Co, Ge, Mn, Pb, Te, B, Cr, Hg, Na, S and Zn were reduced from 7764 ppb to less than
77.7 ppb with an overall impurity concentration reduction efficiency of 99%. The details of instrumentation
difficulties and modifications are discussed.

JS-O2

STUDIES ON Ti-15V-3Cr-3Sn-3Al (Ti-15–3) METASTABLE-BETA


TITANIUM ALLOY WELDMENTS
Balachandar K., Sarma S., Bhanu Pant, Phanikumar G.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

In this work, an attempt has been made to understand the weldability of Ti-15V-3Cr-3Sn-3Al alloy.
GTAW- DCEN with optimized argon flow in the torch, trailing and backup to reduce the oxidation was utilized
to weld samples. Continuous current and pulsed current with variable frequencies were experimented.
Thermal history of the welds was studied using in-situ temperature measurements. Single step post weld
aging of the welded samples were tried to achieve optimum microstructural properties. Pulsed current
technique was effective in reducing the grain sizes as well as the width of heat affected zone. Sub transus
ageing resulted in allotriomorphs along the grain boundary and lenticular D network along the grains, with
predominant compositional variation between the E matrix and D laths.
ISRS-2008 35

JS-O3
EFFECT OF BORON ADDITION ON THE GRAIN REFINEMENT OF
Az91 (Mg-9Al-1Zn-0.2Mn) MAGNESIUM ALLOY
Suresh M., Srinivasan A., Pillai U.T.S.* and Pai B.C.
Materials and Minerals Division, National Institute for Interdisciplinary Science & Technology (CSIR),
Thiruvananthapuram, India

Exploitation of magnesium alloys have been increased significantly in the automotive industry because
of their great potential in reducing the weight of the components thus resulting improvements in fuel
efficiency of vehicles. Among the various Mg alloys, AZ91 alloy has the best combination of castability,
mechanical strength and ductility. These excellent properties have made AZ91, as the most preferable
magnesium alloy for the production of light weight automobile components. The performance of the
components made by AZ91 alloy can be improved further by increasing its tensile properties, particularly,
its yield stress. As it is well established that the yield strength is directly related with the grain size, it is
essential to reduce the grain size of the cast alloy to a maximum extent to get a higher tensile properties.
It is well known that grain refinement can be achieved in the castings by several methods like faster
solidification, melt agitation, solute additions, etc. Due to simplicity and efficiency, solute addition as a grain
refiner has become more popular in casting industries. Generally, the grain refinement of Mg-Al alloys is
achieved by introducing any of these additives such as Sr, RE, Th, Si, Ca, AlN, etc. into the melt. In the present
study, the grain refinement efficiency of boron in Az91 alloy is investigated. Boron addition (0.01 to 0.2 wt
%) is carried out to Az91 using Al-4B master alloy and its effect and mechanism of grain refinement studied
is reported.

JS-O4
GRAIN REFINED BORON MODIFIED Ti-6Al-4V ALLOY:
ROLE OF Ti-B COMPOUND IN TEXTURE EVOLUTION
Shibayan Roy
Laboratory for Texture and Related Studies, Dept. of Materials Engineering, Indian Institute of Science,
Bangalore, India

Owing to their high strength-to-weight ratio, excellent mechanical properties and corrosion resistance,
titanium (Ti) and its alloys, especially (alpha+beta) alloys like Ti-6Al-4V, are the backbone materials for
aerospace, energy, and chemical industries. Pure titanium has hexagonal (alpha) crystal structure at room
temperature, which transforms to bcc (beta) structure at ~885qC following specified orientation relationship.
Based on this orientation relationship and the symmetries of cubic and hexagonal structures, a total of 12
phase can result from theDcrystallographically distinct variants of grain. The basis for tailoring a
suitableEtransformation of single texture and microstructure during heat treatment of titanium alloys,
therefore, depends strongly on the E to D transformation. The same is applicable for (alpha+beta) titanium
alloys.Trace boron addition (~0.1 wt. %) to the alloy Ti-6Al-4V produces a reduction in as-cast grain size by
roughly an order of magnitude. Special attributes of Boron addition includes enhanced ductility, higher
stiffness and strength in addition to good fracture resistance. Recently, Ti-alloys have been produced by
Induction skull melting (ISM) technique, which offers number of advantages in terms of improved ingot
quality. Boron addition as well as ISM technique could affect the evolution of texture and microstructure in
the material. A research program has been developed in order to study different aspects of texture evolution
36 ISRS-2008

in ISM processed Boron modified Ti-6Al-4V.The solidification microstructure of Boron free as well as Boron
containing Ti-6Al-4V after ISM processing are found to be almost homogeneous from periphery towards the
center of as-cast ingot in terms of both D-colony size and distribution. Boron addition substantially reduces
D-colony size (~50-80 Pm). Needle shaped Ti-B particles texture fromsegregate at the grain boundary. A
gradual change in periphery towards the center has been observed with orientations close to specific texture
components suggesting the formation of texture zones. The mechanism of texture evolution can be visualized
as a result of variant selection during solidification through (alpha+beta) phase field. A fine observation using
local area EBSD scans with very small step size supports the above preposition.

JS-O5
MELT RHEOLOGY OF BRANCHED POLYLACTIC ACID
Deenadayalan E., Naveen R., Lele A.K. and Balasubramanian M.
Indian Institute of Technology Madras, India

Polylactic acid (PLA), a biodegradable polymer which can also be produced from annually renewable
resources, has recently gained growing attention. Branching and crosslinking of polylactic acid was carried
out in a Haake batch mixer using varying percentages of 2, 5-dimethyl-2, 5-di-(t-butyl peroxide) (Lupersol
101) and a multifunctional epoxy based additive. Based on the extrusion temperature and the relative content
of peroxide/epoxy, branching, crosslinking, and chain scission can occur separately or simultaneously. The
total degree of branching (short and long chain branching) was determined by 13C NMR spectroscopy. Gel
content was determined by Soxlet apparatus. The rheology of linear and modified poly (lactic acid) was
investigated in shear and uniaxial extensional modes. Time sweep experiments were performed on these
samples at different temperatures to test the melt stability. Influence of branching and crosslinking on melting
temperature and glass transition temperature was studied by using differential scanning calorimetry.

JS-P1
DIFFUSION BONDING OF Ti-6Al – 4 V WITH INCONEL
718 WITHOUT AND WITH INTERLAYERS
Krishnamoorthi J., Balusamy V., Angelo P.C., Ravisankar B.
PSG College of Technology, Coimbatore, India

Joints of titanium alloys with super alloys have wide applications like aerospace engine parts and fuel
tanks. Joining of these materials by conventional welding processes fails due to the formation of number of
intermetallics resulting embrittlement. Solid state diffusion bonding can minimize the structural
in-homogeneities and assures sound bond. Diffusion bonding is the joining of two nominally flat surfaces
by the action of temperature and pressure. In order to avoid fusion, the temperature is chosen less than the
absolute melting temperature of the lower melting point material. Bulk plastic deformation is avoided by
keeping the bonding pressure well below the yield stress of the materials. The bond strength of the diffusion
bonded joints can be further improved by inserting suitable material in between the two metals as interlayer.
The present investigation attempts were carried out to bond Ti-6Al-4V with INCONEL718 without any
interlayer and with interlayers like nickel and tantalum foils. The experiments were performed using specially
constructed diffusion bonding set-up with varying process parameters viz temperature from 500 to 900qC,
bonding pressure from 2 to 10MPa and time from 1 to 5hrs. The relative importance of the process parameters,
the mechanism(s) responsible for bonding and the joint characteristics were analysed by optical & electron
microscopy and hardness survey across the interface. Energy Dispersive Spectroscopy analyses were also
ISRS-2008 37

carried out to understand the elemental distribution across the interface of the joints. The optimum process
parameters for the perfect bonding of Ti-6Al-4V with INCONEL718 without and with interlayers were
identified using the above test results. The influence of interlayer metals and the corresponding bonding
conditions on the Ti-6Al-4V with INCONEL718 joints was also investigated.

JS-P2

EFFECT OF METAL-MOLD INTERFACE HEAT FLUX DISTRIBUTION


ON MACRO SEGREGATION AND MICROSTRUCTURE
DURING GRAVITY DIE CASTING
Sreenivas Rao K.V., Phanikumar G. and Prasanna Kumar T.S.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

Experiments were conducted to study the effect of interfacial air gap formation on microstructure and
macro segregation of die-cast Al-4.5%Cu alloy. An experimental method which involved mold filling was
designed to accurately capture the thermal histories of the mold and casting. An IHCP algorithm was used
to estimate multiple heat flux components at the metal-mold interface. The estimated heat flux values show
a spatial variation along the vertical length of the mold. The analysis indicates that the non-uniform air gap
formation at the metal-mold interface leads to spatial variation of interface heat flux. The spatial variation
of interface heat flux gives rise to spatial variation of microstructure and macro segregation. Fine grained
columnar structure was observed at the bottom of the casting near the mold wall whereas; coarse grains were
seen towards the top of the casting. The copper content decreases from bottom to top near the mold wall.

JS-P3

INFLUENCE OF GATING SYSTEM ON MICROSTRUCTURE


AND MECHANICAL PROPERTIES OF MELT AND HEAT TREATED
CAST Al-7Si-0.35Mg ALLOY
Swamy N.H.S., Ravi Naika, Josepha M.A., Nagarajan N.M. and Sateesh N.H.
National Institute Of Technology Calicut, India

In the present investigation the effect of low frequency mould vibration and the influence
heat-treatment parameters on microstructure and mechanical properties of modified cast Al-7Si-0.35Mg wt.
% alloy in different sand moulds with two different runner designs/systems are studied. The microstructure
and mechanical properties of the alloy are found to be affected significantly by the combined effect of mould
vibration and heat treatment in all the cases. Heat treatment produces greater refinement, uniform silicon
distribution and formation of spheroids. Scanning electron microscopy of tensile fractured surface reveals
the influence of vibration and solution temperature on the mode of fracture. Among the different sand systems
used in the investigation, castings from dextrine chromium trioxide no-bake system sand mould yield castings
with better mechanical properties. A comparison of the influence of different moulds with two different runner
designs with vibration on the tensile strength of the alloy has shown that filtered rectangular runner (FRR)
yield castings with higher and more reliable tensile strength than the unfiltered vortex flow runner (UVR)
system.
38 ISRS-2008

JS-P4
CONTINUOUS DRIVE FRICTION WELDING OF INCONEL 718 – EN24
DISSIMILAR METALS: EFFECT OF PRE-HEAT TREATMENT
Sree Vardhan Lalam, G. Madhusudhan Reddy, T. Mohandas, Kamaraj M. and Murty B.S.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India

The microstructure and mechanical properties are compared for continuous drive friction welded
Inconel 718 and EN24 dissimilar joints, in four different combinations of pre-weld heat treatment conditions.
The dissimilar welds exhibited low strength and low toughness in all the combinations. The welds made with
Inconel 718 in solutionized condition resulted in formation of wide HAZ in EN24 than welds made with
Inconel 718 in annealed condition. At the weld interface diffusion of Fe from EN24 into Inconel 718 was
observed for the welds made with EN24 in annealed condition and diffusion of Ni, Cr. Mo and Nb from
Inconel 718 into EN24 was observed in welds made with EN24 in Q&T condition. The observed trends in
mechanical properties are explained in relation to microstructure, fracture behaviour, EPMA, EDS and XRD.

JS-P5
EXPERIMENTATION, FEM AND STATISTICAL ANALYSIS FOR
PARAMETER OPTIMIZATION IN MIAB WELDING PROCESS
Arungalai Vendan S., Nagamani C., Manoharan S. and Buvanashekaran G.
National Institute of Technology, Trichilapalli

The magnetically-impelled arc butt welding process (MIAB) is a solid state joining technique that uses
arc heating of the components to be joined, the arc being struck between two tubular components, and then
magnetically rotated rapidly around the circumference. The arc disrupts the surface oxides and softens the
interfacial material without necessarily melting it, and the components are then forced together to forge out
those oxides and leave only clean material in the joint. MIAB can reduce welding time by up to 90%, cut out
the need to rotate components and weld circular or non-circular components with the same ease. Any angular
orientation can be welded. The process can be used to weld steels, stainless steel, aluminum alloys, etc. In
this study, a laboratory MIAB welding module is designed and developed. Experimental trails are conducted
to achieve the arc rotation by varying the input parameters. Further, finite element analysis is performed for
determining the distribution of various parameters across the joint that governs the MIAB welding process using
finite element code ANSYS. In addition, Statistical analysis is performed to determine the most significant
parameter that governs the arc speed in MIAB welding. The results emphasizes that the welding current and
magnetic coil current importantly governs the arc rotation and also has a linear relation with the arc speed.

JS-P6
DISSIMILAR ELECTRON BEAM WELDING OF MARAGING STEEL
MDN 250 TO HIGH STRENGTH LOW ALLOY STEEL AIR 15CDV6
Venkateshwara Rao V., Madhusudhan Reddy G. and Sitaramaraju A.
JNTU, Hyderabad, India

Recent advances in manufacturing processes using electron beam welding have led to increased use
of advanced and dissimilar materials. Dissimilar metal joints are widely used in various industrial applications
due to both technical and economical reasons. The adoption of dissimilar metal combinations provides
ISRS-2008 39

possibilities for flexible design of the product by using each material efficiently i.e., befitting from specific
properties of each material in a functional way. In the aerospace scenario, ultra high strength steels such as
18% maraging steel (MDN 250) and low carbon low alloy Cr-Mo-V steel (AIR 15CDV6) are widely used
in the fabrication of various critical components.
As there is a considerable difference between the costs of materials MDN 250 and AIR 15CDV6 steel,
one of the ways to reduce the total fabrication cost of the component as well as taking the advantageous of
the specific properties of each of them by adopting a dissimilar metal joining. The data on characteristics
dissimilar metal weldment will be extremely beneficial to the designers to generate a cost effective design.
In the present work MDN 250 is welded to 15CDV6 material by using electron beam welding process. The
study consists of mechanical property evaluation such as tensile, impact and hardness coupled with
microstructural examination. Influence of post weld heat treatments also forms part of the study. The post
weld heat treatments investigated are quenching and tempering treatment i.e., employed for low alloy steel,
post weld ageing at 4800C and post weld solution treating and ageing which is adopted for maraging steel.
Maraging steel welds exhibited lower tensile strength and toughness compared to as received solution
treated parent metal. Post weld ageing, post weld solutionizing and ageing further reduced the impact
toughness, due to precipitation hardening. However, quenching and tempering treatment similar to that
employed for the low alloy steel, which does not involve precipitation hardening experienced marginal
reduction in toughness from the as-welded condition. AIR 15CDV6 welds exhibited low strength and
toughness compared to parent metal. The strength could be improved by quenching and tempering treatment.
In tensile testing, all the failures of dissimilar welds are located outside the weld region.
Dissimilar welds exhibited low strength, low toughness compared to respective parent metal. Post weld
heat treatment resulted in further reduction in toughness compared to that in the as-welded condition. Impact
toughness of dissimilar weldments is higher than similar welds. The observed mechanical properties are
correlated with microstructure and fracture features. The study assumes special significance as studies on
these aspects are not reported hitherto our knowledge.

JS-P7
FRICTION WELDING OF AZ91D MAGNESIUM ALLOY
Govindaraju M., Prasad Rao K., Uday Chakkingal, Balasubramanian K.
Dept.of Metallurgical & Materials Engg, Indian Institute of Technology, Madras, India
Magnesium alloys, one of the lightest commercially used alloys, have poor weldability by fusion
welding. Among that, AZ91C and D (Mg-9%Al-1%Zn) are work horse magnesium alloys, in which AZ91D
has superior corrosion resistance. In this study, AZ91D magnesium alloy was subjected to friction welding
in various conditions like as cast and fully heat treated. For friction load of 45 MPa and upsetting load of 90
MPa, sound joints with joint strength more than base metal were obtained. Welded microstructure reveals
that that the grain size is refined in the weld region, and the porosity is eliminated/ minimized. All the
experiments were carried out by using 15mm diameter samples. When the upsetting load exceeded 90MPa
(1.6 ton), the samples started buckling. Welding speed was optimized in between 700 and 1100 rpm, where
below 700 rpm joint strength was inferior to base metal and more than 1100 rpm joints became more brittle.
40 ISRS-2008

<4270=820;1470E8>DA8

M1-O1
EFFECT OF GROOVE AT CONTACT EDGE
ON FRETTING FATIGUE BEHAVIOR
Jayaprakash M., Kimura N., Mutoh Y. and Yoshii K.
Nagaoka University of Technology, Nagaoka, Japan

Fretting fatigue is a serious problem in engineering applications, where two components are in contact and
subjected to cyclic loading. In fretting fatigue, the fatigue strength degradation is due to the high stress
concentrations at the contact edge created by fretting action. If stress concentrations at the contact edge are reduced
then, fretting fatigue strength may be improved. Many research works have been published regarding decreasing
the stress concentrations by applying surface coatings and lubricants. But these methods found to be ineffective
in some critical applications. Recently it has been reported that one of the effective method to reduce the stress
concentrations at the contact edge is by modifying the specimen design by making stress relief grooves at the
contact edge. But the major drawback in this method is the increase in stress concentration at the groove root, so
possibility of failure may occurs at the groove root. It is necessary to optimize the groove dimensions to achieve
the maximum improvement in fretting fatigue strength by making stress relief grooves.
In the present work the effect of groove, groove shape at contact edge on fretting fatigue behavior in
an automobile steel was studied by performing fretting fatigue tests of specimens with grooves of different
groove dimensions at the contact edge. From the result it was identified that the groove at the contact edge
has a significant effect on fretting fatigue strength. Finite element analysis was performed to evaluate the
stress distribution around the contact and groove. The experimental results obtained were discussed based
on the stress distribution around the contact and groove.

M1-O2
MICROSTRUCTURE AND MECHANICAL PROPERTIES OF 16Cr-2Ni
STAINLESS STEEL ELECTRON BEAM WELDS-INFLUENCE OF
SINGLE AND DOUBLE AUSTENITE
Rajasekhar A., Madhusudhan Reddy G. and Mohandas T.
University College of Engineering, Osmania University,Hyderabad, India

The influence of single and double austenitizing treatments on microstructure and mechanical
properties of electron beam welds of AISI 431martensitic stainless steel were studied. The post weld heat
treatments consist of austenitizing the weld samples for one hour at 10000C, 10500C, and double austenitized
at 10500C  10000C and air cooling followed by double tempering i.e., tempering at 6700C  6000C. The
prior austenite grain size increased with increase in austenitizing temperature from 10000C to 10500C. Grain
refinement resulted after double austenitization. Parent metal grain size was coarser as compared to grain
size in the weld zone in respective conditions. Retained austenite content increased after double
austenitization. Presence of undissolved carbides was observed in welds and parent metal austenitized up to
10000C and they dissolved at austenitizing temperature t 10500C. Double austenitization (DA) treatment
resulted in dissolution of most of the carbides. Coarsening of martensite laths was observed after tempering.
Double austenitization (DA) after double tempering resulted optimum mechanical properties i.e., strength,
hardness and toughness.
ISRS-2008 41

M1-O3

FLEXURAL FATIGUE BEHAVIOR OF LONG TERM EXPOSED


NYLON 66 TO MOISTURE
Timmaraju V. Mallina, Gnanamoorthy Rajappaand, Krishna Kannan
Machine Design Section, Dept.of Mechanical Engg, Indian Institute of Technology, Madras, India

Aim of present study is to understand the effect of water content absorbed during the long term exposure
to different surrounding environments on fatigue behavior of nylon 66 under 50% and 100% relative humidity
conditions. Injection moulded nylon 66 samples of 4 mm thick are conditioned in water under ambient
conditions to get varied weight percentage of water content till saturation. Flexural fatigue tests are performed
under displacement control using a specially developed compact close controlled fatigue test rig at a
frequency of 2 Hz. Initial set of experiments are conducted under ambient conditions of 28qC and 50% relative
humidity and later are conducted under 28qC and 100% relative humidity conditions to distinguish the nature
of fatigue experienced by the specimens containing same weight percentage of moisture in different test
environments. Two extreme natures are observed when dry samples (< 0.2%) tested in 50% RH and saturated
samples tested in 100% RH for a particular displacement amplitude. Dry specimens tested in 50% RH
experienced severe cyclic softening while temperature of the specimen is rising with very high approximate
initial stress amplitude of 65 MPa. Saturated specimens tested in100% RH experienced no cyclic softening
during the test with extremely less stress amplitude of 20 MPa on average due to severe plasticization upon
water absorption. Dry specimens in 50% RH are influenced by Tg as well during the test and experienced
fatigue failure with smooth regular striations on fracture surface. A very high fatigue life is observed for
saturated samples due to plasticization effect of water which results in very low induced stresses.

M1-O4

MICROSTRUCTURAL EFFECTS ON THE MECHANICAL BEHAVIOR


OF BORON MODIFIED Ti-6Al-4 V ALLOYS
Indrani Sen and Ramamurty U.
Indian Institute of Science,Bangalore, India

Conventionally cast Ti-6Al-4V alloy possesses coarse grain size of several mm. Extensive and
expensive thermomechanical processing is needed to refine the structure. However, small amount of B
additions (< 1 wt.%) refine the as-cast grain size by an order of magnitude, hence improve their mechanical
performance. In this work, we report the effect of microstructural refinement, achieved through systematic
B additions from 0.0 up to 0.55 wt.% B on the mechanical behavior of as cast Ti64 alloys. These include
tensile properties, fracture toughness as well as un-notched and notched fatigue strength and crack growth
respectively. Experimental results show about 10 % increment in the tensile strength due to microstructural
refinement. However, a gradual reduction in threshold for fatigue crack initiation is noticed depending on
the square root of the microstructural length. Stress-controlled high-cycle-fatigue experiments reveal an
enhancement in the endurance limit of the alloy with B addition, primarily due to the microstructural
refinement. However, intermetallic TiB formed due to B addition, affects the crack initiation. The
strain-controlled low-cycle-fatigue shows variation of the degree of cyclic-softening and
tension-compression asymmetry with B addition.
42 ISRS-2008

M1-O5

EFFECT OF PROCESS VARIABLES ON STRUCTURE AND


PROPERTIES OF Al-Si-Mg ALLOYS
Siddalingaswamy N.H., S.Raghavendra Kumar, Joseph M.A., Nagarajan N.M. and Sateesh N.H.
National Institute of Technology, Calicut, India

Among the different variants under Al-Si alloy system, Al-Si-Mg alloy has received wider acceptance
in aerospace and allied industries particularly owing to its high strength to weight ratio, good machinability
and corrosion resistance. Many researchers and material scientists have been endeavouring over the past four
decades, for effective process variations towards achieving improved mechanical properties of this alloy. This
paper presents the results of investigations carried out on the effects of heat treatment in cast alloys, on major
mechanical properties such as tensile strength, ductility and hardness. Al-Si-Mg alloys with 7, 12, 16 %Wt.
silicon and cast with modification, combined modification & vibration and heat treatment were tested
adopting standard testing procedure have been compared. Samples cast with modification, vibration during
solidification and heat-treated exhibit relatively better mechanical properties. Optical microscopy study of
these samples show enhanced Spheroidisation and uniform distribution of eutectic silicon crystals particularly
at higher solutionising temperature. Scanning Electron microscopy slides clearly indicate while modified
alloys show predominantly cleavage fractured surface and modified and vibrated alloys a mixture of cleavage
and dimple fractured surfaces, samples with modification, vibration and heat treatment exhibit predominantly
dimple fractured surface.

M1-P1

EFFECT OF PARAMETERS ON MECHANICAL PROPERTIES


OF AUSTENITIC STAINLESS STEEL (304) AND 6063 ALUMINIUM
ALLOYS BY FRICTION WELDING
P. Sammaiah, G.R.N. Tagore, K. Prasada Rao and V.G.N. Rao
Osmania University

The aim of this study is to investigate experimentally the mechanical properties in terms of friction
pressure and upset pressure. Friction pressure, upset pressure is varied; burn-off length, rotational speed and
duration of welding are fixed. The tensile strength and impact strength are increased with increase in upset
pressure. The tensile strength and impact strength are decreased with increase in friction pressure. It is
observed that the joint efficiency of friction welded dissimilar materials is proportional to upset pressure and
inversely proportional to friction pressure. The mechanical properties of friction welded parts also relates
with the rate of axial shortening length. The rate of axial shortening of welded parts increases with increase
in upset pressure. Microstructures using micro photographs were examined in the heat affected zone of
welded parts. Hardness variations in welding zone were also obtained. Experimental results were compared
with those of parent metals.
ISRS-2008 43

M1-P2
FEM SIMULATION OF POROUS STEELS UNDER
CONTACT FATIGUE LOADING
Govindarajan N. and Gnanamoorthy R.
Dept. of Mechanical Engg, Indian Institute of Technology, Madras, India
Powder metallurgy route is becoming progressively more essential in automotive sector principally
due to save weight and cost of production. The application of sintered steels depends on the mechanical
properties which are greatly influenced by densification process. Presence of pore edges in sintered steels
may worsen the contact fatigue properties. Effect of porosity under the contact fatigue conditions has been
elaborately discussed in the previous publications. The objective of this paper is to investigate the effect of
the porosity in different amount and shape under the fatigue cyclic loading by numerical approach. The
induced contact stresses near to the pore edges have been simulated in sintered steels by available general
purpose code, with this the contact fatigue life is predicted and compared with the experimental results. For
this Dang Van fatigue model is used.

M1-P3
INVESTIGATES OF CRACK STRUCTURE
USING FINITE ELEMENT METHOD
Hari Prasad K.
Sathyabama University, Chennai, India
This paper investigates the accuracy of predicting the dynamic response by finite element modeling
of structures with cracks. Steel and composite materials are widely used in various construction elements
and composites in particular have increased substantially over the past few years. These materials are
subjected to various types of damage, mostly cracks and delaminations. These result in local changes of the
stiffness of elements from such materials and consequently their dynamic characteristics are altered.
The cracks are modeled as such in case of stress analysis to study the stress pattern at those local regions
of crack, while in case of dynamic analysis an equivalent model is built with many assumptions. While there
are many literatures available on these, there is literally none that has investigated the effect on the results of
the analysis with such models.
The aim of the work presented in this paper is to analyse the influence of mesh and spring stiffness
values on the error in dynamic analysis and modal frequency values of a beam. This problem has been solved
by using the finite element method. The damaged part of the structures has been modeled by contact finite
elements with failures, while the undamaged parts have been represented by other, well-known finite
elements.
44 ISRS-2008

M1-P4

EFFECT OF SLOT NOTCH ON LOW CYCLE FATIGUE BEHAVIOR OF


ALLOY 718 AT 25qC AND 650qC
Sridhar A.a,b, Vikas Kumar a, Gogia A. K. a and Ganesh Sundara Raman S.b
a
Defence Metallurgical Research Laboratory, Kanchanbagh, Hyderabad, India
b
Dept. of Metallurgical & Materials Engg, Indian Institute of Technology Madras, India

Low cycle fatigue (LCF) life can be significantly influenced by notches present in components. Most
of the data available in literature have been generated using specimens having circumferential or single or
double edge notches. Use of specimens with circumferential notch may not be entirely appropriate for
comparison with smooth (unnotched) fatigue specimens, because of difference in their diameters. As the
diameter decreases, there is a decrease in volume or surface area of the specimen. This is of significance,
since fatigue failures usually start at the surface.

In the present study tangential slot notch was used to investigate its effect on LCF behavior of Alloy
718. It removed a very small percentage of the specimen cross-sectional area and did not cover entire
circumference. So a comparison could be made between the smooth and tangential notch specimens without
much variation in their surface areas or volume. Total strain controlled LCF tests were conducted at 25qC
and 650qC (R 0, triangular wave form, 0.3 Hz frequency) using specimens with tangential slot notch and
unnotched specimens. Results indicate that tangential slot notch also reduced significantly the fatigue life of
alloy 718 though it removed only a small amount of material from the gauge portion.

M1-P5

EFFECT OF MELT AND HEAT TREATMENT ON MECHANICAL AND


ABRASIVE WEAR BEHAVIOUR OF CAST Al-Si-Mg ALLOYS
Swamy N.H.S., Raghavendra Kumar S., Joseph M.A., Nagarajan N.M. and Sateesh N.H.
National Institute of Technology, Calicut, India

This paper presents the results of investigations carried out on the effects of heat treatment in cast alloys,
on mechanical properties and dry sliding wear behaviour of Al-Si-Mg cast alloys. Al-Si-Mg alloys with 7, 12, 16
%Wt. silicon and cast with modification, combined modification & vibration and heat treatment were tested
adopting standard testing procedure have been compared. Samples cast with modification, vibration during
solidification and heat-treated exhibit relatively better mechanical properties and improved wear resistance.
Optical microscopy study of these samples show enhanced spheroidisation and uniform distribution of eutectic
silicon crystals. Scanning electron microscopy of tensile fractured and wear surfaces were carried out to analyse
the mode of fracture and mechanism of material removal under abrasive wear condition.
ISRS-2008 45

M1-P6
MECHANICAL PROPERTIES OF MANGANESE DOPED Y-TZP:
THE EFFECTS OF HOLDING TIME VARIATIONS
Meenaloshini S. and Ramesh S.
Universiti Tenaga Nasional, Malaysia
The effect of varying holding times on the mechanical properties of yttria stabilized tetragonal zirconia
doped with 1 wt% MnO2 was investigated. Samples were sintered at 1300qC - 1350qC with holding times
varying from 12 mins up to 2 hours. Longer holding times (1 hour and 2 hours) resulted in enhanced
densification of the undoped Y-TZP as compared to the MnO2 doped Y-TZP. The MnO2 doped Y-TZP
however, recorded better densities, especially for sintering temperatures above 1325qC, for samples with 2
hours holding time. Higher fracture toughness values were obtained for the undoped samples compared to
the doped ones produced at the same temperature and same holding times. Longer holding times resulted in
improve fracture toughness for undoped samples, these being more noticeable for samples sintered at
1325qC. Shorter holding times (12 mins, 30 mins and 1 hour) and higher sintering temperature (>1325qC)
saw an improved hardness in the MnO2 doped samples. Even though lower hardness values were recorded
for the undoped samples, as compared to the doped samples, a consistent increase in hardness values were
depicted as holding time was increased from 12 mins to 2 hours. However, an inconsistent trend was observed
for Young’s Modulus values of the doped samples instead.
46 ISRS-2008

<4270=820;1470E8>DA88
M2-O1
A UNIFIED VISCOPLASTICITY MODEL FOR APPLICATION
IN HIGH TEMPERATURE APPLICATIONS
Shridhar Powar, Lakshmana Rao and Adinarayana Namburi
Indian Institue of Technology, Madras, India

Life estimation of high temperature components in power generation equipments is critical for the safe
operation of these components. Current life estimation codes simplify the interaction of the degradation
mechanisms of creep and fatigue, hence allowing in a large amount of conservatism in the design of the
components to account for the uncertainty. This can be avoided and the life estimation can be improved if
physics based constitutive models, which attempt to model the degradation mechanisms better are applied
to design of components. In this paper a unified constitutive called Bodner model has been utilized for
demonstrating material behavior under diverse loading scenarios. The model has been applied to a uniaxial
specimen with the material parameters of Inconel 718, which is a widely used material in the industry. The
model has been compared with experimental data for uniaxial monotonic and cyclic response. Creep response
has also been simulated under certain conditions. The seamless integration of these two mechanisms and the
resulting accumulation of strains have been demonstrated. In addition the response of the model to widely
varying loading conditions has also been displayed.

M2-O2
EFFECT OF WELDING CONSUMABLES ON TENSILE, HARDNESS
AND IMPACT PROPERTIES OF GAS TUNGSTEN ARC WELDED
MARAGING STEEL JOINTS
Venkata Ramana P. and Madhusudhan Reddy G.
Jawaharlal Nehru Technological University, Hyderabad, India

Maraging steels are widely used in aerospace applications due to combination of strength and
toughness superior to other high strength steels. The unique property of being weldable in the solutionized
condition followed by post weld maraging treatment at relatively low temperature (480qC) makes these steels
attractive for fabrication of large structures. In common practice, however, gas tungsten arc welding is widely
employed in view of the consistency of weld quality and overall economy. The strength and toughness of
fusion zone of considerably lower than that of parent metal and this has been attributed to presence of reverted
austenite. The strength and toughness of welds to a greater extent are dictated by the filler metal selection.
In this investigation an attempt has been made to study the effect of welding consumables on tensile, hardness
and impact properties of maraging steel joints. Three different consumables, namely maraging steel,
austenitic stainless steel and medium alloy medium carbon filler have been used to fabricate joints by gas
tungsten arc welding processes. Weldments were subjected to direct aging treatment at 480qC/3h/air cooling.
Microstructure and mechanical properties such as tensile, hardness and impact toughness in the as-weld and
aged conditions were evaluated. The joints fabricated using maraging steel filler metal showed superior
strength than other joints. The joints fabricated using austenitic stainless steel filler metal exhibited superior
toughness than other joints. Optimum combination of strength and toughness are obtained by welds made
with medium alloy medium carbon filler metal. The observed mechanical properties have been correlated
with microstructure and fracture features.
ISRS-2008 47

M2-O3
STRESS AND DEFLECTION ANALYSIS IN THE CERAMIC
ORTHOTROPIC COMPOSITE PLATES WITH CIRCULAR HOLE(S)
SUBJECTED TO TRANSVERSE LOADING
Jain N.K., Shrihari Agrawal and Rajput P.S.
Sagar Institute of Research and Technology, Bhopal, India

The distributions of stresses and deflection in rectangular ceramic orthotropic composite plates with
two coaxial circular holes subjected to different transverse static loading conditions have been studied using
finite element method. The aim of author(s) is to analyze the effect of D/A, D/L and X/D ratio (where D is
hole diameter, A is plate width, X is centre distance of holes and L is plate length) upon stress concentration
factor (SCF) for normal stresses in X, Y directions, shear stress in XY plane and von mises stress, and
deflection in transverse direction in ceramic orthotropic rectangular composite plates. The D/A ratio is varied
from 0.1 to 0.5. The results of ceramic fibre composites are also assessed with results of glass fibre and
graphite fibre composites. The results are obtained for three different boundary conditions as all edges are
simply supported, all edges are fixed and two edges are simply supported and two edges are fixed. The
variations of SCF and deflection with respect to different parameter are presented in graphical form and
discussed. The finite element formulation is carried out in the analysis section of the ANSYS package. This
work will also provide the guidelines to designer to select the material as per their requirements. This work
will helpful for the designing of members of marine, aircraft, nuclear reactors and chemical vessels where
such situations are commonly met width.

M2-O4
EFFECT OF Pt CONTENT ON THE TENSILE PROPERTIES OF
FREE STANDING PtAl BOND COATS AS DETERMINED
BY MICROTENSILE TESTING
Md. Z. Alam, Srivathsa B., Kamat S.V., Jayaram V. and Das D.K.
Indian Institute of Science, Bangalore, India

Pt-aluminide (PtAl) bond coats typically 50-100 Pm thick, are widely used for imparting oxidation
resistance to Ni-based superalloy components of gas turbine engines. These coatings exhibit a multilayer
structure and show a graded composition. Despite their excellent oxidation resistance, PtAl coatings are
brittle and, are known to degrade the mechanical properties of the coated components. In order to determine
the mechanism by which these coatings affect the tensile properties of the substrate alloy, the tensile properties
of free-standing PtAl coatings have been evaluated at room temperature, using microtensile testing. The
design of the test specimens was established by parametric studies using finite element method (FEM) based
simulations using ANSYS. The microsamples that were designed had a parallel gage length of 2 mm, gage
width of 0.5 mm, thickness ~ 90Pm with an overall length of 8 mm. The elastic stress concentration factor
due to the 0.5 mm fillet radius was calculated to be in the range of 1.12 to 1.28. These dimensions ensured
the failure of the samples within the gage length.
PtAl coating samples with varying Pt content were tested at room temperature (RT). Results indicate
that incorporation of Pt upto 5 %m does not affect the tensile properties significantly. However, for high Pt
levels which corresponded to an initial Pt layer thickness of 10 %m, the UTS increases by almost two times.
48 ISRS-2008

Since the brittle-to-ductile transition temperature of these coatings are above 600qC [1, 2], the measurable
ductility for all the samples was approx. 0.2%. Fractography studies indicate with significantly higher Pt
content, these coatings show an increased tendency for brittle cleavage failure. Apart from the
above-mentioned results, the various issues regarding the preparation of these coating microsamples and the
aspects of testing at such small length scales will be discussed.

M2-O5
CREEP STRENGTH OF CENTRIFUGALLY CAST Al-RICH TIAL ALLOYS
Sturm D.3, Heilmaier M.3, Saage H.3, Paninski M.1, Schmitz G.J.1, Palm M.2, Stein F.2, Drevermann A.1,
Engberding N.2, Kelm K. 4, Irsen S.4
1
ACCESS e.V., Intzestraße 5, D-52072 Aachen, Germany
2
Max-Planck-Institut für Eisenforschung GmbH, Max-Planck-Str. 1, D-40237 Düsseldorf, Germany
3
Otto-von-Guericke-Universität Magdeburg, Institut für Werkstoff- und Fügetechnik, Lehrstuhl
Werkstopffprüftechnik, Postfach 4120, D-39016 Magdeburg, Germany
4
Stiftung caesar, Electron Microscopy, Ludwig-Erhard-Allee 2, 53175 Bonn, Germany

Al-rich Ti-Al alloys are considered as promising candidates for the development of novel light-weight
materials for structural applications at high temperatures. Compared to Ti-rich J-TiAl-based alloys Al-rich
Ti-Al alloys offer an additional reduction of the density of 20%, a better oxidation resistance - which are both
due to the increased Al content - and sufficient strength at high temperatures. The material has been
centrifugally cast by ACCESS in Aachen. Microstructural characterization was carried out employing
light-optical, scanning and transmission electron microscopy and XRD analyses. High temperature creep of
a binary Ti-60 Al (at. %) and a Ti-62 Al (at. %) alloy in the cast state and after annealing at 950qC for 200 h
which produced lamellar J-TiAl  r-Al2Ti microstructure were studied utilizing creep compression tests in
a temperature range between 900 and 1050qC in air. In particular, it is shown here that the as-cast alloys
exhibit already quite reasonable creep resistance at 900$C, especially with regard to their low density of
around 3.8 g/cm3. Stress exponents calculated as the slope n 'log (strain rate)/'log (stress) 4 were found
to be relatively constant for the temperature and stress regime investigated. This indicates that dislocation
climb may be the rate controlling creep mechanism. The assessment of creep tests conducted at identical
stress levels and varying temperatures yielded activation energies for creep of around Q = 420 kJ/mol for the
annealed Ti-60 Al (at. %) alloy. This value is significantly higher than the once found in literature for
interdiffusion of Al or Ti in J-TiAl which may arise from the two-phase microstructure of the alloys
investigated here. Whereas the value of Q 347 kJ/mol obtained for the annealed Ti-62 Al (at. %) material
coincides well with that of Al diffusion in J-TiAl.

M2-P1
MULTIMODE LAMB WAVES INTERACTION WITH DEFECT IN
METALLIC STRUCTURES USING EMAT:
MODELING AND EXPERIMENT
Dhayalan R., Krishnan Balasubramaniam, Krishnamurthy C.V., Janardhan Padiyar M., Maxfield B.W.
Indian Institute of Technology, Madras, India

This paper describes the finite element simulations and experiments to examine the generation and
interaction of Lamb waves with defects in thin plate using Electromagnetic Acoustic Transducer (EMAT).
ISRS-2008 49

This type of transducer can generate or detect sound waves in electrically conductive or magnetic materials
through the Lorentz force principle or magneto-elastic effects. This paper also describes the design principles
of developing electromagnetic acoustic transducers using both experimental and simulation for lamb wave’s
generation. At low values of the frequency-plate- thickness product (f*d), multiple Lamb wave modes are
excited with different group velocities. The fundamental Lamb wave modes (A0) and S0) are excited at 500
kHz in a 2mm thick aluminum plate and these modes are allowed to interact with slot type defects of different
depths. The fundamental lamb wave modes (A0 and S0) are mode converted by the slot type defects which
observed in the output signals. The mode converted Lamb wave modes are analyzed and identified with the
help of Dispersion curves for 2mm thick aluminum plate. In this paper we combine the experimental work
with the finite element simulation to understand the, propagation and interaction of the multimode Lamb
waves with defects.

M2-P2
FLOW BEHAVIOR OF AZ31 Mg ALLOY UNDER COMPRESSION
Rajesh Korla and Atul H. Chokshi
Indian Institute of Science, Bangalore, India

In textured HCP metals, there is a strong asymmetry in tensile - compressive flow behavior due to a
lack of sufficient number of slip systems, along with high possibility of twinning. The influence of grain size
(8 to 51 Pm) and temperature (298 to 673 K) on the flow behavior of highly basal textured AZ31 alloy was
studied under compression. There is a clear transition in the flow behavior with increasing temperature, at
523 K. It was also observed that twinning operates only above a certain critical grain size; below this size,
slip is the dominant deformation mechanism. The effect of strain rate on transition temperature was also
studied. The experimental results will be discussed with reference to existing deformation models, and the
implications for creep will also be considered.

M2-P3
DAMPING AND STIFFNESS BEHAVIOR OF FLY ASH REINFORCED
FUNCTIONALLY GRADED RUBBER COMPOSITE
Doddamani M.R. and Kulkarni S.M.
National Institute of Technology, Surathkal, India

The paper presents extensive analysis of dynamic behavior of a very special class of composite. A
systematic experimental investigation was conducted to evaluate the stiffness & damping ratio of
unreinforced and fly ash reinforced functionally graded rubber composite (FGRC). FGRC coupons were
prepared using conventional casting technique. Presence of gradience in prepared specimens is attributed
towards variable density particles present in fly ash which settles variably while solidifying. The methods
considered for evaluation were Logarithmic Decrement Analysis, Hilbert Transform Analysis, Moving Block
Analysis, and Modified Half Power Bandwidth method. Stiffness as a function of filler addition as well as
geometrical parameters was investigated. The damping response of varying fly ash bearing FGRC system
was studied. Experimental investigation was carried out using single channel Fast Fourier Transform analyzer.
The results obtained from our Experimental investigations show that, with the increase in filler weight fraction
& the thickness there is net increase in damping ratio. In present work, experiments are designed based on
Taguchi’s Design of Experiments approach.
50 ISRS-2008

M2-P4
A STUDY ON LARGE DEFORMATION ANALYSIS
OF HYPERELASTIC MATERIAL
Sujithra R. and Dhanaraj R.
Department of Rubber Tech., Department of Aerospace Engg. Madras Institute of Technology, Chennai, India

Rubber-like materials which undergo large elastic deformations, leads to numerous applications in
biomedical and meteorological fields. An increase of applications requires better understanding of
mechanical behavior which cannot be described by a simple stress-strain relation, but by their strain energy
function.In this paper, hyperelastic constitutive equations are discussed based on various strain energy
functions using theory of large elastic deformations. From the literature, few examples are considered here:
inflation of spherical balloons, inflation of a circular flat elastomer plate, thick walled cylinder subjected to
internal pressure, uniaxial and biaxial stretch. A comparison study has been done based on the analytical
solution for various material models and the results are also validated with FEA simulation (ANSYS).

M2-P5
TEXTURE AND MICROSTRUCTURE EVOLUTION IN COMPRESSION
OF TITANIUM - A MICROMECHANICS BASED APPROACH
Nilesh Gurao and Satyam Suwas
Indian Institute of Science, Bangalore, India

Evolution of microstructure during room temperature compression of hexagonal commercially pure


Ti with different initial orientation was studied using Orientation Imaging Microscopy (OIM). All the
different initial textures yielded the same end texture despite of different microstructural evolution in terms
of twin boundaries. This is due to the operation of different slip and twinning systems during deformation.
Micro-mechanics based Visco-plastic self consistent model using secant approach was used to reproduce and
thus validate the observed experimental results.

M2-P6
RESIDUAL STRESSES INDUCED BY COLD HOLE EXPANSION USING
BALL-SPLIT SLEEVE AND TAPERED PIN- SPLIT SLEEVE METHODS
Gopalakrishna H.D., NarashimaMurthy H.N., Krishna M.
R.V. College of Engineering, Bangalore, India

This paper reports experimental results on the determination of residual stresses in cold expanded holes
using ball with split sleeve and tapered pin with split sleeve methods. The results of measurements in the
vicinity of cold expanded holes in Al 2024 T3 alloy plates of thickness 4 mm are presented. The holes of
diameter 10.78, 10.67, 10.56, 10.45 and 10.34 mm were expanded by 2, 3, 4, 5 and 6 % respectively adopting
hardened steel ball of diameter 8.27 mm, EN24 hardened tapered pin and spring steel split sleeve using an
Instron machine. Tangential and radial residual stresses were measured using strain gauge method. The
gauges were mounted in radial and tangential directions at different distances from the hole to determine the
stress distribution around the hole. The two methods of expansion were compared based on the amount of
residual stresses induced around the hole and the zone of compressive stresses to establish the influence of
cold expansion on the parameters. The residual stresses verses the degree of hole expansion was studied in
both the methods. Selected specimens were subjected to cyclic loading of 125 KN (tensile and compressive)
corresponding to 50 % of the yield strength of Al 2024, at room temperature with a sinusoidal waveform of
a frequency of 25 Hz.
ISRS-2008 51

<0C4A80;B346A030C8>=

MD-O1
EFFECT OF GAS TUNGSTEN ARC WELDING (GTAW) AND LASER
BEAM WELDING (LBW) ON CORROSION OF Ti6Al4V ALLOY
Bupesh Raja V.K., Palani Kumar K., Elangovan K.
Sathyabama University

The titanium alloys are extensively used due to the properties like high strength-to-weight ratio,
excellent mechanical properties and high resistance to corrosion. Among the titanium alloys, Ti6Al4V alloy
is used widely due to its good weldability. In this investigation the effect of the welding process on the
corrosion behaviour of 3mm thick plates of Ti6Al4V alloy, is studied. The corrosion behaviour of the Ti6Al4V
weldments was studied using the gas tungsten arc welding (GTAW) and laser beam welding (LBW)
technique. These two processes were done to compare the fusion process and high-energy beam processes
and their effect on the corrosion behaviour of Ti6Al4V alloy. Further the corrosion behaviour of Ti6Al4V
weldments would be an indication of the quality of the weldment. The corrosion shall be more than the
acceptable value, if there is a breach in the argon gas shielding and contamination of the weldment by the
atmospheric gases and other inclusions. Generally pitting corrosion is observed in Ti6Al4V alloy; therefore
the pitting corrosion tests were done in this investigation. The pitting corrosion was studied using
potentiodynamic polarization technique, with non-deaerated 3.5% NaCl solution of pH 7, to create a
corrosion environment. The results show joints made by gas tungsten arc welding (GTAW) process yield
better pitting corrosion resistance when compared to laser beam welding (LBW) welding process.

MD-O2
WEIGHT LOSS CORROSION STUDIESS OF Al6061 / RED MUD
METAL MATRIX COMPOSITES IN SEA WATER
Abdul Jameel 1, Krupakara P.V.2, Nagaswarupa H.P.3
1
Department of Chemistry, Jamal Mohammed College, Tiruchirapalli.
2
Department of Chemistry, Auden Technology and Management Academy, Bangalore.
3
Department of Chemistry, East west Institute of Technology, Bangalore.

This paper deals with the corrosion characterization of Al6061- red mud particulate metal matrix
composites (MMCs). Al6061 alloy is used as matrix. Commercially available alloy is used. Red mud is the wastage
obtained after the removal of aluminium from its ore and conatis silics, alumina, titanium diaoxide and ferric
oxide. Being a ceramic material red mud remains inert and is hardly affected by the corrosion medium. Red mud
particles of size 50-80 microns are used as reinforcement. Experiments were conducted to determine the corrosion
rate of the samples in sea water procured from Arabian sea in malpe, Udupi District, Karnataka. MMC’s are
prepared according to ASTM standards by liquid melt metallurgy technique using vortex method. Composites
containing 2, 4, 6% by weight of Red mud and unreinforced matrix were tested using Arabian sea water at room
temperature. Specimens are taken in the form of 20mm u 20mm cylinders. They were exposed to sea water for
different intervals of time. Corrosion rates of all samples were calculated using the formula 534W/DAT mpy. The
results were computerised and simulation curves were obtained. The composite was found to be more corrosive
resistant than matrix alloy. In each test the corrosion resistance of both alloy composites was found to decrease
with the exposure time. The decrease in the corrosion rates of composites when compared to that of matrix
alloy is due to the physical barrier created by Red mud particles.
52 ISRS-2008

MD-O3
STUDIES ON CORROSION BEHAVIOR OF ANNEALED 18 Ni 250
GRADE MARAGING STEEL IN ORTHOPHOSPHORICACID MEDIUM
Poornima Shettya T., Jagannatha Nayak and Nityananda Shetty A.
National Institute of Technology Karnataka, Srinivasanagar
The corrosion behavior of annealed sample of 18 Ni 250 grade maraging steel was investigated in
orthophosphoric acid,which is a potential high strength steel for advanced technologies such as aerospace,
nuclear, and sporting goods. The corrosion test was carried out at different temperatures, in a corrosion
medium of orthophosphoric acid at different concentrations using electrochemical techniques like Tafel
polarization, electrochemical impedance spectroscopy (EIS) and scanning electron microscope (SEM)
studies.The results obtained from Tafel extrapolation techniques and EIS techniques are in good agreement.
The results show increase in corrosion rate with increase in temperature and also with increase in
concentration of corrosion media. The thermodynamic parameters like activation energy, enthalpy and
entropy of activation were calculated using transition state theory equations.

MD-O4
ASSESSMENT OF CORROSION RESISTANCE OF Cu-10Ni-1Fe AND
Cu-12Zn IN CLEAN AND SULPHIDE POLLUTED SYNTHETIC SEAWATER
Khan A.F., Patil A.P., Rao T.S.
VNIT, Nagpur
Cu–10Ni–1Fe is widely used in the marine environments. However, it suffers from accelerated
corrosion in sulphide-polluted seawater. It is known that addition of Zn to Cu-alloy improves resistance to
sulphide attack as in Cu–Zn alloy, but the data is scanty. The present study therefore investigates corrosion
resistance of Cu-10Ni alloy and Cu–12Zn alloys, so as to understand the role of Zn. Test method used was
cathodic polarization in clean and sulphide polluted synthetic seawater (SSW). The SSW was prepared as
per ASTM D 114-75 and sulphide was added through sodium sulphide. Two concentrations of sulphide were
taken viz. 0.1 g/L and 0.2 g/L. Ecorr of both the alloys become active on addition of sulphide in the test
solution. In case of Cu-10Ni it decreases substantially from –0.24 V Vs (SCE) in SSW to –0.92 V Vs (SCE)
in SSW  0.2 g/L Na2S. Whereas, the drop in Ecorr of Cu-12Zn alloy is only marginal i.e. from –0.30 V Vs
(SCE) in SSW to –0.44 V Vs (SCE) in SSW  0.2 g/L Na2S. Thus, the corrosion tendency of Cu-10Ni alloy
increases manifold from that of Cu-12Zn alloy on addition of sulphide to SSW. Corrosion current density
(icorr) of Cu–10Ni is found to be lower than that of Cu–12Zn alloy in SSW. The icorr of Cu-10Ni increases
from 8.78 PA/cm2 for SSW to 21.07 PA/cm2 for SSW0.2 g/L Na2S. Whereas, the corrosion rate of Cu-12Zn
alloy actually decreases on addition of 0.1 g/L sodium sulphide and increases on addition of 0.2 g/L Sodium
sulphide, but still is less as compared to that of Cu–10Ni–1Fe. Thus it is found that Cu–10Ni–1Fe is more
corrosion resistant in clean SSW and less corrosion resistant in sulphide polluted SS than Cu–12Zn alloy.
The drop in corrosion resistance of Cu–10Ni–1Fe in sulphide polluted SSW is attributed to formation of
Cu2S, that is less protective than Cu2O. Relatively better corrosion resistance of Cu–12 wt% Zn alloy in
sulphide polluted SSW is attributed to the formation of ZnS that is bad conductor.
ISRS-2008 53

MD-O5
PHENOMENOLOGICAL STUDY OF HOT TEARING
IN AZ91D MAGNESIUM ALLOY
Bichler L. and Ravindran C.
Centre for Near-net-shape Processing of Materials, Ryerson University, Toronto, Ontario, Canada

Hot tearing in steels and aluminum alloys has been rigorously investigated in the past decades.
However, the interaction between the key factors such as solidification, microstructure and stress and strain
at the onset of hot tearing in magnesium alloys remains unclear. Specifically, the stress and strain conditions
required to nucleate hot tears are unknown. In this research, neutron diffraction (ND) residual strain mapping
was used to determine the stress and strain conditions in a casting at the onset of hot tearing. The results
indicate that tensile residual stress of ~12 MPa in a casting region with a stress concentration was necessary
to nucleate and propagate hot tears. Microstructural analysis revealed that hot tears propagated via regions
of high interdendritic shrinkage porosity. These results were compared to the predictions of numerical
computer modeling and key issues preventing accurate computer modeling of hot tearing were identified.

MD-P1
STUDIES ON PASSIVATION OF AISI 304 STAINLESS STEEL IN
0.4N/0.5N H2SO4 AND EFFECT OF OXIDIZER (MnO4-) ADDITION
Khobragade N.N. and Patil A.P.
Visvesvaraya Natioanal Institute of Technology,Nagpur

Austenitic stainless steel, particularly SS 304 is a popular material for application in chemical and
fertilizer industry. It has excellent corrosion resistance in sulfuric acid owing to formation of a fine and
compact Cr2O3 film. Sulfuric acid is an oxidizing acid but when its concentration is low, the film is not stable
and does not heal by itself quickly, if damaged. Therefore, if film is damaged by turbulences or erosion, the
alloy suffers from accelerated corrosion. The situation can be salvaged by addition of an oxidizer. Present
study is aimed at finding out how the passivity in dilute acidic solution can be restored so that the SS 304
does not suffer from accelerated corrosion. Test solutions were 0.4N and 0.5N H2SO4 without or with an
oxidizer (0.1, 0.2, 0.5,1 and 2% KMnO4). Test method was potentiodynamic polarization 1V from open
circuit potential. It is found that in absence r with scan range of of oxidizer the cathodic part shows instability
and few segments of cathodic/anodic switch over; indicating thereby that active and passive states are stable
simultaneously. This means that the passivity is not truly stable and there is risk of accelerated corrosion in
case of damage to the film. On addition of oxidizer, the Ecorr shifts in noble direction and the feature of
simultaneous presence of active acid and passive state is removed. It is found that the cathodic plot has linear
region extending more than two order of magnitude of current; this part is used to workout cathodic current
density at OCP (icorr). Anodic part of the plots containing 0.1 KMnO4 has no passive phase and the icorr
obtained from cathodic part is highest. On increasing KMnO4 addition further, few plots exhibit two segment;
first limiting current region and second typical passivation region. However, the current density in this region
is too high for this to term as true passivity. The current density in limiting current region is also higher than
icorr obtained from cathodic part. Thus, corrosion of stainless steel in these test solutions is under cathodic
control. The optimum amount of KMnO4 both the solutions is 1%. It means, on additions 1% KMnO4 to
0.4N and 0.5N H2SO4 solutions, the passivity will become stable. However, corrosion will remain under
cathodic control.
54 ISRS-2008

MD-P2
CORROSION BEHAVIOUR STUDIES OF 6061 Al-15vol.pct.SiC
COMPOSITES IN ACID MEDIUM
Geetha Mable Pinto, Jagannath Nayak, Nityananda Shetty A.
NITK, Surathkal, Karnataka

The corrosion behavior of 6061 Al-15vol.pct.SiC composite is investigated which is potential structural
material for aerospace and automotive applications. The corrosion test was carried out at different
temperatures in the concentration range of 0.01N to 1N of 1:1 mixture of hydrochloric acid and sulphuric
acid as corrosion media using Tafel Extrapolation Technique and Electrochemical impedance
spectroscopy(EIS). Tafel extrapolation plot was obtained by polarizing the specimen to about 250 mV
anodically and –250 mV cathodically from the open circuit potential. The EIS measurements were carried
out in a frequency range of 100000Hz to 0.01Hz using the amplitude of 10mV peak to peak with AC signal
at the open circuit potential. The corrosion current density icorr was calculated using the charge transfer
resistence, Rct together with Stern-Geary equation. The results obtained from Tafel Extrapolation Technique
and Electrochemical impedance spectroscopy were in good agreement. The results show a increase in the
corrosion rate with increases in temperature as well as the increase in the concentration of the corrosion
media. The thermodynamic parameters like activation energy, enthalpy of corrosion and the change in the
standard free energy were calculated using transition state theory equations.

MD-P3
THE INFLUENCE OF SODIUM MOLYBDATE ON L-VALINE-Zn2+ SYSTEM
CONTROLLING CORROSION OF CARBON STEEL IN RAIN WATER
Wilson Sahayaraj J.1 and Susai Rajendran2*
1
Department of Chemistry, Jeppiaar Engineering College, Chennai
2
Corrosion Research Centre, Department of Chemistry, GTN Arts college, Dindigul, Tamil Nadu

Cooling water treatment plays a key role in most industries. In most cooling systems carbon steel is
used as construction material for heat exchangers and piping. Carbon steel in contact with water however
will corrode. To fight with corrosion in cooling water system, the chemicals with anti-corrosive properties
are dosed into the water. Though corrosion inhibitors such as chromate, polyphosphate and nitrite provided
a reliable measure of corrosion protection, discharge of such toxic materials was considered unacceptable
due to environmental safety guidelines. So L-valine (LV) used as environmental friendly inhibitor in this
study. The synergistic effect of L-valine and Zn2 on the inhibition of corrosion of carbon steel in rain water
(collected form roof top and stored in concrete tank environment) containing 72 ppm of chloride, 273 ppm
of TDS, 14 ppm of sulphate and 9 ppm of nitrate. The formulation consisting of 50 ppm of L-valine and 50
ppm of Zn2 has 74% inhibition efficiency (IE). To enhance the IE of L-valine - Zn2 system sodium
molybdate (SM) added. As the concentration of SM increases, IE also increases. As the immersion period
increases, the inhibition efficiency decreases. Polarization study reveals that the L-valine - Zn2 - SM system
functions as mixed inhibitor. AC impedance spectra reveal that a protective film is formed on the metal surface.
The FTIR spectra study lead to the conclusion that the Fe2 - LV complex and Fe2 - SM complex formed
on anodic sites of the metal surface controlled the anodic reaction and Zn(OH)2 formed on the cathodic sites
of the metal surface controlling the cathodic reaction. The L-valine - Zn2 - SM system may found in cooling
water system.
ISRS-2008 55

MD-P4
EROSION WEAR BEHAVIOR OF DETONATION SPRAYED
WC-Co COATINGS
Suresh Babu P., Basu B., Sundararajan G.
IIT Kanpur, Kanpur, ARCI, Hyderabad
Thermal spray techniques have become very popular for depositing wear resistant coatings to enhance
the component life and performance.Plasma spray technique is being used widely for depositing WC-Co
coatings characterized by greater thermal energy and low velocity of the particles, the plasma spray technique
results in substantial decomposition of WC leading to formation of brittle and amorphous phases with inferior
wear properties. In order to minimize decomposition, these coatings have been successfully deposited using
High Velocity Oxy-Fuel (HVOF) or Detonation spray coating (DSC) techniques. Despite the lower thermal
energy and high velocity used in both the HVOF and detonation processes (compared to plasma spraying),
decomposition still occurs though to a lesser extent. A review of the literature indicates that the erosion
resistance depends on multiple parameters, which are related to the deposition process, coating microstructure
including decomposition and coating mechanical properties and erosion test conditions. However, none of
the earlier studies employed a single technique to systematically vary the extent of decomposition and study
the influence of WC decomposition and coating structure on the wear properties. In the present talk, room
temperature dry solid particle erosion behavior of detonation sprayed WC-12Co coating will be discussed as
a function of processing parameters, coating microstructure and test conditions like various erodents, impact
velocities and impact angles.

MD-P5
OXIDATION BEHAVIOUR OF 30v%ZrB2-SiC & 30v%MoSi2-SiC
COMPOSITES UNDER DIFFERENT CONDTIONS
R.Suresh Kumar*, D.Sivakumar**, Ashutosh S.Gandhi*
*
Department of Metallurgical & Materials Science, IIT Madras
**
Materials & Metallurgy Group, Vikram Sarabhai Space Centre, Trivandrum, E-mail: r_sureshkumar@vssc.gov.in
Oxidation studies were conducted on two types of near theoretical density SiC based composites
containing 30v% ZrB2 and 30v%MoSi2 processed from powders through hot pressing. While isothermal
oxidation studies were conducted at 1500qC upto 12 hour duration to understand the oxidation kinetics of
these materials, the performance under rapid heating under oxidizing conditions was evaluated by conducting
rapid heating short duration tests through joule heating of the samples upto 2200qC. The features of oxide
surfaces of samples, both isothermal and rapid heat oxidized, were investigated through X-ray diffraction
technique and scanning electron microscopy and are presented in this paper.
56 ISRS-2008

MD-P6
STUDY OF ABRASIVE WEAR BEHAVIOUR ON COBALARC/
DUROMANGAN MULTILAYER HARDFACED MILD STEEL
FOR SLURRY PUMP APPLICATION
Vikas Kholar, Bhanu Kiran V. T., Samarjeet Chanda, Sanglap Ghosh, Siddhartha Dasgupta, Soumen Dutta

The objective of the paper is to study abrasive wear behaviour of cobalarc / duromangan multilayer
hardfaced mild steel using sand slurry abrasion tester. Cobalarc (Hardfacing layer) and Duromangan (Buffer
layer) electrodes were selected for replacing conventional hardfacing electrodes such as Stellite. The required
minimum hardness for slurry pump component material of 60 HRC is achieved by the use of cobalarc /
duromangam multilayer hardfaced mild steel. The multilayer hardfaced material (10mm thickness) showed
hardness and wear properties comparable to high chromium steel material (30mm thickness) currently being
used for slurry pump lining and impeller. The multilayer hardfacing is usually restricted to two hardfacing
layers, as triple or multiple layers result in the formation of cracks due to welding contraction strain. The
cobalarc / duromangam multilayer hardfaced mild steel can be considered as an alternative material for slurry
pump applications.

MD-P7
LOW TEMPERATURE OXIDATION BEHAVIOUR OF
NANOCRYSTALLINE vis-à-vis MICROCRYSTALLINE Fe-10Cr ALLOYS
Rajeev K. Gupta1, Singh RamanR.K.1,2, Murty B.S.3, Carl C Koch4
1.
Department of mechanical and aerospace engineering, Monash University, Australia
2.
Department of chemical engineering, Monash University, Australia
3.
Department of metallurgical and materials engineering, IIT-M
4.
Department of materials science and engineering, North Carolina state university, NC, USA

Nanocrystalline Fe-10Cr alloy with a mean grain size of 52 r 4 nm, prepared by high energy ball
milling followed by compaction and sintering, was oxidized in air at 300oC for 52 hours. Its oxidation
behaviour, determined by measuring the weight change after regular time intervals and post-oxidation
characterization of oxide film using secondary ion mass spectrometry (SIMS), was compared with that of
microcrystalline alloy of similar chemical composition, prepared by similar processing route and oxidized
in similar conditions. It was found that grain refinement to nano-scale level leads to a significant improvement
in the oxidation resistance of Fe-10Cr alloy. SIMS analysis reveals that the improved oxidation resistance is
due to the formation of a Cr rich inner passive scale and Cr content in the passive film of nc alloy is much
higher than that of mc alloys. Cr enrichment is due to the unique structure of nanocrystalline material where
grain boundaries enhance the diffusion of Cr towards the oxide/alloy interface. A mechanism of improved
corrosion resistance, based on the kinetic curves, SIMS analysis and theoretical knowledge of oxidation of
binary alloys is proposed.
ISRS-2008 59

<06=4C82<0C4A80;B
MM-O1
INVERSE MAGNETOCALORIC EFFECT
IN Ni-Mn-Sn MELT-SPUN RIBBONS
Babita I.1,2*, Chandrasekaran V.1, Ram S.2
1
Defence Metallurgical research Laboratory, Hyderabad 500 058
2
Materials Science Centre, Indian Institute of Technology, Kharagpur 721 302

Materials exhibiting large magnetocaloric (MC) effect under relatively low applied magnetic fields
are of great interest for environmental friendly room temperature magnetic refrigerant.1 Recently, in Ga free
Ni50Mn50-yXy (X In, Sn and Sb) series of Heusler alloys, positive magnetic entropy change, ('SM) often
termed as inverse MC effect (IMCE) has been reported in the vicinity of the first order structural
transformation (FOST) due to the strong coupling between magnetism and the structure2-3. Rapid
solidification/melt spinning offers metallurgically an interesting process route to synthesis ribbons of these
materials with fine microstructure and the ribbon thus processed can be used as precursor for powder
production. The fine powders in the form of bed or consolidated shapes are technologically attractive for
fabrication of MCE devices. Two alloys of compositions Ni49Mn37.4Sn13.6 (R1) and Ni50Mn34.5Sn15.5 (R2)
were prepared by arc melting of high purity Ni, Mn, Sn in argon atmosphere. The alloy ingots were
homogenized by turning and re-melting for four times. About 5-10 gm of each alloy was melted in a quartz
crucible and ejected on to a copper wheel with surface velocity of 50 m/s. The composition of the ribbons
was analysed using EDX and EPMA. DSC measurements were carried out to identify the structural
transformation temperatures. The magnetic entropy change, 'SM was calculated from M-H data using the
Maxwell relation,In this paper, we report the IMCE observed in melt spun Ni-Mn-Sn ribbons and the results
are discussed in association with FOST and magnetic transitions. Interestingly, in R1 ribbon, the structural
transformation occurs prior to magnetic transition incongruous to that observed in Ni50Mn34.5Sn15.5 ribbons.
A maximum positive magnetic entropy change, 'SM ~6.0 Jkg-1K-1 and ~1.6 Jkg-1K-1 for a field change
of 2 T was observed in Ni49Mn37.4Sn13.6 and Ni50Mn34.5Sn15.5 ribbons respectively.

MM-O2
EFFECT OF TEMPERATURE ON MAGNETIC DOMAIN STRUCTURE IN
MULTIFERROIC DY SUBSTITUTED BISMUTH FERRITE THIN FILMS
Prashanthi K., Mandal M., Duttagupta S.P. and Palkar V.R.
Centre for Excellence in Nanoelectronics, Indian Institute of Technology Bombay, Mumbai-400076, India

Multi-ferroïcs are exceptional materials whose fundamental state is both magnetic and ferro-electric.
Because of coupling between magnetization and polarization (ME coupling) wide range of application can
be proposed with these materials. Possible applications of magnetoelectric materials include
magnetic-electric energy converting components, solid-state nonvolatile memory and multi-state memories.
Perovskite BiFeO3 (BFO) is one of the very few room temperature multiferroic materials and has been
attracted many researchers in this field. It exhibits ferroelectricity and antiferromagnetism at room
temparature. However to explore this material for device applications it is essential to induce ferromagnetism
without disturbing ferroelectricity at room temperature. We have been successful in achieving the desired
properties by partial substitution of Dysprosium (Dy) at Bismuth (Bi) sites. In this paper, we present the
60 ISRS-2008

effect of temperature on magnetic domain structure in Bi0.7Dy0.3FeO3 (BDFO) thin films grown by pulsed
laser deposition technique on Pt/Si substrate. Magnetic force microscopy (MFM) was used to image the
magnetic domains and effect of temperature was observed in-situ. Interestingly, as-grown film shows irregular
magnetic domain pattern but as the temperature increases, domains start aligning and around 200oC change
to stripe domains. However, above 250oC, once again the domain alignment is disturbed. This could be
attributed to magnetic transition which occur around 270oC as indicated by Differential Thermal Analysis
(DSC) curve. Upon quenching the system back to room temperature, an irregular pattern is recovered with
larger magnetic domains. The observed changes in the magnetic domain structure with temperature suggest
a strong thermal history dependence of the system related to the internal strains in the sample.

MM-O3
MAGNETIC AND OPTICAL PROPERTIES OF Co AND Mn CO-DOPED SnO2
Balamurugan K.
Indian Institute of Technology Madras, Chennai
The non-magnetic wide-band gap semiconducting oxides, such as ZnO, TiO2 and SnO2 etc., have been
found to exhibit interesting magnetic and optical properties when they are doped by 3d transition metals.
More interests on these materials are due to the fact that they exhibit ferromagnetism with Curie temperature
(TC) greater than 300 K. It has been shown by ab initio calculations that doping the wide band gap (Eg 3
eV) TiO2 (rutile) with double impurities of transition metals would create impurity states and Fermi level
close to the bottom of the conduction band. This double doping could give doped oxide semiconductors
without oxygen vacancies. Also, it was proposed that these doubly doped oxide semiconductors might be
suitable for spintronic applications.
SnO2 is a wide band gap semiconductor with optical band gap Eg 3.6 eV, having rutile structure.
The polycrystalline powder sample of composition Sn0.95Co0.03Mn0.02O2 was prepared by solid state
reaction method. This sample was found to exhibit a clear non-linear filed dependent magnetization, similar
to a ferromagnet. A maximum magnetization of 0.033 emu/g was observed for the applied magnetic filed of
1 tesla, at room temperature. Temperature dependent magnetization showed a drop in magnetization around
145 K and the overall data looks similar to that of Mn-doped ZnO nanorods. This drop in magnetization
suggests that there might be magnetic impurities of the doped metals Co and Mn, either in the form of metal
or metal-oxide. Correspondingly we find some secondary phase in the scanning electron microscope (SEM)
images of the sample. This implies that the observed ferromagnetism at room temperature might be either
from Co metal or Mn3O4 or from both. The diffuse reflectance spectrum (DRS) of the Co-3% and Mn-2%
co-doped SnO2 shows two more electronic transitions in addition to that of the host SnO2. Of the two
additional transitions, one is in the visible region and the other is in the near infra red (NIR) region of the
electromagnetic spectrum. These transitions might be due to the creation of additional impurity energy levels
as an effect of doping.
ISRS-2008 61

MM-O4
EFFECT OF THICKNESS ON MAGNETIC PROPERTIES
OF NICKEL FERRITE THIN FILMS
Gagan Dixit*, Singh J.P., Srivastava R.C. and Agrawal H.M.
G.B. Pant University of Agriculture & Technology, Pantnagar, Uttarakhand, India

Ferrites are soft magnetic material having high value of resistivity and low eddy current losses . This
make ferrite thin films suitable for magnetic recording and high frequency microwave device applications.
Nickel ferrite has inverse spinel structure. The present work is motivated to study the effect of thickness on
the magnetic properties of the nickel ferrite thin films. The thin films were deposited on Si (100) substrate
by pulsed laser deposition technique (PLD) as it preserves the target stoichiometry [1]. The deposition time
was varied from 16 min to 40 min in order to have the films of different thickness.The thickness of the films
range from 80nm to 200 nm as measured by surface profilometer.All the films were characterised by XRD,
AFM, &VSM. The XRD confirmed the spinel phase. The microstructure of the films was studied by AFM
.Both the roughness and grain size of the films were found to increase with the thickness of the films. The
particle size was estimated from the X-ray diffraction line broadening also. It gives values less than that
obtained by AFM. This may be because AFM gives the grain size with surroundings such as oxides.
Nanograins are built of several coherent diffraction domains that also causes the grain to look larger in size.
Magnetic properties were studied by vibrating sample magnetometer. M-H curves were recorded for all the
films at room temperature and at10K.. At 10K the films having thickness 200,150,100 and 80 nm show the
coercivity values 430, 571, 611 and 1112 Oe and saturation magnetisation 233, 173, 170, 97 emu/cc
respectively. The coercivity of the films increase with decrease in thickness while saturation magnetisation
decrease with decrease in thickness. The higher coercivity for low thickness film is attributed to the fact that
as the thickness decreases the grain size also decreases and this causes increase in grain boundary and the
consequence of which is increase in coercivity[2]

MM-O5
HEALTH AND USAGE MONITORING OF COMPOSITE STRUCTURES
WITH SMART MAGNETOSTRICTIVE SENSORY LAYER
Anand Kumar & Bishakh Bhattacharya
IIT, Kanpur

Fundamental research and development in smart materials and structures have shown great potential
for enhancing the functionality, serviceability and increased life span of civil and mechanical infrastructure
systems. Researchers from diverse disciplines have been drawn into vigorous efforts to develop smart and
intelligent structures that can monitor their own conditions, detect impending failure, control damage and
adapt to changing environments. The potential applications of such smart materials and systems are
abundant--ranging from design of smart aircraft skin embedded with smart sensors to detect structural flaws,
bridges with sensing and actuating elements to counter violent vibrations and flying micro electro-mechanical
systems with remote control for surveying and rescue missions. Smart structures are generally created through
synthesis by combining sensing, processing and actuating elements integrated with conventional structural
materials such as steel, concrete, or composites. Composite structures are now gaining attention due to
overriding advantages over the conventional metallic structures. The conventional non destructive evaluation
techniques are not very effective in monitoring the structural integrity of composite structuress due to their
micro-mechanical complexities. Various types of smart patches e.g. PZT patches and PVDF films have been
62 ISRS-2008

used as smart alternatives to sense and detect damage in composite structures. Magnetostrictive materials,
like piezoelectric materials, can be used both as sensors and actuators. With the commercial availability of
the magnetostrictive material Terfenol-D in particulate form, it is feasible to develop particulate sensors to
detect damage with minimum effect on structural integrity. These smart sensors provide real time sensing by
exploiting their functional properties. They are light in weight, consume less power and have better reliability.
In present investigation, the electromagnetic response in the MS layer at the onset of delamination in one of
the weakest ply of the composite laminate has been analyzed. For the numerical analysis, a number of
symmetric and asymmetric carbon epoxy laminates with one of its layers embedded with Terfenol-D particles
have been taken. Terfenol-D layer experiences a change in stress due to onset of delamination causing a
change in its magnetic state which can be sensed as induced open circuit voltage in the sensing coil enclosing
the laminate beam. The effect of material properties, lamination schemes and placement of MS layer on the
sensing capabilities has been analyzed. Classical laminate theory has been used.

MM-P1
ELECTRICAL AND MAGNETIC STUDIES OF MONOVALENT
DOPED CMR MANGANITES
Kalyana Lakshmi .Y and Venugopal Reddy .P
Department of Physics, Osmania University

In recent times, monovalent (A Li, Na, K, Rb & Ag) doped rare earth manganites are found to exhibit
significant CMR at or near room temperatures at low fields. Among these, K and Ag have been tested as
oxidation catalysts for exhaust gauges in internal combustion engines. The physics of these manganites is
less understood. Therefore, a systematic investigation is carried out after synthesizing nano crystalline
samples with compositional formula La1-XAXMnO3 (A Li, Na, K, Rb & Ag) and characterizing by X-ray
diffraction (XRD) and Transmission electron microscopy (TEM) studies. The XRD data have been analyzed
by Rietveld refinement technique and it has been confirmed that most of the materials have Rhombohedral
crystal structure with R‘3 c space group. The particle size is found to vary between 10–55nm. The ferro to
paramagnetic and metal-insulator transition temperatures strongly depend composition (x) and dopant and
these are found to vary between 100-330K. A sharp decrease in resistivity is found with increasing magnetic
field. The percentage of magnetoresistance is found to increase linearly with decreasing temperature, which
is a typical characteristic of a granular system. The low temperature (T<50K) upturn in the resistivity is
analyzed using the combined effect of weak localization, electron-electron and electron-phonon scattering
mechanism.

MM-P2
EFFECT OF ANNEALING ON THE MAGNETOIMPEDANCE
OF Co-Mn-Si-B RIBBONS
Sandhya Dwevedi and Markandeyulu G.
Indian Institute of Technology Madras, Chennai

Magnetoimpedance (MI) is the change in the impedance of a soft ferromagnetic material in the
presence of an external steady magnetic field. The MI arises due to skin depth and its origin is the change in
the permeability of the material with respect to external magnetic field. Sensors based on this phenomenon
have ultra high sensitivities compared to the GMR sensors. In this paper, the dependence of MI of as cast
ISRS-2008 63

and annealed Co(68)Mn(5)Si(12)B(15) ribbons on the magnetic field and frequency is presented. High pure
elements of the alloy were taken in proper proportions and were melted in an arc furnace under argon
atmosphere and then the corresponding ribbons were obtained by melt-spinning method and the as cast
ribbons are amorphous. The crystallization temperature was found to be 573 degree from the DSC study. MI
measurements were done on 7 cm long ribbons in the frequency range 100 kHz – 13 MHz employing the
HP4192A impedance analyzer with the application of external magnetic field along the length of the ribbon,
up to 80 Oe. The amplitude of the alternating current was maintained at 10 mA during the measurements.
The MI is defined as MI% = [{Z(H)-Z(Hsat)}/Z(Hsat)] x 100, where Z(H) is the impedance at the field H
and Z(Hsat) is the impedance at the saturating field. The MI increases with increase in frequency and a value
of 161% was obtained in the as cast ribbon at 13 MHz. The MI versus magnetic field plots exhibited double
peak behaviour indicating the presence of the transverse domains. Heat treatment was carried out for an hour
near the crystallization temperature under vacuum, argon and the nitrogen atmosphere respectively.
Annealing under nitrogen atmosphere has increased the anisotropy field leading to a decrease in the MI to
as small as 1%. Under the argon atmosphere, brittleness of the ribbon increased and no appreciable change
in the impedance was observed while an MI of 43% was obtained when annealed in vacuum.

MM-P3
HALF-METALLIC COMPENSATED FERRIMAGNETIC HEUSLER
ALLOYS Mn2-XCoXVAl (X = 0.5, 0.75 and 1)
Ramesh Kumar K., Arout Chelvane J., Markandeyulu G. and Harish Kumar N.
Indian Institute of Technology Madras, Chennai

Half-metallic ferromagnets (HMFs) are known to have peculiar band structure viz. the majority spin
sub-band possess metallic band structure where as the minority spin sub-band exhibit semi-conducting or
insulating type of band structure. Heusler alloys are a class of materials exhibiting half-metallic property,
crystallize in cubic L21 structure with stoichiometry X2YZ or XYZ (X and Y are transition metal elements
where as Z is an element with sp valent electron). Many of these Heusler alloys are magnetically ordered
systems with very high Curie temperature and their crystal structure is very similar to the well known
semiconducors such as GaAs, GaN etc. Due to these advantages half-metallic Heusler alloys are found to be
attractive for magneto-electronic applications. Most of the Mn based ferromagnetic Heusler alloys such as
Co2MnZ (Z Al, Si, Ga, Sn and Ge) are extensively studied both theoretically as well as experimentally.
Recently, it has been proposed that the Mn moments prefers anti-ferromagnetic coupling if it is occupied in
the X site. The compounds Mn2VZ (Z Al, Ga) are the well studied half-metallic ferri-magnetic systems.
These low magnetic moments systems are further advantageous for spintronics applications due to the fact
that they do not give raise any stray field in the devices. Hence half-metallic anti-ferromagnetic systems
would be an ideal material for device applications. We have investigated the structural and magnetic properties
of half-metallic fully compensated ferri-magnetic Mn2-xCoxVAl (x = 0.5, 0.75 and 1) systems. All the
compounds were prepared using an arcfurnace under argon atmosphere and the materials are homogenized
in vacuum for three days at 1073 K. The stochiometry was confirmed by EDS analysis. XRD analysis revealed
that the compounds formed in single phase with a small atomic anti-site disorder which was evident from
the weak order dependent reflections. The lattice parameter was found to decrease with the Co substitution
from 5.864 Å to 5.806 Å indicating the replacement of Mn. Magnetic moment per formula unit was estimated
from 5 K magnetization data and the value decreased from 2 PB to 0.23 PB for the compound with 50%
substitution of Co. The reason could be the anti-ferromagnetic coupling between Mn-V moments being
compensated by the Co-V ferromagnetic coupling with the substitution of Co. Magnetization variation as a
64 ISRS-2008

function of temperature was carried out at the field of 100 Oe and the measurements showed that the Curie
temperature decreases with the Co substitution which is consistent with the theoretical estimation of the curie
temperature for Mn2VZ (Z-sp valent element) systems.

MM-P4
MAGNETIC PROPERTIES OF La(1-x)Sr(x)MnO3
Ramesh Babu, M. Junyang Chen, Han X.F. and Jayavel R.
Anna University, Chennai
La(1-x)Sr(x)MnO3 (LSMO) nanowires are prepared using a simple sol–gel process and alumina oxide
template. The as prepared LSMO nanowires are 20 and 200nm in diameter and tens of microns in length.
Prepared nano rods were annealed at 700qC for one hour and exhibit polycrystalline perovskite structure.
Magnetization and photoluminescence studies were performed from low temperature to room temperature.
Field cooled and zero field cooled magnetic measurments with 500Oe field reveals the cluster glass behaviour
of the nano rod below Curie temperature. At room temperature hysteresis measurements shows paramagnetic
nature.

MM-P5
MAGNETOCALORIC STUDIES ON TELLURIUM DOPED
NANOCRYSTALLINE MANGANITES
Rabindra Nath Mahato, Sethupathi K. and Sankaranarayanan V.
Indian Institute of Technology Madras, Chennai
Nanocrystalline manganites with perovskite structure R1-xAxMnO3 (where R is a trivalent rare-earth
element and A is the divalent cation) have been the subject matter of large number of recent studies due to
their unusual colossal magnetoresistance along with the other extraordinary structural, magnetic and
electrical properties. The manganite perovskites are also studied for magnetic refrigeration applications due
to their properties of low-field induced high magnetocaloric effect and wide range of their magnetic transition
temperature below and above room temperature. Nanocrystalline La1-xTexMnO3 (x 0.2, 0.3) compounds
were prepared by citrate complex method. The phase purity and crystal structure of the obtained powder are
studied using powder X-ray diffraction. The crystallite size is measured using Debye-Scherrer formula and
it is found to be 40 nm and 36 nm for x 0.2 and 0.3 samples respectively. The scanning electron micrographs
of the sample reveals that the sizes of fine particles, are in agglomerated form, decreases as tellurium content
increases. Transmission electron microscopy image shows that the particles are spherical in shape and the
average particle size was determined. The magnetic measurements were carried out using vibrating sample
magnetometer and they show Curie temperatures (Tc) of 217 K and 258 K for the samples x 0.2 and 0.3
respectively. The magnetocaloric effect is found to be 2.9 J/kg-K in an applied field of 1.2 T for
La0.7Te0.3MnO3 which is large when compared to most of the other perovskite manganites.
ISRS-2008 65

MM-P6
EFFECT OF Pr ADDITION ON THE MAGNETIC PROPERTIES
OF Nd2Fe14B/Fe3B NANOCOMPOSITES
Rajasekhar M.1,2, Akhtar D.2, and Ram S.1
1
Materials Science Centre, IIT Kharagpur, Kharagpur, India.
2
Defence Metallurgical Research Laboratory, Hyderabad, India.

Nanocomposite magnets composed of hard and soft magnetic phases with grain size in nanometer
range exhibit excellent permanent magnetic properties. These materials also known as exchange coupled
magnets have attracted considerable interest in recent years for development of permanent magnets. A strong
coupling between the soft and hard magnetic grains leads to a high remanence (Br) and maximum energy
product (BH)max in these materials. Nanocomposite consisting of Nd2Fe14B hard magnetic phase along
with Fe3B/Fe soft phase(s) has been studied in the recent past. Magnetic properties and the degree of exchange
coupling in nanocomposite magnets depends on microstructural parameters, such as crystallite size, phase
distribution and volume fraction of the hard and soft magnetic phases. Efforts have been made to synthesize
such materials by melt-spinning, mechanical milling, thin film techniques etc. It has also been suggested that
some magnetic as well as nonmagnetic elemental additives can further improve the desired permanent
magnetic properties.
In the present study, the effect of partial substitution of Pr for Nd on the crystallization behaviour,
phase formation and magnetic properties of Nd4.5-xPrxFe77B18.5 (x 0, 1, 2 and 3) melt spun ribbons have
been studied. The samples were prepared by melt spinning technique as amorphous ribbons followed by
vacuum heat treatment to develop a nanocrystalline microstructure. The as-spun and annealed ribbons were
characterized using differential scanning calorimetry, X-ray diffraction, magnetic measurement and
Mössbauer spectroscopy techniques. X-ray diffractograms and thermomagnetic curves confirm the presence
of the Nd2Fe14B hard magnetic phase and soft magnetic Fe3B and Fe phases in the heat treated alloys.
Enhancement of Hc and (BH)max was observed for 2 at% of Pr addition. Details of the above investigations
are presented in detail in this paper.

MM-P7
SYNTHESIS, STRUCTURAL AND MAGNETIC NATURE
INVESTIGATION OF Fe AND Ni SUBSTITUTED Y2O3 SYSTEM
Manigandan A., Sathiyakumar S., Anbarasu V., Kaliyaperumal L.K. and Jayabalan K.
Anna University, Chennai.

Synthesis of new magnetic materials and to characterize its physical properties is important because
of their potential applications in particularly memory devices. In present work, the newer magnetic materials
Y0.75A0.25BiO3 (where A Fe &Ni) was synthesized by Solid-State reaction technique. The single phase
formation and its tetragonal crystallization were studied by Powder X-ray diffraction studies. The well
crystallization nature of the prepared compounds was observed by Scanning Electron Microscope (SEM)
images and the stoichiometric ratio was confirmed by Energy Dispersive X – Ray (EDAX) measurements.
The phase transition temperature of both compounds were found to be 600qC and 630qC and the average
weight percentage was found to be 98.94% by Thermal analysis. At room temperature condition
ferromagnetic nature of Y0.75Fe025BiO3 system and diamagnetic nature with ferromagnetic contribution
of Y0.75Ni025BiO3 system were confirmed by Vibrating Sample Magnetometer (VSM) studies.
66 ISRS-2008

<>34;8=6?70B4BC018;8CH

MP 01
SIMULATION OF CARBON DIFFUSION PROFILE IN
DISSIMILAR WELDMENT USING DIFFUSION COEFFICIENTS
EVALUATED BY DEN BROEDER‘S METHOD
Sudha C., Saroja S., Terrance A.L.E., Vijayalakshmi M.
IGCAR, Kalpakkam

When dissimilar weldments between 9Cr-1Mo and 21e4Cr-1Mo ferritic steels are subjected to high
temperature, ‘hard’ and ‘soft’ zones form near the weld interface due to carbon diffusion. Carbon
concentration profile across the weld interface was simulated using a numerical technique in which the
diffusion coefficient of carbon, DC was assumed to be a constant. Since the width of the zones changes with
heat treatment time, it is necessary to study the change in DC to understand the growth kinetics of the zones.
An improved Boltzmann Matano method was used to evaluate DC which showed that carbon diffusion is
slower in the hard zone than in the soft zone. This is in agreement with the ratio of the measured width of
hard and soft zones i.e 1:3. In the base metals DC was calculated using Hall’s method and the values for
21e4Cr-1Mo and 9Cr-1Mo steels were obtained as 1.58 u 10 11 m2/sec and 9.9 u 10 11 m2/s respectively
which agree with literature data.

MP-O2
CUBE TEXTURE EVOLUTION CONTROLLED BY GAS –METAL
ATMOSPHERE DURING D  J  D TRANSFORMATION
IN THE Mn AND Al ALLOYED ULTRA LOW CARBON STEEL
Jai Gautam1&2, Roumen Petrov 1&2, Elke Leunis 3 and Leo Kestens 1&2
1
Materials Science and Engineering Department, Delft University of Technology
Mekelweg 2, 2628 CD Delft, The Netherlands.
2
Dept. of Metallurgy and Material science, Ghent University Technologiepark 903, Ghent, BE 9052, Belgium,
3
OCAS N.V., Arcelor Mittal research Industry, Ghent, Belgium

The <100> //ND crystallographic texture also known as the cube fibre texture is of both technical and
scientific importance because it contributes to favourable magnetic properties of BCC iron alloys. The <100>
directions are the axes of the spontaneous magnetic moments and therefore the directions of easy
magnetization. The <100>//ND cube fibre texture is easily obtained in FCC polycrystalline metals and alloys
by plane strain deformation and recrystallisation. In BCC metals and alloys this fibre texture is never obtained
throughout the thickness of material unless specific processing is employed such as directional solidification,
cross rolling or high temperature annealing. The frequently used methods to obtain <100> orientations // ND
in BCC alloys are based on various ferrite recrystallisation strategies. In contrast, the austenite-to-ferrite
phase transformation, which is an inherent and significant property of low-carbon steels, has scarcely been
investigated to develop cube texture. It is already known that Mn and Al alloyed ULC steels exhibit the <100>
// ND and <110>//ND texture on the cold rolled surface after D  J  D transformation under vacuum. It is
shown that this surface texture is predominantly controlled by the lowest surface energy plane at the gas/metal
interface. Although the exact dependence of the interfacial energy between the annealing atmosphere and the
ISRS-2008 67

steel surface on the crystal orientation is largely unknown, it has been widely accepted that the bcc {100}
and {110} planes display the lower surface energy. The interfacial energy of these planes can be varied by
selecting the furnace atmosphere during transformation annealing.
In the present study different atmospheres like vacuum, inert and reducing gas were used during
D  J  D transformation annealing for inducing a specific surface texture. X-ray diffraction (XRD) and
Orientation Imaging Microscopy (OIM) investigations were carried out on the surface, sub-surface and in
the bulk of annealed sheets to prove the development of the desired cube surface texture in various annealing
conditions.

MP-O3

THERMODYNAMIC ASSESSMENT OF THE Ni-Ti-Mo


TERNARY SYSTEM BY COMBINING FIRST-PRINCIPLES
METHOD AND CALPHAD APPROACH
Santhy K. and Hari Kumar K.C.
Indian Institute of Technology Madras, Chennai-600036

Understanding phase equilibria of Ni-Ti-Mo is important for widen its application in biomedical field.
The Ni-Ti-Mo is calculated by ternary extrapolation of the constituent binary systems. Thermodynamic
parameters of the binary systems were adopted from previous studies. To extend the homogeneity region of
binary phase into the ternary, the sublattice model for the binary phases were suitably modified. The enthalpies
of formation of hypothetical end-members of these phases are calculated from Ultra Soft Pseudo-Potential
with plane wave method. A set of model parameter for each phase are obtained using CALPHAD approach
by combining first-principle data with available experimental data. The calculated isothermal and vertical
sections are compared with experimental results.

MP-O4

LOW TEMPERATURE AQUEOUS SYNTHESIS OF EPITAXIAL ZnO:


THERMODYNAMIC CALCULATIONS AND OBSERVATIONS
Jacob J. Richardson and Fred F. Lange
University of California, Santa Barbara.

Low temperature synthesis from aqueous solutions is an attractive method of producing epitaxial ZnO
due to low cost and environmental impact as well the ability to perform bottom up patterning and sequential
processing on temperature sensitive substrates. The technique however suffers from the lack of a full
understanding of the solution behavior and the growth mechanism, which would allow for enhanced control
over the material produced. A simple thermodynamic model is detailed here for predicting the solubility and
speciation of Zn(II) in an aqueous solution. From these calculations it was found that dissolved ammonia
plays a critical role in the solubility of ZnO by forming relatively stable zinc amine complexes. It was also
found that ZnO should exhibit retrograde solubility with temperature under certain conditions. This behavior
is the basis for the construction of a continuous growth reactor. The design of this reactor and experimental
results are discussed in light of the thermodynamic calculations.
68 ISRS-2008

MP-O5
AB-INITIO CALCULATION OF ELECTRONIC STRUCTURE AND
STRUCTURAL PROPERTIES OF MgS
Gupta D.C., Sonia Mehra, Subhra Kulshrestha, Singh K.C. and Raypuriya G.S.*
Jiwaji University

DFT based ab-initio pseudo potential approach within local density approximation (LDA) using Siesta
code has been employed to compute the electronic structure of magnesium sulfide (MgS). The computed
band gap is found to be indirect and its value is in good agreement with experimental value. The phase stability
of MgS has also been computed using Siesta. This compound undergoes structural phase transition from B2)
under high pressure. The presently<71>rock-salt to cesium chloride (B1 computed values of lattice constant
and zero pressure bulk modulus and its pressure derivative are found to be in good agreement with
experimental data and better than those obtained by earlier workers. The band structure shows the
semiconductor nature of MgS.

MP-P1
A STUDY OF MAGNETRON SPUTTERED THIN FILMS OF TYPE 316
STAINLESS STEEL IN ARGON AND NITROGEN ATMOSPHERE
Akila1 B., Dona Amalorpavam1 M., Thirumurugesan R., Kuppusami P.*, Mohandas E. and Johnson I.
1
Physical Metallurgy Division, Indira Gandhi Centre for Atomic Research, Kalpkkam-603 102.
Department of Physics, St.Joseph’s College, Tiruchirappalli -620 002

Over the last decade, the use of nanostructured materials has already changed the approach to designing
materials in many applications by seeking structural control at the atomic level and tailoring mechanical
properties. It is also known that a strong refinement of the grain size can lead to additional increase of strength
due to the Hall–Petch relationship. With the emergence of methods to produce nanostructures, new routes to
enhance properties of metals and alloys have been reported. Type 316 austenitic stainless steel is a widely
used engineering material due to its excellent corrosion and oxidation resistance and good formability.
However, application of this material is hindered by its low mechanical strength and poor anti-friction
properties. Strengthening the stainless steel has drawn much attention in the past decades and various
approaches have been developed, such as varying its chemical compositions to induce solid solution
hardening and grain refinement. In the present work, thin films of type 316 austenitic stainless steel films
deposited on Si(111) single crystal and D-9 alloy substrates by pulsed DC magnetron sputtering in argon and
nitrogen atmosphere are investigated. X-ray diffraction of the films deposited with pure argon atmosphere
for different substrate temperatures indicate that there is only D-phase at lower temperatures (RT- 473K) and
D and J phases in the temperature range of 673-873K.The size of the nano-crystallites of both D and J phases
increase with increasing substrate temperature. The nickel content and deposition temperatures are crucial
factors for phase formation and phase stability.
XRD analysis of the films grown at different nitrogen flow rates indicate that the crystalline structure
of the films changed from bcc ferrite D, to nitrogen-stabilized fcc austenite J , then to expanded austenite
phase (also called S-phase) with nitrogen supersaturation, and finally to Fe4N phase. SEM studies at different
substrate temperatures confirmed coarsening of particles with increasing substrate temperature.
Nano-indentation results showed that there is an increase in the hardness of the deposited films than that of
the bulk stainless steel.
ISRS-2008 69

MP-P2
PHASE TRANSITIONS AND MICROSTRUCTURE OF
THERMO-RESPONSIVE NANOGEL DISPERSIONS
Brijitta J., Tata B.V.R. and Kaliyappan T.
Materials Science Division, Indira Gandhi Centre for Atomic Research, Kalpakkam, 603 102
1
Department of Chemistry, Pondicherry Engineering College, Pondicherry 605014.

Thermo-responsive nanogel dispersions are polymeric hydrogel particles containing cross-linked


three-dimensional networks dispersed in water. These particles exhibit sudden decrease in size beyond a
critical temperature known as volume phase transition (VPT). As a consequence, the volume fraction (f) of
these particles is tunable over a wide range by varying T but without changing the number density np of the
particles. Further, the interparticle interaction between the particles in the dispersion can also be tuned from
repulsive to attractive as a function of T. Hence these nanogel dispersions serve as an ideal condensed matter
system to study cooperative phenomena such as structural ordering and phase transitions by varying f and T.
Apart from the fundamental interest, these nanogel dispersions are studied with great interest due to their
practical applications: drug delivery, artificial muscles, photonic crystals, and sensors.
One of the fascinating phenomenon of these nanogel dispersions is that they freeze into a crystalline
order with lattice constants in the visible range. Hence static light scattering (SLS) is the appropriate tool to
investigate the structural ordering in these suspensions. The time scales associated with the motion of these
particles are in the dynamic light scattering (DLS) regime. The structural ordering of larger size particles
(diameter d > 300nm) can be investigated in real space using confocal laser scanning microscope (CLSM).
We report here, the results obtained using these techniques in thermo-responsive Poly
(N-isopropylacrylamide) nanogel dispersions with varying np and T.
We have synthesized monodisperse PNIPAM microgel spherical particles of two different sizes (d =
273 nm and d = 512 nm) in an aqueous medium by free radical polymerization method. From the mother
suspension, different samples with varying np were prepared by dilution. The np for samples S1, S2, S3 and
S4 are 4.36c 1011, 4.36c 1012, 8.71c 1013, 1.01c 1014cm3 respectively.

Volume phase transition


To study the effect of temperature on particle size, dilute sample S1 was prepared. This sample was
found to be non-interacting (gas-like) by performing SLS measurements. At T 25qC the average diameter
d of the particles was found to be 273 nm. The particle size was found to vary as a function of T. A
non-continuous collapse transition, known as volume phase transition (VPT) was found to occur at around
32qC [14]. This transition was found to be reversible upon lowering the T. Below the VPT these gel particles
are highly swollen in water, but upon increasing the temperature above the VPT they rapidly de-swell to a
collapsed polymer globule [1-4]. Because of this effect, on increasing the temperature from 25qC to 40qC
the particle size is found to decrease from 273 nm to 114 nm, which corresponds to about 93% change in the
volume of the particles. Below VPT water is a good solvent for the polymer whereas above VPT water turns
to be a poor solvent.

Melting/Freezing Transition
A concentrated suspension S3 upon repeated annealing above the VPT showed iridescence due to
Bragg diffraction of visible light. Iridescence in the samples suggests that particles order into a crystalline
state. SLS studies on this sample have revealed the occurrence of first Bragg peak at 2.84c 105 cm-1 from
70 ISRS-2008

which the lattice constant is determined to be 383nm. The melting transition of these crystals was identified
by monitoring the Bragg peak intensity, Imax as a function of T. For the first time, we found that the intensity
of the Bragg peak exhibits a sudden decrease at around 26oC. The sudden change in intensity is also associated
with loss of iridescence suggesting the melting of crystals into a liquid state at 26oC. Further we observed
that the first peak position to remain same across the meting transition suggesting no measurable change in
np across this transition. Though the phase behavior of PNIPAM nanogel dispersions closely resembles that
of hard-sphere colloidal system, the volume fraction f at which the crystallization appears is much higher f
was found to be 0.93 at 25qC and 0.85 close to the melting. Such high values of f suggest that PNIPAM
particles behave as soft spheres. This crystalline assembly of the nanogel particles can be used as a
thermo-sensitive photonic crystal and also as temperature sensor.
Fluid-Fluid transition
Upon further increasing the T of sample S3 beyond the melting point, the peak first peak intensity was
found to decrease and showed a change in slope at 30.5$C. Beyond 30.5qC, the structural ordering in the
suspension was found to be gas-like. The change in slope across 30.5qC was identified as fluid-to-fluid
transition temperature as the structure changes from liquid-like to gas-like without a change in np. From SLS
studies sample S2 is found to be liquid like ordered and this sample also exhibited a fluid-fluid transition
similar to that observed in S3 upon increasing T.
By analyzing the volume fractions across the transitions, we conclude that the observed phase behavior
is to due repulsive soft-sphere interactions.

Glass-like order: Sample S4 with np 1.01c 1014 cm-3 did not show iridescence. Further the ensemble
averaged electric-field correlation function f(q,t) as a function of time t obtained from DLS measurements
showed non-decay suggesting that the structural ordering in S4 is glass-like.

Microstructure of PNIPAM microgel crystal


We have observed crystallization in suspensions of 512nm particles. Since these crystals are relatively
turbid, we investigated the microstructure of these crystals using CLSM. We observed (111) planes of crystals
to be parallel to the coverslip having point defects and grain boundaries. The lattice constant of these crystals
is found to be 620nm with long-range order extending over several micrometers. Analysis of stack of optical
slices recorded along (111) direction (z-stacks) showed crystalline regions with FCC and HCP stacking. The
3D-pair correlation function calculated from particle positions, which are obtained by image analysis of the
z- stacks, have confirmed HCP structure.
To summarize we have synthesized monodisperse PNIPAM nanogel particles of different diameters
and observed variety of phase transitions as a function of T in samples of varying f. CLSM studies on large
size particles showed an overall HCP structure with domains of FCC and HCP co-existence.

MP-P3
STUDY OF PHASE TRANSITION IN SmTe THROUGH
AB-INITIO PSEUDO-POTENTIAL APPROACH
Gupta D.C., Subhra Kulshrestha, Sonia Mehra, Poonam Sharma and Ashok, Baraiya K.
Condensed Matter Theory Group, School of Studies in Physics, Jiwaji University, Gwalior-474 011

ab-initio pseudo-potential approach has been used to compute the structural properties of SmTe. In
this approach, we have used the local density approximation (LDA) that is based on exchange-correlation
ISRS-2008 71

energy optimization for calculating the total energy. The optimized lattice constant (a = 6.5936 Å) for SmTe
which agrees well with the experimental value (a = 6.6008 Å). This compound is found to be stable in B1
(NaCl structure) and undergoes a structural phase transformation to B2 (CsCl structure) under pressure. The
value of phase transformation pressure and zero pressure bulk modulus (PT = 13.64 GPa and B0 = 38.8 GPa)
show reasonably good agreement with their corresponding experimental data (PT = 12.9-14 GPa and B0 =
40 GPa). Beside this, we have also analyzed the change in the nature of bands at different pressures.

MP-P4
KINETICS OF HCP TO BCC PHASE CHANGE IN PURE TITANIUM :
EFFECT OF HEATING /COOLING RATES ON TRANSFORMATION
ASYMMETRY
Josephine Prabha1 A., Raju2 S., Jeyaganesh2 B., Arun Kumar Rai2, Mohandas2 E.,
Vijayalakshmi2 M. and Johnson3 I.
1
Bishop Heber College, Tiruchirappalli, 620017
2
Physical Metallurgy Division, Indira Gandhi Centre for Atomic Research, Kalpakkam, 603 102
3
St. Joseph’s College, Tiruchirappalli, 620 002 .
The kinetics of polymorphic changes in pure metals is a topic of both basic and applied interest. Albeit
having a long history with extensive investigations on various theoretical and experimental fronts, a firm
understanding of the structural transformation kinetics as dictated by microstructural and thermomechanical
constraints is still elusive. Facilitated by the recent developments in advanced in-situ experimental techniques
and also by the enhancements in the theoretical armory, certain basic issues connected with allotropic phase
change have resurfaced to offer further feed into applicable basic research. It is in this connection that we
have undertaken to study the kinetics of a hcp to bcc phase transformation in pure titanium using a
combination of thermal analysis and metallography.
It emerges that within the range of heating and cooling rates adopted in this study, namely 1 to 99 K
min-1, the on-heating transformation kinetics can be nicely accounted for by a standard KJMA
(Kolmogorov-Johnson-Mehl-Avrami) prescription of a simple nucleation and growth phenomenon, with of
course a mild heating rate dependent values for the apparent (overall) activation energy. It is further supposed
that there is a nice power-law scaling of the transformation kinetics with heating rate, if an Arrhenius
formulation of activation is considered phase nucleation and growth. On the contrary, the reverse
transformation bcc to hcp that occurs on cooling, despite showing a certain degree of superficial resemblance
to the on-heating one, is not described at all by the KJMA formalism. In fact, the observed kinetics is better
described by an empirical formalism attributed to Kamamoto, or to a lesser extent by the Koistinen-Marburger
relation for the martensitic mode, if the later stages of transformation are ignored. Apart from generating a
systematic dataset on the heating / cooling rate dependence of transformation characteristics, including the
nature of cooling rate dependent microstructural characteristics (grain size, hardness), the present study
brings out certain outstanding conceptual issues on the mechanics asymmetry between onward and reverse
transformation modes in simple polymorphic change.
72 ISRS-2008

MP-P5
PRESSURE INDUCED PHASE TRANSFORMATION
IN THORIUM PNICTIDES
Gupta D.C., Baraiya A.K., Singh K.C., Subhra Kulshrestha, Raipuriya G.S. and Sonia Mehra.
Condensed Matter Theory Group, School of Studies in Physics, Jiwaji University, Gwalior – 474 011
Department of Physics, Govt. Modal Science College, Gwalior – 474 001

Thorium pnictides (ThP, ThAs, ThSb) have NaCl (B1) structure at ambient condition and transform
to CsCl (B2) phase under pressure. The survey of the literature revealed that a wealth of measured data is
available on these compounds, but a very scant amount of theoretical works have been done on them. Earlier
works have, in general calculated the band structure or phase transition of these compounds. A modified
charge-transfer potential (MCTP) model has been developed to study the phase transition properties of ThX
(X=P, As, Sb) compounds. The present MCTP model consist of long-rang coulomb and charge transfer
interaction modified by covalency effect found in these compounds and short-range repulsive interaction
extended up to next-nearest neighbours. The present model have been used to compute the equilibrium lattice
parameters at zero as well as at high pressures in both the phases, cohesive energy ,phase transition pressure,
equation of state, volume collapse. The results on these transition pressure (PT = 29.76, 24.70 and 8.95 GPa)
shows a reasonably good agreement with the available experimental data (PT = 30, 25 and 9.12 GPa) for
these pnictides. The equation of state in both NaCl (B1) and CsCl (B2) structure has also V(P)/V(0)) ' been
obtained. The calculated value of the volume collapse ( at the phase transition (9.45, 9.7 and 14.62%) are
closer to the experimental data (11.9, 10 and 9.4%).

MP-P6
PHASE TRANSITION AND THERMAL PROPERTIES
OF SULFIDES OF Ca, Eu AND Th
Gupta D.C., Kailash, Singh C., Raipuriya# G.S., Baraiya* A.K., Subhra Kulshrestha and Sonia Mehra,
Condensed Matter Theory Group, School of Studies in Physics,
Jiwaji University, GWALIOR – 474 011 (M.P.) INDIA
School of Studies in Physics, Jiwaji University, Gwalior-INDIA

We have investigated the pressure induced structural phase transition in sulfides of Ca, Eu and Th by
means of modified charge-transfer (many-body) potential (MCTP) model. This model includes effects due
to long-range attraction due to Coulomb, charge-transfer mechanism and covalency effects and short-range
overlap repulsion extended up to next nearest interactions and zero point energy. It is interesting to note that
the present MCTP model is capable to explain the Cauchy-violations C12  C44 z 0 . These compounds
undergo structural transition from six-fold coordinated NaCl (rock-salt) to eight-fold coordinated CsCl phase
under high pressure. The computed values of the phase-transition pressure (PT = 39.23, 20.25 and 18.75 GPa)
shows reasonably good agreement with the available experimental data for CaS, EuS and ThS, respectively
and better than the values computed earlier. The calculated values of relative volumes V(P)/V(0) associated
with compression have also been obtained and plotted in figures to depict the phase diagrams / equation of
state for these sulfides. The phase-transition volume collapses at transition pressure are 10.32%, 11.70%, and
8.90% for CaS, EuS and ThS, respectively. The pressure variation of second order elastic constants
C11,C12 and C44 and there combinations BT C11  2C12 /3, CL C11  C12  2C44 /2 a n d
CS C11  C12 /2 is computed and depicted in figures. It is found that they also show a change at transition
ISRS-2008 73

pressure. Besides this, we have T), T calculated the thermal properties, i.e., Debye-temperature ( m. It is found
that the present model, which hasaverage wave velocity less parametric (range U , hardness (b) and charge
transfer potential (fm)) nature, is capable of predicting mechanical and thermal properties of sulfides of
alkaline/rare earth materials.

MP-P7
MATHEMATICAL MODELING OF CARBOTHERMAL
REDUCTION OF ILMENITE
Manju M.S., Savithri S
University of Kerala
A novel mechanism for the carbothermal reduction of Ilmenite in a rotary kiln reactor is proposed and
validated with a mathematical model. The proposed mechanism involves two solid state diffusion processes
namely the diffusion of atomic carbon through the metallic iron layer and the diffusion of oxygen through
the oxide (mainly rutile) phase. It has been reported by many researchers that the diffusion of CO gas to the
oxide phase is inhibited by the formation of a dense metallic iron product layer around the surface of the
particle. Hence in the present study oxygen diffusion is assumed to be rate controlling. A mathematical model
is developed to evaluate the rate of reaction of a single Ilmenite spherical particle. The results of modeling
are validated with the experimental data reported in literature for reduction of ilmenite in commercial rotary
kiln reactors. It has been observed that the reduction rate increases with temperature at constant pressure.
The excellent agreement of modeling results with experimental data confirm that the oxygen diffusion
towards the oxide/iron interface acts as the rate determining step during the carbothermal reduction of ilmenite
in a rotary kiln reactor.
74 ISRS-2008

=0=>B284=240=3C427=>;>6H8
N1-O1
DEFORMATION STUDIES OF NANOCRYSTALLINE NICKEL AND
NICKEL-ALUMINA COMPOSITES BY MICRO-INDENTATION
Pradipta Ghosh and Atul Chokshi H.
IISc Bangalore

In this study the mechanical behavior of nanocrystalline nickel and nickel-alumina composites was
investigated over a range of grain size (12nm to bimodal). The nanocrystalline materials were obtained by
pulse-electrodeposition technique. A special surfactant was used for codepositing Al2O3 particles with
nickel. The isothermal stability of both deposits was characterized at 523 K. It was observed that Al0O3
particles retarded the grain growth kinetics at 523 K, despite their large sizes.
Microindentation tests with constant loading rate to load ratio were done at 303 K for understanding
the strain rate effect and deformation mechanisms in these materials. A four fold increase in the strain rate
sensitivity was observed ~ 0.01 to~ 0.04 for both nanocrystalline nickel and nickel-alumina composites,
compared to coarse grain nickel. It was suggested that grain boundary contribution may be playing a
significant role below 16 nm for nanocrystalline nickel. This was supported by the activation volume (V*)
measurements. It was observed that, V* increases gradually from ~5b3 to ~100 b3 (b, burger’s vector) with
increasing grain size beyond 12 nm, suggesting a gradual change of deformation mechanism.

N1-O2
DEVELOPMENT & CHARACTERISATION OF POLYURETHANE
PROTECTIVE AUTOMOTIVE COATINGS INCORPORATING
LAYERED NANOSILICATES & FUMED SILICA
Gaurav Verma*, Anupama Sharma and Anup Ghosh K.
Panjab University Chandigarh

Advent of new models and glittering colours in the passenger cars and other vehicles is the prerogative
of the highly competitive automobile industry. Apart from the exterior shape the finish attracts the consumer
the most. Various industries catering to the automotive coatings are facing challenges in clearcoats. The
clearcoat is the coating layer that forms the last interface to the environment. It should have unchanged high
gloss and color stability over a long period and must be able to resist environmental etch, bird droppings, car
wash machines and other outside influences like industrially generated chemicals & pollutants. Attempt has
been made to in-situ polymerize a two pack Polyurethane consisting of a polyol & isocyanate with
incorporation of layered silicates (MMT, O-MMT, Cloisites & Bentone 38) in low loadings (0-5wt %) to
improve the barrier properties and solvent resistance. The first challenge faced is proper dispersion,
distribution & homogenization of layered silicates into the two pack system to get optimum properties. This
is tackled by use of combination of mechanical, magnetic mixers as well as ultrasonication and confirmed
by XRD analysis. The effect of various organic solvents on the ‘macroscopic swelling’ of layered silicates
has been investigated apart from increasing the interlayer distance. The organic modification of MMT into
OMMT is also shown by FTIR and XRD. The barrier properties and swelling kinetics have been studied and
improvements observed by incorporation of layered silicates. This improvement is related to proper
dispersion and distribution of layers of silicates in PU system.
ISRS-2008 75

After incorporation of fumed silica (average size less than 100nm) as filler in very low weight % (0-2
wt %) it was found to improve anti graffiti properties and accomplish ‘easy cleaning coats’. Kept in
environment over specific periods of time fumed silica nanocoatings shows better resistance. At weight %
above 3wt% adhesion tests failed. Low weight % addition of either layered silicates or fumed silica in PU
system doesn’t affect the ‘clarity’ of coatings if the dispersion and distribution is uniformly achieved.

N1-O3
FLUORINE DOPED TiO2 NANOCATALYST
FOR DEGRADATION OF AN ORGANIC POLLUTANT
Sivarajasekar N., Saravanan K., Velmani N.
Kongu Engineering College/ Anna University

In this study tetra butyl titanate was used as a precursor, and Anatase fluoride doped TiO 2 sol
F  TiO2 catalyst was prepared by a modified sol-gel hydrothermal method. The influences of F doping,
temperature of hydrothermal, values of medium pH on the morphology and crystallization were studied. The
microstructure and morphology of sol sample were characterized by XRD, TEM, UV–Vis–DRS, and particle
size distribution (PSD). The results showed that F  TiO 2 nano particles in sol were spherical and partly
crystallized to anatase structure, and dispersed in the aqueous medium homogeneously and that the average
particle size was ca. 10.2 nm calculated from XRD and TEM results. It was also found that the crystallization
and adsorption of particles significantly improved by addition of fluorine. The batch reactor experiments
showed that the photocatalytic activity for decomposition of phenol was enhanced remarkably with the doping
of fluorine.From batch reactor data, it was known that the rate of degradation followed the first order kinetics

N1-O4
HIGH TEMPERATURE TENSILE BEHAVIOR OF
ELECTRODEPOSITED NANO-Ni-P ALLOY
Prasad M.J.N.V. and Chokshi A.H.
Department of Materials Engineering, Indian Institute of Science, Bangalore – 560 012, India

Nano Ni-P alloy foils were synthesized by pulsed electrodeposition from Watts bath with phosphorous
acid (H3PO3) as a source of phosphorous. Nano-Ni-P foils with a grain size down to 3 nm were obtained
with saccharin (sulfur based organic compound) in bath. The thermal stability of the as deposited nano Ni-1.1
at% P alloy with an as-deposited grain size of 6 nm and a nano Ni-2.4 at% P alloy with an as-deposited grain
size of 3 nm was studied using differential scanning calorimetry and isothermal annealing. The high P alloy
with a larger fraction of Ni3P particles exhibited sluggish grain growth. The nano Ni-P alloy samples with
two different P levels, with the same grain size, were tested under tension at different temperatures and strain
rates. The Ni-1.1 P exhibited almost zero ductility at 573 K and it exhibited superplasticity with 470 %
elongation at a temperature of 777 K and at a strain rate of 3 u 10 3 s 1. The Ni- 2.4 P also exhibited
superplasticity at 777 K, with a higher elongation to failure of 890 %. There was significant grain growth
during the heating up to test temperature so that the initial grain sizes just before testing at 777 K were ~300
nm and 200 nm in the low P and high P alloys, respectively. Strain rate jump tests yielded a strain rate
sensitivity m of ~0.5. Microstructural characterization of the fractured specimens indicated considerable
grain growth and cavitation near the fracture tip.
76 ISRS-2008

N1-O5
SYNTHESIS, ELECTRICAL AND DIELECTRIC PROPERTIES OF THE
NANOCRYSTALLINE Ce0.8Eu0.2O2-8
Ashok Kumar Baral and Sankaranarayanan V.
Indian Institute of Technology Madras, Chennai

In the recent years, the fluorite structured nanocrystalline materials of pure and doped ceria have
attracted much attention for being studied and improved the electrochemical properties for the application
in intermediate temperature solid oxide fuel cell (SOFC). In this work, the nanocrystalline material of 20
mol% europium (Eu) doped ceria Ce0.8 Eu0.2 O2  G with average grain size of 12 nm is synthesized by
citrate complex method. The phase purity and microstructure of the material are studied using powder XRD
and HRTEM. The material is found to be ionic in nature with ionic conductivity of 1.39 u 10  4 Scm  1 at
550qC. The material shows two different temperature regions of conductivity with activation energies 1.13
and 0.91 eV below and above 470qC respectively. The electric modulus spectra show the presence of a
relaxation peak corresponding to bound motion of oxygen vacancy around the Eu+3 ions in the lattice. The
migration energy of the oxygen vacancy in the long range motion is found to be 0.77 eV whereas association
energies are found to be 0.36 and 0.14 eV in two different temperature regions.

N1-P1
ELECTRICAL RESISTIVITY AND MORPHOLOGICAL PROPERTIES
OF PP/MMT/OMMT HYBRID NANO COMPOSITES
Rajarajan S., Raja J.
Sathyabama University, Chennai

The preparation of hybrid polymer nanocomposites by melt compounding Polypropylene(PP) with


montmorillonite(MMT) and organically modified montmorillonite(OMMT)using polypropylene grafted
maleic anhydride(PP-g-mA)as compotibilizer is described.Compositions with MMT and OMMT content
1%,3%,5% and 7% were prepared and tested.The influence of nanoclays on morphology of the
nanocomposites was studied by Scanning Electron Microscopy(SEM).
The results of this investigation of surface resistivity and volume resistivity of polymer hybrid
nsnocomposites are presented.

N1-P2
CHARACTERIZATION OF CdS-ZnS NANOCOMPOSITES
SYNTHESIZED BY MICROWAVE-ASSISTED SOLUTION METHOD
Selvarajan P., Kumar E. and Balasubramanian K.
Aditanar College of Arts and Science, Tiruchendur, Tamil Nadu

In the recent years, nanoscience is an intense and rapidly developing field. Due to the arrangement of
atoms or molecules on the 1 to 100 nm scale, nanocrystalline materials possess unique and interesting
mechanical, optical, electrical, magnetic, thermal and other properties. Nanocomposites are also possessing
unique properties like pure nanomaterials. In this work, We report the synthesis of nanocomposites of
CdS-ZnS by wet chemical method using a microwave oven. The precursors used were cadmium nitrate, zinc
ISRS-2008 77

nitrate and thiocarbamide. The capping agent used to control the size of nanoparticles was ethylene glycol.
At different pH values (10, 12, 14) , the nanocomposites of CdS-ZnS were prepared. The synthesized
nanocomposites were centrifuged, filtered, washed and dried.
The nanocomposites were characterized by powder XRD, SEM, TEM, atomic absorption, dielectric
and conductivity studies. Powder XRD studies reveal the hexagonal structure of nanocomposites and the size
of nanoparticles was estimated to be below 100 nm. The morphology of most of the nanoparticles was
observed to be spherical from SEM and TEM studies. The synthesized nanocomposites of CdS-ZnS were
pelletized and dielectric and conductivity studies were carried out. The obtained results from various studies
are presented and discussed.

N1-P3

TEMPERATURE DEPENDENT PROPERTIES OF NANO CERIA THIN


FILMS PREPARED BY PULSED LASER DEPOSITION
Balakrishnan1 G., Kuppusami* P., Thirumurugesan R., Mohandas E., Chandramohan2 P.,
Srinivasan2 M.P. and Sastikumar D.
1
Physical Metallurgy Division,
2
Water and Steam Chemistry Division, BARCF, Kalpakkam-603 102, Tamilnadu
1
National Institute of Technology, Tiruchirapalli-620015, Tamilnadu

Cerium Oxide CeO2 or Ceria is an ionic metal oxide in the visible and near infrared (VIS-NIR)
spectral region. It possesses physical properties such as high refractive index (2@ 500 nm), large dielectric
constant (~26), wide band gap (3.6eV), good transparency, chemical stability, good adhesion, hardness and
thermal stability. Also, CeO2 exhibits cubic structure with a lattice parameter (a= 0.541nm), matching with
silicon. Hence CeO2 thin films have been extensively used as ultra thin gate oxide in CMOS technology,
stable capacitor devices for large scale integration, stable buffer layers between high temperature
superconducting materials and silicon substrates, single and multilayer coatings for optical devices,
electro-chromic windows , oxygen sensors, solid oxide fuel cells, dynamic random access memory (DRAM),
and corrosion resistant coatings.

CeO2 thin films have been prepared by pulsed laser deposition technique using KrF excimer laser of
248 nm wavelength with a repetition rate of 10 Hz. The sintered ceria pellet was used as target material and
Si (100) and glass were used as substrates. The films were prepared at various temperatures with an optimized
oxygen partial pressure of 3 u 10 2 mbar. In the present study, the influence temperature on the structural
and optical properties of the films were investigated. The x-ray diffraction (XRD) analysis showed that the
films were polycrystalline with cubic structure. The crystallite size increased from 19 to 50 nm in the
temperature range RT- 973 K. At room temperature, the intensity of (111) reflection was maximum and at
an increased temperature in the range 573-973 K, the (200) reflection was predominant. The texture
coefficient for the (200) reflection increased with the increase of temperature. The Raman studies showed a
peak appeared at ~ 463 cm-1 due to the F2g Raman active mode of CeO2 cubic structure. However, there
was no peak in the Raman spectrum for the films prepared at room temperature because of poor crystallinity.
When the temperature was in the range 573 K-973 K, the Raman shift was observed from 459 to 464 cm-1.
The trend observed in the FWHM of Raman lines are in agreement with our XRD study. The optical studies
have been carried out using UV-VIS-NIR spectrophotometer with a wavelength range of 190-3000 nm. A
small variation in the band gap energy from 3.0 to 3.3 eV was noticed.
78 ISRS-2008

N1-P4
RAMAN SPECTROSCOPIC INVESTIGATIONS
ON NANOSTRUCTURED ZINC FERRITE
Singh J.P., Gagan Dixit, Srivastava R.C. and Agrawal H.M.
G. B. Pant Univ. of Agriculture & Technology, Pantnagar, Uttarakhand (India)

Zinc ferrite has normal spinel structure, in which all ferric ions remain at octahedral site and zinc ions
at tetrahedral site. It is paramagnetic at room temperature in bulk form. This material exhibits unusal physical
and chemical properties when size is reduced to nano regime. Due to its interesting properties in nanoregime
this material is widely studied to understand the underlying physics. The present investigation aims to study
the microstructural state and other local environment of this material through the Raman spectroscopy.

Zinc ferrite was synthesized by using the nitrate route [1,2]. The precursor for the present investigation
was sintered at 400qC, 500qC, 700qC, 900qC and 1000qC. The particle size at these sintering temperatures
were found to be 12, 16, 18, 31 and 62 nm respectively by using the Scherrer’s formula. TEM micrograph
also supports the particle size estimated from XRD pattern. We have recorded the Raman spectra for all the
samples in the range 200-1500 cm-1. The Raman system used for the present study consists of Ar-ion laser.
The laser power used for recording the spectra is 5 mW. As zinc ferrite belongs to Oh7(Fd3m) space group,
it should exhibit five Raman active modes: A1g Z 669cm  1 , Eg Z 410cm  1 and 3T2g
Z 193cm  1, 300cm-1, 540cm-1) [3]. The recorded spectra were Lorentz fitted and the values of several
Raman modes are estimated. A visual inspection shows that all spectra consist of three bands in the 200-800
cm-1. It may be concluded that due to broadening of the Raman bands other active modes may merge together.
For the present case no Raman band is observed at 1320 cm-1 which rules out the presence of Fe2O3 in our
samples.

N1-P5
EFFECT OF ANNEALING ON THE SURFACE MORPHOLOGY OF ZnO
NANORODS GROWN ON POROUS SILICON SUBSTRATE
Amizam13 S., Rafaie1,3 H.A., Mamat 2,3 M.H., Khusaimi1,3 Z., Sahdan2,3 M.Z., Abdullah1,3 S. and Rusop2,3 M.
1
Faculty of Applied Sciences,
2
Faculty of Electrical Engineering,
3
Centre for Nanotechnology Laboratory (NANO-SciTech), Institute of Science,
University Technology MARA, 40450 Shah Alam, Malaysia

The effect of annealing on the surface morphology of ZnO Oxide (ZnO) Nanorods grown on Porous
Silicon (PSi) substrate was studied. The zinc nitrate hexahydrate (Zn(NO3)2.6h2O) and hexamethenamine
(C6H12N4) was synthesized . A homogenous and stable solution was prepared by dissolving the
Zn(NO3)2.6h2O in a solution of DI water and hexamethenamine. The molar ratio of nitrate solution and
hexamethenamine is 1:1. Afterthat the immersion method used to prepare the ZnO Nanorods on PSi. The
samples were annealed at 200, 400, 600 and 800qC for 60 min. The surface morphology and optical properties
of the samples was characterized using Scanning Electron Microscope (SEM) and photoluminescence (PL)
spectroscope. The result indicated that the ZnO Nanorods morphology is most sensitive to the temperature.
Room-temperature PL measurements shows the ZnO nanorods exhibit a strong ultra-violet (UV) emission
of 400 nm and several weak emissions in the blue and green bands.
ISRS-2008 79

N1-P6
MAGNETOCAPACITANCE, MAGNETORESISTANCE AND
MAGNETOSTRICTION STUDIES OF NANOSIZED NiZn FERRITE
SYNTHESIZED BY HIGH ENERGY BALL MILLING
Sreenivasulu1 G., Markandeyulu2 G., Murty1 B.S.
1
Dept. of Metallurgical and Materials Engg. and 2Dept of Physics,
Indian Institute of Technology Madras, Chennai-600036.
Ni Fe1.98O4\ Ni (1-x) ZnxFe1.98O4 (x = 10, 20, 30, 40 and 50 mol %) were synthesized by high energy
ball milling with the starting materials were NiO (99.9% pure), Fe2O3 (99.5% pure), CoO (99.9% pure). The
milled powders were compacted and sintered at 1200qC. The phase formation was confirmed by X-ray
diffraction technique. The X-ray densities were calculated and were compared with bulk densities of the
sintered samples were about 97-99%. The nanocrystallinity is retained even after sintering and this has been
confirmed by atomic force microscopy (AFM) and transmission electron microscopy (TEM). The effect of
Zn content on DC resistivity, magnetization, magnetocapacitance, magnetoresistance and Magnetostriction
were studied. DC resistivities were measured with Keithley electrometer and were found to be in the range
of 108 to 109 :-cm, which is 2 to 3 orders of magnitude higher than Zn free ferrite (106 to 107 :-cm). The
magnetization measurements were carried out with the help of vibrating sample magnetometer. The
magnetization increased from 51 to 77 emu/g with increasing Zn content as compared to the pure Ni ferrite
(46 emu/g). Magnetocapacitance (8%), magnetoresistance (10%) and Magnetostriction measurements were
carried out with the electromagnets at a sweeping field of 1tesla. Raman spectroscopy analysis has been
carried out to correlate the site occupancies of the individual elements with the magnetic moment to
understand the influence of Zn.
80 ISRS-2008

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N2-O1
CHARACTERIZATION AND CONDUCTIVITY STUDY OF
POLYPYRROLE NANOROD SYNTHESIZED BY INTERFACIAL
METHOD IN POLYVINYL ALCOHOL MATRIX
Bhadra J., Sarkar D.
Gauhati University

The intriguing optic and electronic properties of - conjugate back bone conducting polymers have
captivated much interest in the scientific community. We report here the polymerization of pyrrole by
interfacial method in polyvinyl alcohol (PVA) matrix taken pyrrole and PVA in the ratio of 1:100 by weight.
The surface morphology study was done by FESEM, which shows fine nanorods of approximate length of
2ìm and diameter of 50 nm. Further the films are characterized by FTIR, UV, XRD and PL for optical study.
The FTIR results significants peaks for interlinking of polypyrrole (PPY) and PVA molecules. The UV spectra
shows characteristic peak PPY-PVA at 284 nm. And PL spectra shows at excitation wavelength 344 nm
emission occurs at 692 nm. The films show homogeneous structure with good electrical properties and non
ohmic I-V characteristics.

N2-O2
EVIDENCE OF FORMATION OF ZnO NANOCLUSTERS
IN VAPOR PHASE
Antaryami Mohanta and Raj, Thareja K.
Indian Institute of Technology, Kanpur

Pulsed laser ablation technique is an efficient way of depositing high quality thin films of various
materials such as metals, semiconductors, and ceramic for a variety of applications. Growth of ZnO thin films
by pulsed laser deposition technique has been made increasing attention amongst the researchers recently,
because ZnO is a promising semiconductor materials for optoelectronic devices in the ultraviolet range due
to its wide band gap (~ 3.37 eV) and its high excitonic binding energy (~ 60 meV) which assures the lasing
action due to possibility of excitonic recombination at room temperature (~ 25 meV). As laser ablated plasma
is the main source of pulsed laser deposited thin films, a detailed investigation on the physical and chemical
properties of the laser ablated species are inevitable. A third harmonic of Nd: YAG laser [355 nm, pulse-width
of 5 ns, 10 Hz repetition rate] is used for ablation of a sintered target of ZnO (99.999 % purity) to produce
plasma in air. The plasma expands in air; the species of ZnO plasma collides with the molecules of air which
slows down the species inducing rapid cooling of plasma and initiation of chemical reactions, electron-ion
recombination, production of clusters etc. In this abstract, an evidence of formation of ZnO clusters in ZnO
plasma by photoluminescence (PL) technique and by Rayleigh scattering experiment is reported. In order to
observe the photoluminescence, the fourth harmonic of a Nd:YAG laser [266 nm, pulse-width of 4 ns, 10 Hz
repetition rate] referred as probe beam is passed through the ZnO plasma perpendicular to the expansion axis
of plasma at various distances from the target surface and at various time delays with respect to the ablating
pulse. The emission spectra are recorded by imaging on to a fiber placed perpendicular to the axis of both
the beams, and the other end of the fiber is coupled to the entrance slit of a monochromator. An Intensified
charge coupled device (ICCD) is used at the exit slit of the monochromator in order to record the spectra. An
ISRS-2008 81

emission spectrum at 1 ìs delay of probe pulse (266 nm) with respect to the ablating pulse is observed which
shows the Zn I transition lines along with a broad-emission band. This broad-emission band falls in the
spectral region of PL band of ZnO and is attributed to the PL from gas-suspended ZnO clusters. As the delay
time of the probe pulse with respect to the ablating pulse increases, decreasing intensity of the Zn I transition
lines with increasing PL intensity is observed. This shows an evidence of formation of ZnO clusters in ZnO
plasma. On the other hand, Rayleigh scattering of visible radiation has widely been used for verification of
the existence of clusters. Therefore, a second harmonic of Nd: YAG laser [532 nm, pulse-width of 6 ns, 10
Hz repetition rate] referred as probe beam is passed perpendicular to the expansion axis of plasma at various
distances from the target surface and at various time delays with respect to the ablating pulse (355 nm), and
the emission spectra are recorded. The Zn I transition lines are observed at 500 ns delay with respect to the
ablating pulse without passage of the probe pulse (532 nm). When probe pulse (532 nm) is passed
perpendicular to the expansion axis of plasma at 500 ns delay with respect to the ablating pulse, a signal at
532 nm, referred as Rayleigh scattered signal is observed along with the ZnI transition lines. On increase of
delay time of probe pulse with respect to the ablating pulse, decreasing intensity of Zn I transition lines with
increasing intensity of the scattered signal is observed. At 2 MUs delay of probe pulse with respect to the
ablating pulse, the scattered signal dominates the Zn I transition lines. At higher delay (~ 5 MUs) of the probe
pulse with respect to the ablating pulse, only the scattered signal is observed with complete suppression of
Zn I transition lines. This shows the evidence of formation ZnO clusters due to cooling of plasma by collision
of the laser ablated ZnO species with the molecules of the ambient (air) and the signal observed at 532 nm
is the scattering of the probe pulse by the gas-suspended ZnO clusters.

N2-O3
PHYSICAL AND OPTICAL PROPERTIES OF NANOSTRUCTURED
ZnO DEPOSITED ON SILICON DIOXIDE CATALYST
USING DIFFERENT THICKNESS
Sahdan M.Z., Kamaruddin S.A., Mamat M.H., Amizam S., Rafaie H.A., Khusaimi Z., Hashim Saim,
Noor U.M., Ahmed A.Z., Abdullah S., Rusop M.
University. Teknologi MARA Malaysia
Nanostructured materials have been researched recently due to their novel properties compared to their
bulk materials. Nanostructured ZnO has been grown using various techniques since difference techniques
would produced different nanostructures. This paper presents new approach of using silicon dioxide
SiO2 as catalyst in sol-gel method to grow nanostructured ZnO. The physical and optical properties of
nanostructured ZnO deposited using this approach is studied and the correlation between the catalyst
thickness and the material properties will be discussed. The physical characterization using scanning electron
microscope (SEM) and x-ray diffractometer (XRD) shows different SiO2 thickness has produced different
ZnO nanostructures. The optical properties using UV-VIS-NIR and photoluminescence (PL) spectrometer
have shown ZnO is very sensitive at ultraviolet (UV) region. This UV emission and absorption is strongly
correlated with the surface morphologies and crystallite size.
82 ISRS-2008

N2-O4
SYNTHESIS AND CHARACTERIZATION OF EDTA
CAPPED ZnS NANOPARTICLES
Vijai Anand K., Karl Chinnu M., Marx Nirmal R., Mohan kumar R., Alagesan T., Pandian K., Mohan R., Jayavel* R.
Presidency College, Chennai

The study of nanomaterials provides an opportunity to observe the evolution of material properties
with crystal structure, size and shape. The synthesis of nanomaterials is an ultimate challenge of modern
material research that has an outstanding fundamental and potential technological consequence because of
their special properties such as large surface to volume ratio, increased activity, special electronic properties
and unique optical properties as compared to those of the bulk materials. Among a variety of semiconductor
materials, the binary metal chalcogenides of group II have been extensively studied because of their
outstanding potential applications owing to their non linear optical and luminescence properties, quantum
size effect and other important physical and chemicals properties. Among II-VI compound semiconductors,
ZnS is one of the important optoelectronic device materials which are used for a variety of applications such
as optical coatings, photoconductors, optic-modulators and electro-optic modulators owing to its wide band
gap energy. In this present work, we have synthesised Zinc sulfide nanoparticles by a simple chemical
co-precipitation method using disodium ethylenediaminetetraaceticacid (EDTA) as capping agent. The role
of EDTA was to stabilize the nanoparticle against aggregation and also to provide chemical passivation that
leads to a significant influence on the chemical, optical and electronic properties of nanoparticles. The
synthesized ZnS nanoparticles were characterized by X-ray diffraction (XRD), UV-Visible absorption, FTIR
and fluorescence emission spectra in order to study their crystal structure and optical behaviour.

N2-O5
CHEMICAL VAPOUR SYNTHESIS OF PURE AND DOPED
NANOCRYSTALLINE TITANIA AND ITS CHARACTERISATION
Imteyaz Ahmad Md a, Bhattacharya a S.S and Horst Hahn b
a
Department of Metallurgical and Materials Engineering,
Indian Institute of Technology Madras, Chennai- 600036, India.
b
Darmstadt University of Technology, 64287 Darmstadt, Germany and Director,
Institute for Nanotechnology, Forschungszentrum Karlsruhe GmbH,
Hermann-von-Helmholtz-Platz 1 76344 Eggenstein-Leopoldshafen, Germany.

During the last decade chemical vapour synthesis (CVS) has been projected as one of the viable
methods for the synthesis of high pure, nanocystalline ceramic powders with a good control over the resultant
powder characteristics. In this process, a metallorganic precursor is decomposed/pyrolysed within the
well-defined high temperature zone of a hot-wall reactor and the nanocrystalline powders synthesized therein
are collected by a suitable method. In the current work it was demonstrated that the chemical vapour synthesis
(CVS) route is a suitable method for synthesis of highly crystalline, strain-free and agglomeration- free pure
as well as doped/modified nanocrystalline titania. Titanium tetra isopropoxide was used as the precursor for
the synthesis of pure nanocrystalline titania, while triethyl boron and ammonium hydroxide were respectively
used as additional precursors for doping/modification of nanocrystalline titania with boron and nitrogen. The
powders synthesized were well below 10 nm with a narrow size distribution and exhibited a high degree of
crystallinity. The synthesised powders were characterized by the standard methods of x-ray diffraction, high
resolution transmission electron microscopy, nitrogen adsorption etc. as well as by using specialized methods
such as X-ray photoelectron spectroscopy, electron paramagnetic resonance spectroscopy, nuclear magnetic
resonance and UV-vis spectroscopy in case of the doped/modified powders. The results of the studies and
the conclusions drawn are reported.
ISRS-2008 83

N2-P1
MICROWAVE ASSISTED SYNTHESIS AND CHARACTERIZATION OF
EUROPIUM DOPED YTTRIUM OXIDE NANOPARTICLES FOR
LUMINESCENCE APPLICATIONS
Srinivasan R., Rajeswari Yogamalar N. and Chandra Bose A.
Department of Physics, National Institute of Technology, Tiruchirappalli - 620 015
Oxide nanomaterials have prospective applications in the field of phosphor industries. Rare earth doped
yttrium oxide (Yttria) nanomaterials are very important in the field of luminescence and phosphor materials.
The luminescence efficiency of these oxide nanomaterials are depends upon the crystallite size and synthesis
method also. These materials are prepared by various techniques such as hydrothermal, solvothermal,
co-precipitation, and combustion method. Here microwave synthesis is used for preparation of europium
doped yttria nanoparticles. In this method the reaction time is very short and controlling the particle size is
simple by changing the power level of microwave source. The domestic microwave oven is modified slightly
for holding the reflux condenser set up. The required amount of molar solution of yttrium nitrate and europium
nitrate was taken in round bottom flask and this is fitted with reflux condenser set up. The solution was heated
by microwaves with power 700 W and frequency 2.45 GHz for 30 minutes. Then the certain amount ammonia
is added with above solution. The precipitate is obtained and this precipitate is washed by water and dried.
The final powder is annealed at different temperatures. All the samples are characterized by XRD for particle
size, SEM for morphology, TEM for particle size, FTIR for structural study, and UV for band gap calculations.
All the result will be presented in the conference.

N2-P2
INFLUENCE OF NANO SIZE INERT FILLERS ON THE
TRANSPORT CHARACTERISTICS OF MECHANOCHEMICALLY
SYNTHESIZED NaSn2F5
Laxmi Narayana Patro and Hariharan* K.
Solid State Ionics Laboratory, Department of Physics, Indian Institute of Technology Madras, Chennai 600036, India
NaSn2F5 dispersed with nano size fillers such as Al2O3 and SiO2 of various concentrations have been
prepared through high energy ball milling at room temperature. XRD, DSC, and SEM result indicates the
biphasic nature of the samples. The transport properties of the samples have been investigated by means of
impedance spectroscopy. In the present investigation, Al2O3 fillers of different particle sizes (60nm, 1ìm)
have been used and it is found that the improvement in conductivity decreases with increase in the particle
size of the filler. An enhancement in conductivity of one order in magnitude is obtained for NaSn2F5 with
Al2O3 dopant concentration of 10 mol%. The activation energies for all the composites (0.900.02eV) are
close to the activation energy of pure NaSn2F5. The transport number measurement by dc polarization
technique with the cell of configuration Ag/ electrolytes /Ag reveals that the electronic transport number is
0.01. This indicates the enhanced conductivity in the present investigated system is due to F- ions. Further,
the impedance data have been analyzed in the frame work of complex permittivity and electric modulus
formalisms to obtain the better insight of the relaxation dynamics of the materials. The scaling result of the
conductivity and imaginary part of modulus shows the relaxation mechanism is independent of temperature.
84 ISRS-2008

N2-P3
SYNTHESIS AND CHARACTERIZATION OF Ce DOPED
ZnO NANOCRYSTALLINE
Ilanchezhiyan P., Mohan Kumar G., Subramaniam M. and Jayavel R.
Anna University, Chennai

Zinc Oxide is a wide band gap n-type semiconducting material having wide applications such as gas
sensors, optoelectronic devices, such as light-emitting diodes and solar cells. In this report, Ce doped ZnO
Nanorcrystalline thin Films have been synthesized using Spray Pyrolysis Technique onto Si (100) substrates.
XRD analysis is carried out to determine the crystal structure. The diffraction peak shifts towards the higher
angles as Ce is added which shows that it has entered the ZnO lattice and substituted Zn ion. Morphological
and luminescence property were carried out using Scanning electron microscope and photoluminescence.

N2-P4
SYNTHESIS AND CHARACTERIZATION OF METAL
SULPHIDE NANOPARTICLES BY THERMAL DECOMPOSITION
OF METAL COMPLEXES
Marx Nirmal R., Pandian K., Jayabalan K.
Anna University, Chennai

A detailed investigation has been carried out on synthesis and characterization of Metal sulphide
nanoparticles by thermal decomposition of metal complexes in presence of hexadecylamine. Different metal
complexes such as cadmium pyrrolidine dithiocarbamate complex and Zinc prrolidine dithiocarbamate
complex have been prepared by simple chemical route. The growth of metal sulphide nanoparticles (CdS,
ZnS) were synthesized by thermal decomposition on both normal and microwave heating of metal complex
in presence of Hexadecyl amine (HDA). HDA has the functioning of solvent as well as shape directing agent.
The prepared CdS and ZnS nanoparticles were characterized by X-ray diffraction (XRD), Laser Raman,
Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDX) and High resolution
transmission electron microscopy (HRTEM) studies. The optical properties of CdS and ZnS nanoparticles
were studied through UV-visible and fluorescence emission spectral techniques. The present work proposes
thermal decomposition technique as one of the simple way to synthesis large quantity of semiconductor
nanoparticles.

N2-P5
AQUEOUS SYNTHESIS OF Co DOPED CADMIUM
SULPHIDE NANOPARTICLES
Saravanan L., Tamil Selvan S., Pandurangan A., Jayave R.
Centre for Nanoscience and Technology, Anna University Chennai

Colloidal inorganic nanocrystals are of great interest both for fundamental research and technological
applications, due to their strong size and shape dependent properties and excellent chemical processibility.
The introduction of dopants and defects in solids has always been a problem of central importance to materials
science in view of their implications for device science and technology. In recent years, CdS nanostructural
materials have been widely investigated. In this work we have synthesised cobalt doped cadmium sulfide
ISRS-2008 85

nanocrystals with different cobalt concentration by aqueous precipitation method. Dopant incorporation was
recognized by X-ray diffraction (XRD) and the morphology was observed by scanning electron microscopy
(SEM). Variation in the luminescence properties was analysed using fluorescence spectroscopy and the results
will be discussed.

N2-P6
LOW TEMPERATURE SYNTHESIS OF SHAPE-
AND SIZE- CONTROLLED ZnO NANOSTRUCTURES BY
SOLVOTHERMAL TECHNIQUE
Saravana Kumar R., Sathyamoorthy* R., Sudhagar P., Matheswaran P., Mageshwari K.
PG and Research Department of physics, Kongunadu Arts and Science College,
Coimbatore - 641 029. Bharathiar University
In recent years, Zinc oxide (ZnO) nanostructures have been extensively investigated due to their great
potential for fundamental studies of the effects of morphology, dimensionality and size on the materials
properties as well as for their application in optoelectronic nanodevices. In the present work, ZnO
nanoparticles with different surface morphology were obtained by solvothermal reaction technique without
using surfactants. The influence of solvent and reaction temperature on the growth of nanoparticles was
studied. ZnO nanoparticles prepared under different solvent showed that the polarity of solvent and the
reaction temperature greatly influences the growth of the nanorods. X-ray diffraction (XRD) patterns exhibit
hexagonal wurtize structure. Transmission electron microscopy (TEM) showed single crystalline nature of
the nanorods. Optical band gap energy was calculated by diffused reflectance spectroscopy. Presence of defect
levels and excitons emission behavior of ZnO nanostructures were investigated by photoluminescence (PL)
spectra. Both optical and PL spectra reveals the quantum confinement effect. The results are discussed based
on growth mechanism.
86 ISRS-2008

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N3-O1
STRUCTURE AND PROPERTIES OF POLY (BUTYLENE
SEBACATE-CO-BUTYLENE ISOPHTHALATE)/CLAY
NANO-BIOCOMPOSITE.
Siva kumar* G., Nanthini R. and Suganya G.
*Department of Chemistry, Panimalar Engineering College, Chennai-602103 Post- Graduate and Research
Department of chemistry Pachaiyappa’s College, Chennai 600030

Aliphatic-aromatic biodegradable random copolyester, poly (butylene sebacate-co-butylene


isophthalate) PBSeI was synthesized by a two step direct melt polycondensation method. This copolyester
was characterized by solubility, viscosity measurements, IR, 1H NMR, 13C NMR and thermal studies. But,
to be a real alternative to classical synthetic polymers and find applications, biodegradable polymer properties
have to be enhanced. Synthesis of nano–biocomposites, which are obtained by incorporation of nanofillers
in to a biomatrix, is an interesting way to achieve the polymers with characteristic properties. In present study,
the bio nanocomposites were synthesized by dispersing different weight percentage (1, 3 and 5%) of Organo
modified montmorillonite clay (OMMT) into the biodegradable polyester matrix by solvent intercalation
method. The structural characterization and thermal analysis have been carried out to understand better the
relationship between the nanofillers structuring and the properties of nano-biocomposites. The X-ray
diffraction patterns obtained for the systems confirmed the nanodispersion of OMMT-clay in the polyester
networks. The results show that the clay incorporation enhances the thermal properties of PBSeI due to the
exfoliated structure of the nanocomposites formed, and thus may increase the applicability of this
biodegradable polymer in different fields.

N3-O2
DESIGN AND CHARACTERISTICS OF A BURNER
FOR THE CONTROLLED PRODUCTION OF NANOPARTICLES
IN A FLAME REACTOR
Manjith Kumar B, Bhattacharya S S and Shet U S P
Indian Institute of Technology Madras, Chennai.

The study of nanoparticles has invited the attention of researchers across the globe due to the possibility
of developing unusual properties, which are often not obtained in the conventional bulk form. Since these
properties are closely dependent on the size and morphology of the synthesized powders, efforts are on to
develop effective methods for producing nanomaterials in relatively large quantities with controlled size and
morphology.
Flame reactors are among the most promising gas phase synthesis routes to large volume production
of submicron and nanosized particles. They offer reasonably good control of the product particle properties,
short process chains, a self-purifying high temperature synthesis environment, and a wide product range. In
principle, these reactors contain diffusion burners within a reaction chamber. The burner consists of concentric
tubes for the independent passage of the precursor, a dilutant medium, fuel and an oxidizer gases. The gases
flow through the tubes to reach the burner head, where they mix and facilitate burning and
ISRS-2008 87

combustion/pyrolysis of the precursor resulting in the production of nanoparticles of interest. These


nanoparticles are then collected by a suitable system. The flame characteristics play an important role in
deciding the size and morphology of the nanoparticles.
In this work the design and characteristics of a burner to be used for the controlled production of
nanoparticles in a flame reactor was studied. It is expected that the velocity differences at the burner outlet
would influence reactant mixing and, therefore, the nucleation and onset of particle growth. The flame height,
on the other hand, would decide on the residence time and the extent of particle growth. A brass burner,
suitable for the synthesis of oxide nanoceramics (such as titania or alumina) was designed and fabricated.
This was initially tested for flame stability using acetylene as fuel and oxygen as oxidizer. The gas flow rates
were regulated and controlled using standard flow meters. The minimum and maximum gas flow rates and
flow velocities at which the flame was stable and soot-free were determined, thus giving an idea of the stable
region of operation. The flame heights were measured at the beginning of an oxidation flame as well as at
the point where the flame started to become discontinuous and was repeated for different flow rates. The
results of these studies are reported.

N3-O3
SYNTHESIS OF PURE AND CO DOPED SnO2 NANOPARTICLES
SATHYASEELAN B. and JAYABALAN K.
Anna University, Chennai.

Tin oxide materials present numerous applications like gas sensors, basic components in optoelectronic
devices or nano and ultrafiltration membranes. Moreover, SnO2 polycrystalline materials prepared by sol-gel
technique have recently been used for shielding fluoride glasses against corrosion. In the present work, pure
and Co doped SnO2 Nanoparticles have been synthesized using Sol-Gel Technique. Tin chloride and Cobalt
chloride were used as metal sources. XRD analysis shows that all the samples consist of single phase with
rutile phase. The diffraction peak shifts towards the higher angles as Co is added which shows that it has
entered the SnO2 lattice and substituted Sn site. The crystallite size of the pure and Co doped samples lie
between 12 to 18 nm. Morphological characterizations were carried out using Scanning electron microscope.

N3-O4
SYNTHESIS OF SILVER NANOFLUIDS WITH POLY
(VINYLIDINE FLUORIDE)
Phule1 A.D., Susrutha1 B., Ram1* S., Tyagi2 A.K.
1
Material Science Centre, Indian Institute of Technology, Kharagpur-721 302, India
2
Solid State Chemistry Section, Applied Chemistry Division, BARC, Mumbai -40009, India.

Nanofluids consisting of nanoparticles (NPs) of noble metals dispersed in an organic or inorganic fluid
offer wide spread applications as computing systems, sensors, colored dyes, pharmaceutical tools, catalysts,
biomedical materials, electronic devices, and nonlinear optical devices [1,2]. Apart from the optical
applications as bandpass filters, there is a tremendous interest in achieving an optical absorber or emitter in
the uv-visible to infrared regions [3]. Here we report part of our broad investigation on synthesis of optical
silver nanofluids and composites with selective ferroelectric media. A simple Ag  o Ag0 chemical
reduction reaction and in-situ dispersion of the resulting Ag atoms in form of Ag-NPs in polymer molecules
of poly(vinylidiene fluoride) (PVDF) has been developed and explored to devise stable Ag-PVDF nanofluids.
An organic solvent such as dimethylformamide (DMF) was used to obtain the precursor solutions from PVDF
88 ISRS-2008

and AgNO3 as the starting reagents. The reaction was carried out by adding AgNO3 (dissolved in DMF) into
PVDF in DMF under the utrasonication and heating conditions at 50  60qC in air. The Ag-NPs content was
varied as 0.1, 0.5, 2.0, and 5.0 wt% in order to devise Ag-PVDF nanofluids of selective optical properties.
All these nanofluids (which appear in selective apparent colors depending upon the Ag-contents) are radiation
emitting in the uv-visible region. Strong photoluminescence bands appear at 392, 394, 403, and 405 nm when
irradiating the nanofluids at 220-300 nm from a xenon source. In general, the spectrum presents considerable
red-shift with increasing the Ag-content over the range. The results are analyzed in correlation to size and
shape of Ag-NPs which were studied with transition electron microscopic images.

N3-O5

SYNTHESIS AND CHARACTERISATION OF BORON NITRIDE


NANOTUBES BY CHEMICAL VAPOUR DEPOSITION (CVD) METHOD
Shrine Maria Nithya J. and Pandurangan* A.
Institute of catalysis and petroleum technology, A.C. Tech, Anna University, Chennai – 600 025,India

Boron nitride nanotubes (BNTs) found to be a novel material in high temperature applications,
bio-sensors, nano-electronic devices and drug delivery systems. BNTs could be used in the fabrication of
novel devices in which pure carbon nanotube do not perform very efficiency. Generally BNTs were
synthesized by Arc discharge, laser ablation and CVD method. Among these CVD method is best way to
synthesis of boron nitride nanotubes using boric acid (Boron source) and urea, ammonium chloride, ammonia
gas as the nitrogen source by using CVD method we achieved good purity of BNTs in the short period of
reaction time. The synthesized BNTs were characterized by XRD, FT-IR, TGA, scanning electron
microscopy (SEM), and transmission electron microscopy (TEM) techniques. The reaction parameters such
as temperature, molar ratio of the reactants and time were optimised for the better formation of BNTs. These
results open up a new kind of synthesis method with low expensive and important perspectives for use in
large quantity production.

N3-P1

HYDROTHERMAL SYNTHESIS AND STUDIES OF PURE AND Ni


DOPED ZnO NANORODS FOR PHOTOCATALYSIS APPLICATIONS
Mohan Kumar G., Ilanchezhiyan P., Jayavel R.
Centre for Nanoscience and Technology, Anna University, Chennai.

Pure and Ni doped ZnO Nanorods have been synthesized using Hydrothermal Technique. Zinc acetate
and Nickel acetate were used as metal sources. XRD analysis shows that all the samples consists of single
phase with hexagonal wurtzite structure. The diffraction peak shifts towards the higher angles as Ni is added
which shows that it has entered the ZnO lattice and replaces Zn ion. The crystallite size of the pure and Ni
doped samples lie between 12 to 18nm. Morphological characterizations were carried out using Scanning
electron microscope. The morphology of the samples appears to be in the form of rod like structures.
Photocatalysis reaction were carried out for the both pure and Ni doped samples, whose results were analyzed
using IR and UV (vis spectra). Ni doped samples were found to be more efficient while compared to the pure
ZnO nano crystallites.
ISRS-2008 89

N3-P2
SYNTHESIS AND CHARACTERIZATION OF Bi2S3 NANORODS BY
SURFACTANT-ASSISTED SOLVOTHERMAL METHOD
Mageshwari K., Sathyamoorthy* R., Sudhagar P., Saravanakumar R.
PG and Research Department of physics, Kongunadu Arts and Science College,
Coimbatore - 641 029. Bharathiar University

Bismuth sulfide Bi2S3 nanorods have been prepared by surfactant-assisted solvothermal method.
Bismuth acetate and thioacetamide were used as precursors. Triton 100-X was used as surfactant for
controlling the morphology of the product. The microstructure and optical properties of the Bi2S3 nanorods
were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive
and X-ray spectroscopy (EDX), optical absorption and PL spectrum. The XRD pattern reveals that the
Bi2S3 nanoparticles possess polycrystalline structure with orthorhombic phase. SEM images identified the
nanorods formation. The rod-like morphology obtained by short-time ultrasonic treatment for 10 minutes.
The optical and photoluminescence properties of Bi2S3 nanorods have been characterized. The UV absorption
spectrum reveals a clear band shift towards the blue region. The results are discussed on the basis of reaction
time, temperature and surfactant for the formation of nanorods.

N3-P3
SYNTHESIS AND CHARACTERIZATION OF SOL-GEL DERIVED
NANOCRYSTALLINE TIN OXIDE THIN FILM FOR GAS SENSOR
APPLICATIONS
Vasudevan R., Vijayalakshmi S., Sathayaseelan B., Alagesan T., Jayabalan K.
Anna University, Chennai

In the present investigation, nanocrystalline tin oxide SnO2 semi- conducting thin film was coated
on the glass substrate by sol-gel spin coating technique. The deposited sample was annealed at 200qC to
improve the crystallinity of the film. The XRD confirming the tetragonal structure and the particle size was
calculated approx. 25 nm also it is confirmed through the AFM topography technique. The SEM analysis
reveals that the SnO2 film was uniformly coated over the glass substrates and the particles were in the
nanometer range. The functional groups and the band gap of the material were calculated using the FT-IR
and UV-Visible spectroscopy respectively. Under these conditions, SnO2 would be a promising material for
the gas sensor also it has sharp increase in conductivity when exposed to a reducing gas.

N3-P4
PREPARATION OF ANATASE TiO2 NANO-PARTICLES
BY SOL-GEL METHOD
Karthik K., Kesava Pandian S., Victor Jaya N.
Anna University, Chennai.

Titanium dioxide TiO2 is widely used in various technological applications such as photocatalysis,
sensors, and photo electrochemical solar cells. The applications of TiO2 are strongly dependent on the
crystalline structure, morphology and size of particles. The high surface to volume ratio is inherent in a nano
particle which is useful for photocatalysis and hence most of the studies are focused on the nanosized
90 ISRS-2008

TiO 2 with the purpose of improving the light absorption. Nano TiO 2 powders have been prepared by sol–gel
technique using titanium (IV) isopropoxide as the precursor. The crystalline structures and anatase phase of
the nano TiO 2 powders have been characterized by using X-ray powder diffraction (XRD) and Laser Raman
Spectroscopy. The surface morphology of the prepared nano TiO 2 was carried out by using SEM. The average
particle size was found to be ~17nm. The anatase phase of the prepared TiO 2 was conformed by the three
(A1g, B1g, and Eg) Raman active modes.

N3-P5
EFFECT OF METAL CONCENTRATION AND TEMPERATURE
FOR THE SYNTHESIS OF
Atchudan R. and Pandurangan* A.
*
ICPT, A. C. Tech, Anna University, Chennai-25, India

Appropriate weight percentage of antimony (Sb) supported on mesoporous MCM-41 molecular sieves
were prepared by wet impregnated method. The above prepared mesoporous Sb/MCM-41 molecular sieves
were calcined at 500qC for 3 hrs. The calcined materials were characterized by various physicochemical
techniques such as X-ray diffraction (XRD), thermo gravimetric analysis (TGA), DRS-UV spectroscopy and
scanning electron microscopy (SEM). The calcined samples were used as catalytic template for the growth
of carbon nanotubes using acetylene as a carbon precursor by chemical vapor deposition technique at 700,
800 and 900qC. The reaction parameter such as effect of metal concentration and temperature were optimized
for better formation of carbon nanotubes. The deposited carbon materials were purified by acid treatment
and air oxidation. The purified materials were characterized by XRD, SEM, HRTEM and Raman
spectroscopy techniques. Carbon nanotubes morphology was observed from HRTEM. The good thermal
stability and high productivity observed in this study suggested that the metal loaded MCM-41 could be a
kind of promising supports for catalytically synthesizing CNTs.

N3-P6
ECONOMICALLY SYNTHSISED NANOSIZE SiC
BY ADAPTING SOL- GEL AND
Anthuvan Rajesh J. and Pandurangan* A.
ICPT, A. C. Tech, Anna University, Chennai-25, India

A two-step sol–gel processing was used to synthesize SiO2– carbon hybrid gels as SiC precursors,
with tetraethoxysilane (TEOS), and starch being the starting materials, oxalic acid (OA) and
hexamethylenetetramine (HMTA) are being the catalysts. At the first step TEOS was prehydrolyzed under
the catalysis of OA. At the second step HMTA was added to facilitate gelation. The influences of the molar
ratio of OA/TEOS and prehydrolysis time on the sol–gel reaction were investigated. There existed an optimum
OA/TEOS ratio where prehydrolysis time needed to form transparent gels was the shortest. The conversion
of the gels to silicon carbide powders via carbothermal reduction was complete when heated at 1300qC for
2 hrs. The homogeneous distribution of silica within carbon and their loose structure result in the formation
of nanosize silicon carbide powders. The as synthesized sample was heated in air at 700qC for removal of
the residual carbon and treated by nitric acid and then hydrofluoric acid for elimination of unreacted silica
and other impurities. The precursors and their carbothermal reduction products are investigated by XRD,
FT-IR, Raman spectroscopy, XPS, SEM with EDX, and HRTEM. The effect of heat treatment temperature
on the synthesis of SiC powder was also discussed.
ISRS-2008 91

>?C820;<0C4A80;B
OM-O1
EFFECT OF ANNEALING TEMPERATURE ON PROPERTIES OF ZINC
OXIDE THIN FILM GROWN BY THERMAL-CVD
Rafaie1,* H.A., Suhaidah 1 A., Mamat 2 M.H., Khusaimi1 Z., Sahdan2 M.Z., Abdullah1 S. and Rusop2 M.
1
Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
2
Faculty of Electrical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
Zinc oxide (ZnO) thin films were successfully grown on glass substrate by vapor phase Thermal-CVD
method. Vapor process by Thermal-CVD was employed at low deposition temperature in the range of
400qC  500qC. The samples were characterized using Scanning Electron Microscope (SEM), UV-VIS-NIR
Spectroscope and Photoluminescence Spectroscope (PL). SEM micrograph confirmed the growth of ZnO
structure while PL spectra showed that the PL intensities increase as the deposition temperature increases.
An estimated bandgap energy obtained from UV-VIS-NIR also reported.

OM-O2
DEVELOPMENT OF HIGH QUALITY LARGE SIZE UNIDIRECTIONAL
ADP SINGLE CRYSTAL FOR ELECTRO-OPTICAL DEVICES
Rajesh P. and Ramasamy P.
Centre for Crystal Growth, SSN College of Engineering, Kalavakkam- 603 110, India
<10 0> directed ammonium dihydrogen phosphate single crystal has been grown using the uniaxially
solution-crystallization method of Sankaranarayanan–Ramasamy (SR). The size of the grown crystal is 40
mm in diameter and 50 mm in thickness. The growth rate was approximately 1 mm/day. The grown crystals
were characterized by UV–Vis spectroscopy, Vicker’s hardness and dielectric studies. ADP crystal grown
from SR method has 10% higher transparency than the ADP crystal grown from conventional method.
Dielectric constant and dielectric loss increases with increase in temperature for all the frequencies. This may
be due to the contributions of all the four polarizations such as electronic, ionic, dipolar and space charges
are predominant in the lower frequency region. The hardness of ammonium dihydrogen phosphate single
crystal increases with increase of load. The cracks were formed in the conventional grown crystal at 100 g,
but no cracks were observed up to 100g in SR ADP. Comparing the <1 0 0> plane of the conventional method
grown ADP crystal with <1 0 0> directed SR method grown ADP crystal, the optical transparency, dielectric
constant and Vicker’s hardness number are increased and dielectric loss is decreased in SR method grown
crystal. The low dielectric loss, higher transparency and higher hardness indicates that the low concentration
of defects in the SR method grown single crystal. These are the requirements for the good electro-optical
material. The result shows that the SR method grown crystal has higher quality than the conventional method
grown crystal.
92 ISRS-2008

OM-O3
CHARACTERISATION OF CHEMICALLY SYNTHESISED
NANOCRYSTALLINE CADMIUM SULPHIDE FILMS
Kusumanjali Deshmukh, Mukherjee M. and Bhushan S.
Pt. Ravishankar Shukla University

The films formed by wide gap II-VI semiconductor are of considerable interest, as their emissions
cover the technologically attractive blue and green spectral region. In particular, thin CdS films deserve
attention, as these films are an appealing host for photonic devices. It has advantage of size-induced changes
in structural, optical and electronic properties, which deviate from the corresponding bulk phase properties.
In this paper growth of Nanocrystalline CdS semiconducting films on the glass substrate by means of chemical
bath deposition method (CBD), with Cd CH3COO 2 as Cd ion source, NH2 2CS as S ion sources and
Thioglycerol and Methanol together as capping agent(stabilizing agent) is reported. UV-VIS absorption
spectral studies and SEM images indicate that the volume of capping agents adjust the band gap of CdS to
obtain stable and homogenous films. XRD studies reflect the existence of hexagonal planes and confirm the
particle size reduction. Band gaps are found to increase and particle size is found to be in nano region from
optical absorption studies.

OM-O4
PRESSURE DEPENDENT IONIZATION ENERGIES
IN A SPHERICAL QUANTUM DOT
Sivakami1* A., Senthur Pandi 1 R., Chokkalingam1 R., Kanistha1 R.,
Mahendran1* M. and Navaneethakrishnan2 K.
1
Department of Physics, Thiagarajar College of Engineering, Madurai-625 015, India.
2
School of Physics, Madurai Kamaraj University, Madurai-625 021, India.

At present, there is a considerable interest in the physics and applications of Low-Dimensional


Semiconductor Systems (LDSS). The most widely investigated quantum dot system is the GaAs/
Ga1-xAlxAs. The quantum dot occurs in the GaAs region with GaAlAs providing the barrier. The optical
and transport properties of semiconductors are sensitive to impurities, external fields and stress therefore, it
is important to consider these aspects in heterostructures.
In the present work, a hydrogenic donor is introduced in the GaAs region and calculated the ionization
energy in a spherical quantum dot. The donor ionization energies in a GaAs spherical quantum dot under
hydrostatic pressure is calculated by using a variational approach (with the inclusion of polaronic effects)
within the effective mass approximation. The ionization energy is computed as a function of hydrostatic
pressure and the dot size with inclusion of the band non-parabolicity and polaronic effects. All the calculations
have been carried out for finite barrier with square well confinement. Our results reveal that, (i) the hydrostatic
pressure increases the ionization energy and also the variation is larger for smaller dots only, (ii) as the dot
size decreases the ionization energy increases for the finite potential well and (iii) the hydrostatic pressure
decreases the sub band energy with the different dot size. These results are in good agreement with S T
Perez-Merchancano et.al, (J. Phys. Condens. Matter 19 (2007) 026225) in which they have used the
variational approach without considering the polaronic effects. Finally, we concluded that the hydrostatic
pressure affects the ionization energies appreciably for narrow dots only. The ionization energies have been
investigated for singlet state and will be addressed in the conference.
ISRS-2008 93

OM-O5
INVESTIGATIONS ON MMTC SINGLE CRYSTAL
FOR LASER APPLICATIONS
Rajesh Kumar T., Jeyasekeran R., Gunaseelan R., Prabha K. and Sagayaraj P.
LOYOLA COLLEGE, Madras Univeristy, Chennai, India
Recently, second-order (NLO) materials capable of efficient frequency conversion of visible and
ultraviolet wavelengths, especially materials which can generate blue-violet light for applications including
telecommunications, optical computing, optical information processing and optical disk data storage are
widely studied. Manganese mercury thiocyanate (MMTC) crystal is an excellent second-order nonlinear
optical material; it is normally grown by slow evaporation method. Deviated from the earlier article, the
present work deals with the growth of MMTC by temperature lowering method for the first time. Single
crystals of nonlinear optical MMTC were grown by temperature lowering method. The UV cut-off
wavelength of MMTC was found to be at 373 nm. The blue and violet emission from the crystal was evident
from the PL spectrum. The ac and dc conductivity studies are reported. Surface morphology study was done
on the selected face on the grown crystal. Dendrite growth pattern was observed on the surface of the crystal
from SEM.

OM-P1
STRUCTURAL AND OPTICAL PROPERTIES OF CdO
NANOCRYSTALLINE THIN FILMS FOR OPTOELECTRONIC
APPLICATIONS
Tamil selvan S., Saravanan L., Arivuoli D., Jayavel R.
Anna University,Chennai.
From the group of II-VI semiconductors Cadmium Oxide is one of the promising transparent
conducting Oxides which have great potential for optoelectronic devices. Compare to other transparent
conducting oxides cadmium oxide is uniquely positioned for application in photometry due to its absorption
of light in the blue region of the electromagnetic spectrum. It has been used as heat mirrors in the solar cells
because of high reflectance in the infrared region, together with high transparency in the visible region.
Formation of cadmium hydroxide at room temperature onto glass substrate from an aqueous alkaline
cadmium nitrate solution using a simple chemical bath deposition and its conversion to cadmium oxide (CdO)
by thermal annealing treatment has been studied in this paper. The structural, surface morphological and
optical studies were performed for as deposited and the annealed films. The structural analyses revealed that
as-deposited films consists of mixture of Cd OH 2 and CdO, while annealed films exhibited crystalline CdO.
From surface morphological studies, conversion of clusters to grains after annealing was observed. After
annealing treatment the band gap energy values were changed from the as-deposited films. The results were
discussed in detail.
94 ISRS-2008

OM-P2
MICROSTRUCTURAL, MECHANICAL AND OPTICAL PROPERTIES
OF CrN THIN FILMS PREPARED BY PULSED
DC MAGNETRON SPUTTERING
Elangovan1 T., Kuppusami* P., Thirumurugesan R., Ramaseshan2 R., Bera3 S., Mohandas E. and Mangala raj1 D.
1
Physical Metallurgy Division, 2Material Science Division, 3Water and Steam Chemistry Division, BARCF, Indira
Gandhi Center for Atomic Research, Kalpakkam-603 102, India.
1
Thin Film Laboratory, Department of Physics, Bharathiar University, Coimbatore-641046, India. Physical
Metallurgy Division, 2Material Science Division, 3Water and Steam Chemistry Division, BARCF, Indira Gandhi
Center for Atomic Research, Kalpakkam-603 102, India. 1Thin Film Laboratory, Department of Physics, Bharathiar
University, Coimbatore - 641046, India.

CrN has received considerable interest over the past several years due to its high hardness and corrosion
resistance, and for applications as hard, wear, and corrosion-resistant coatings. Chromium nitride (CrN) thin
films were deposited on (100) silicon and D-9 alloy steel substrates using an asymmetric-bipolar pulsed DC
magnetron sputtering system. The CrN coatings were deposited at different nitrogen flow rates, substrate
temperatures, pulse width and frequency. The analyses revealed that the nitrogen partial pressure during film
deposition had a strong influence on the resulting deposition rate and crystallinity. At low N2 low rates, ( <
2sccm), pure Cr was detected, while at the intermediate flow rates ( < 5 sccm), the hexagonal and cubic
phases were obtained [Cr2N and Cr N]. Finally, in the r ange of 10-25 sccm, only the cubic Cr N phase was
obtained. Substr ate temper ature, pulse frequency, and pulse width seem to influence the film or ientation.
Also, the films sputtered in pure argon atmosphere contained larger cr ystallites than those sputtered in
nitrogen atmosphere. The Cr 2p3/2 and N 1s XPS spectr a confir med the for mation of Cr N phase. The
refr active index, dielectr ic constant, and absorption coefficient of the Cr N coating in the wavelengthr ange
of 300–1200 nm were deter mined. The Cr N coatings deposited under the optimized process conditions
exhibited an aver age nanoindentation har dness of 15 GPa and an elastic modulus of 283 GPa.

OM-P3
EFFECT OF 50 MEV Si4+ ION IRRADIATION ON CdS THIN FILMS
Chithambararaj A., Chandramohan S., Sathyamoorthy* R., Kanjilal D.
PG & Research Department of Physics, Kongunadu, Art & Science College, Coimbatore

In Recent years, the advantage of Swift heavy Ion irradiation finds attention towards the modification
of material properties from its bulk nature. In this paper, we have reported the Swift heavy ion (SHI) irradiation
on Cadmium sulphide (CdS) thin films deposited on silicon substrate by using 50 MeV Si4  ions of various
doses from 5 u 1012 to 5 u 1013 ions/cm2. The structure, morphology and luminescence properties of pristine
and irradiated films were carried out by using x-ray diffraction (XRD), Raman spectra, AFM and
Photoluminescence, respectively. X-ray diffraction studies reveals that the pristine and irradiated CdS thin
films have cubic or hexagonal phase with preferential orientation along (111) C or (002) H. The improvement
in crystallization and degradation of the film has been studied depends on irradiation energy and the result
is in good agreement with Raman studies. The AFM study implied significant changes in the roughness in
the film due to irradiation. From PL, for lower irradiation energy 5 u 1012ions/cm2 , the defect annihilation
and radiative transition has been observed and at higher irradiation energy 5 u 1013ions/cm2 further defect
creation and non- radiative recombination is noted, it may be due to lattice disorder in the film structure.
ISRS-2008 95

OM-P4
STRUCTURAL AND OPTICAL STUDIES ON WO3
THIN FILMS BY SPRAY PYROLYSIS
Kovendhan1 M., Gokulraj2 S., Ramesh Kumar1 G., Mathivanan1 V., Suriya kumar1K., Sivakumar1 B.,
Paul Joseph3 D., Venkateswaran3 C. and Mohan1 R.
1
Department of Physics, Presidency College, Chennai - 600 005,
2
Department of Physics, National Institute of Technology, Tiruchirapalli - 620 015,
3
Department of Nuclear Physics, University of Madras, Chennai - 600 025.

Tungsten oxide WO3 thin films were deposited onto amorphous glass substrates at different substrate
temperatures ranging from 250qC to 500qC in a spray pyrolysis unit. The precursor solution is prepared by
dissolving appropriate quantity of WO3 powder in a mixture of hot ammonia solution and distilled water. The
XRD analysis indicated crystallinity for the films deposited at substrate temperatures above 350qC. The peak
values 23.10q and 24.06 q correspond to the monoclinc (002) and (020) planes of WO3. SEM analysis reveal
variations in surface morphology for films deposited at different substrate temperatures. The UV-Vis analyses
were performed to study the transparency of the deposited WO3 films as a function of substrate temperature. Laser
Raman measurements for the deposited films were also carried out at 300 K. The results are discussed.

OM-P5
STRUCTURAL AND OPTICAL CHARACTERIZATIONS
OF MN AND IN DOPED ZnS NANOCRYSTALS
Brightson M., Selvarajan P., Freeda T.H., John Kennady S., Meenakshi Sundar S.
Sri Paramakalyani College

Undoped and Mn, In doped ZnS nanocrystals have been synthesized using solvothermal technique.
Microwave oven was used as a method for this technique. Sizes of the particles were determined using the
Debye-Scherrer’s formula from the XRD patterns. Lattice parameter values were calculated using XRDA
software and verified with JCPDS files. Band gap energy values were calculated for the four ratios of Mn
doped ZnS nanocrystals. SEM and EDAX spectra were taken for the Mn doped ZnS
nanocrystals.Co-ordination compounds were identified using the FT-IR spectra for the undoped and doped
crystals. The results will be discussed in detail in the conference.

OM-P6
PREPARATION AND CHARACTERIZATION OF CADMIUM
SULPHIDE NANOCRYSTALS
Nirmala Jothi N.S., Dennis Christy P., Ramalingam G., Muthuvinayagam A.
Loyola college, Madras University.

CdS is one of the important II-VI semiconductor due to its wider band gap (2.42 eV) and non-linear
optical properties. CdS nanomaterials have vital applications in flouresence probe, sensors, solar cells,
photoelectrocatalysis and light emitting diodes etc. Controlling the particle size not only alters the forbidden
gap of the semiconductor, but also its electronic properties. In this investigation, we have reported a new
process using thiourea and cadmium nitrate at partially low temperature which approach nanoparticles having
approximate diameter of 40 nm. The synthesized nanoparticles have been characterized using techniques
such as X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-Vis absorption
spectroscopy. The experimental results have indicated CdS nanocrystals in single phase with hexagonal
structure. From the TEM images, size of the nanocrystals was measured as 40 nm.
96 ISRS-2008

BDA50244=68=44A8=6
SE-O1
PARAMETRIC STUDIES OF LASER SURFACE ALLOYING
PROCESSES OF WALLEX 50 AND COLMONOY 88 DEPOSITS
Shivamurthy R.C., Kamaraj M., Nagarajan R., Shariff S.M. and Padmanabham G.
Indian Institute of Technology Madras, Chennai-600036.
Laser surface alloying (LSA) is a new and promising hardfacing technique for generating surface alloys
having a wide range of favourable properties such as hardness, wear and corrosion resistance. The alloying
can be done in a single-stage or two-stage process. In single-stage process, alloying material is transported
directly to the zone of interaction between the laser beam and the substrate. The two-stage process includes
pre-depositing a layer of desired alloying material on the substrate, followed by laser heat treatment.
The present work describes an investigation of the effect of 3 different parameters of laser surface
alloying—i.e., laser power, laser scanning speed and powder feed rate on deposited height, depth and width.
L8 orthogonal array has been designed to study these 3 parameters at 2 levels each. Commercial Co-based
Wallex-50 and Colmonoy 88 alloy powders have been deposited on AISI 415 martensitic steel by single-step
process of laser surface alloying using 6 kW CW Diode Laser system.
The results of single clad pass with extent of dilution, surface hardness and microstructures produced
by different conditions are presented and discussed. Finally, an attempt has also been made to list out the
parameters at which enhanced hardness, minimum dilution and desired clad height and clad depth can be
obtained.

SE-O2
HIGH TEMPERATURE EROSION RESISTANCE OF STAINLESS STEELS
Bhanu Kiran V.T., Vishal S., Vinayak Tiware S., Ashok T.V., Sriharsha R.V., Kumar R.K.
R. V. College of Engineering, Bangalore / VTU, Belgaum
In this study, the erosion resistance of different grades of stainless steels (SS) such as SS304, SS309L,
15/5 precipitation hardened stainless steel and tungsten carbide (WC) hardfaced stainless steel has been
characterized, under accelerated laboratory conditions. A systematic study on the erosion resistance
characteristics of different grades of stainless steels, using jet erosion type laboratory test rig has been carried
out. The process variables include particle velocity, erodent type, impact angle, exposure time and
temperature. The erosion measurements were carried out at room temperature and at elevated temperatures
300qC, 380qC to ascertain the sensitivity of different grades of SS. The erosion resistance tests were
conducted at different erodent particle impact angles viz. 15, 30, 45, 60, 90q and at different erodent particle
velocities. The data generated is useful for selection of specific grade of stainless steel material, for
applications where high temperature erosion is involved.
ISRS-2008 97

SE-O3

HIGH TEMPERATURE ADHESION EVALUATION OF WC-Co


COATING ON AlSi 440C BY DETONATION SPRAY COATINGS
Edward Kennedy Z., Natarajan S., Aniruddha Chatterjee
National Institute of Technology, Trichy

WC-based coatings are widely used in the Aircraft industry mainly for their resistance to wear,
reworking and rebuilding operations and repair of worn components on landing gear, hydraulic cylinders,
actuators, propeller hub assemblies, gas turbine engines, and so on. Also in automotive parts, to improve the
wear resistance of the cylinder liner of the engines operating in desert area, the tungsten carbide coatings are
used.

In the present work, WC-Co coatings were built up on an AISI 440C stainless steel substrate using
detonation spray. High temperature friction and sliding wear resistance were studied using pin-on-disc
tribo-tester. The various parameters involved like, sliding velocity, sliding distance, Load and temperature
were analyzed. The evaluation of wear was made using mass loss techniques. It was found that the composite
coating showed a better performance even at high temperature when compared with room temperature. Also,
the coefficient of friction increases steadily with time which was confirmed by Lab-view images. The coatings
were characterized using scanning electron microscopy (SEM and X-ray diffraction (XRD). The XRD images
revealed no reflection from substrate element even after several thousand meters ensuring a good adhesion
of coating thickness.

SE-O4

BN-FILLED PRECERAMIC POLYMERS AS BARRIER


COATINGS ON STEEL
Flores O.J.U., Günthner M., Krenkel W., Motz G.
Universität Bayreuth

Preceramic polymers are an excellent alternative to the manufacture of protective ceramic coatings on
steel against oxidation and corrosion attack. In this context, two different particle-filled polysilazane systems
were developed, using BN powder as a passive filler. The ceramic coatings were manufactured on steel
substrates by dip-coating, followed by pyrolysis in air up to 800qC. After the thermal treatment they were
characterized regarding layer thickness, adhesion, oxidation and corrosion resistance. The passive filler
reduces the shrinkage of the layer, which results from ceramization of the precursor content. The SEM
micrographs showed that the combination passive filler/polysilazane leads to a dense and well adhered
coating which is resistant against oxidative environments at high temperatures and free of cracks for thickness
layers up to 15%m. The coated substrates also presented a high resistance against corrosion, once they were
left in a 1N HCl solution for more than 24 hours without suffering delamination.
98 ISRS-2008

SE-O5
STRUCTURAL ASPECTS OF SPUTTER-DEPOSITED
304 STEEL-10 WT% Al COATINGS
Seelam U.M.R. and Suryanarayana C.1Ohkubo T. and Hono K. 2Cheruvu N.S. and Wei R.
Department of Mechanical, Materials and Aerospace Engg., University of Central Florida, Orlando, FL-32816, USA.
1
Nanostructure Analysis Group, National Institute for Materials Science,
1-2-1 Sengen, Tsukuba, Ibaraki-305-0047, Japan.
2
Southwest Research Institute, San Antonio, TX-78228, USA.

It is well known that Al addition to steel improves high temperature oxidation and corrosion resistance.
Microstructural understanding of such steels is important before applying them for high temperature
applications. This investigation deals with the microstructural characterization of magnetron-sputtered
austenitic stainless steel (304SS) coating containing 10 wt% Al. The 304SS+10 wt% Al coating was deposited
on 304SS substrate using plasma enhanced magnetron sputtering (PEMS) technique. The sputter-deposited
32 Pm thick coating was characterized by XRD, TEM (SAD, STEM, EDS and HREM), 3-Dimensional Atom
Probe (3DAP) and SEM techniques. While both XRD and TEM helped in phase identification, TEM and
3DAP studies further helped in revealing the microstructural features of the phases. The coating had columnar
grains with size ranging from 0.8-3 Pm. The coating contained the á-Fe solid solution as matrix and 2-10 nm
ordered FeAl B2 precipitates. The coating also had layered structure with a periodicity of 2-3 nm. The
alternate layers were either enriched or depleted in Al and Ni. In the layer enriched with Al and Ni, Fe and
Cr were depleted and vice versa in the next layer. Detailed results of this investigation will be presented.

SE-P1
STUDY ON THE INFLUENCE OF SURFACTANTS ON COATING
EFFICIENCY, CRYSTALLINITY, WEAR AND CORROSION
BEHAVIOUR OF ELECTROLESS COATING
Elansezhian R., Kesavan Nair P. and Ramamoorthy B.
Indian Institute of Technology Madras

Electroless nickel - phosphorus (EN) coating is a well established surface engineering process that involves
deposition of a metal-metalloid alloy coating on a variety of materials. EN coating has received widespread acceptance
and finds many applications in micro- and nanotechnologies. A major drawback of EN coating is its high cost of
production due to factors such as high cost of chemicals used, wastage in the form of metal bearing sludge, poor
nickel recovery from the bath etc. Due to these reasons, the EN coating efficiency is reported to be poor. Efforts based
on additives which influence the chemical process directly have been made by several researchers. One possible
alternate approach for improving efficiency of EN coating process might be the addition of some suitable surfactants
to the electrolyte bath. The effects of surfactants sodium dodecyl sulfate (SDS) and cetyltrimethyl ammonium
bromide (CTAB), on the coating efficiency, crystallinity, wear and corrosion behaviour EN deposits are investigated
in this study. The variation on surface morphology was examined using high resolution scanning electron microscope
(HRSEM). The EN coated samples were characterized using X-ray diffraction analysis (XRD). Wear studies were
performed on a pin-on-disc wear testing instrument. Accelerated corrosion studies were carried out on a neutral salt
spray chamber. It was observed that coating efficiency, crystalline behaviour, specific wear rate, corrosion rate, and
surface morphology of electroless Ni-P coating were clearly influenced by the addition of surfactants SDS and
CTAB. The complete experimental details, results obtained and their analysis are presented in this paper.
ISRS-2008 99

SE-P2
INVESTIGATION ON SPRAY PROCESSING OF Al-Si
ALLOYS AND THEIR WEAR CHARACTERISTICS
Raju K., Harsha A.P., Ojha S.N.
Institute of Technology/Banaras Hindu University

Spray forming is an attractive novel technique for the production of near net shaped components of a
variety of alloys. In the present investigation Al-12%Si, Al-15%Si and Al-20%Si alloys have been spray
formed at a temperature of 850qC and a pressure of 1MPa. The microstructural and wear characteristics of
these alloys have been evaluated and compared with that of chill cast alloys. The microstructure of spray
formed alloys exhibited ultra fine Si particles with globular shape in the matrix having equiaxed grain
morphology in contrast to the needle like and plate like Si particles in the matrix in chill cast alloys. The wear
rate of spray formed alloys was invariably observed to be lower than that of chill cast alloys over a wide range
of load conditions. The reason for microstructural modification and resultant improvement in wear
characteristics are discussed.

SE-P3
EFFECT OF HARDFACING TECHNIQUES ON WEAR PROPERTIES OF
STELITE-6 AND SS410 COATING ON MILD STEEL SUBSTRATE
Suresh K.V., Kulkarni R.S., Krishna M., Narasimha Murthy H.N.
R V College of Engineering.

The research work is focused on the effect of hard facing techniques such as plasma transferred arc
method, spray fuse method and gas tungsten arc welding method on wear properties of Stelite-6 coated mild
steel and SS410 coated mild steel. The hard faced specimens (2 mm coating thickness) are subjected to
hardness and dry sliding wear tests using Rockwell hardness tester and pin-on-disc wear testing machine
respectively. The dry sliding wear tests are conducted for three sliding distances such as 0.5, 1.0 and 1.5 km
at speed of 500 and load of 10N. The microstructure and chemical composition of the coatings were analyzed
by optical microscopy and XRD respectively. The results demonstrate that the both coating materials increase
hardness and wear resistance of the specimens in all sliding distances. Coatings with stelite-6 with plasma
transferred arc method shows better wear resistance result compared with other two methods.

SE-P4
TRIBO-PERFORMANCE EVALUATION OF FUNCTIONALLY
GRADED CERAMIC COATING BY D-GUN
Raja Kumar S., Vijayaraghavan L., Mayuram M.M.
Indian Institute of Technology Madras, Chennai.

Surface engineering encompass with texture and chemistry alterations on the surface, as today’s
engineering components demand more than one superior value of desirable properties. To meet such
conflicting demands Functionally Graded Coating (FGC) [1] are used. Layer structured FGC’s of Alumina
and Alumina-Titania (AT-13) of different layer thickness are developed by Detonation-gun (D-gun) coating
and subjected to sliding indentation/scratch test [2] to study their response to tribo-logical demands. During
the sliding indentation test, the energy liberation and vibration signal are monitored on-line using Acoustic
100 ISRS-2008

Emission (AE). The friction force was measured using a strain gauge transducer holding the indenter and the
experiment was conducted for different loads and passes. During sliding, the indenter plows on the ceramic
composites and also experience adhesive friction to form a distressed zone around the indenter. Based on the
applied normal load, either relatively smoother groove can occur or a groove associated with formation of
surface fissure and subsequent cracking of the adherent material can result. The typical variation of the
average tangential force with respect to applied normal loads varies non-proportionally for different FGC’s.
Normally co-efficient of friction should be independent of normal load under traditional tribo-logical
environment. However, with ceramic coatings, due to possible defects in the lay-up such as porosity,
un-melted particles and also varying interlayer/cohesive strength, hardness gradient, the co-efficient of
friction exhibits a non-linear relationship. The fluctuation of co-efficient of friction beyond a certain normal
load can be attributed to the damage of the material with high loading, i.e., this load may be critical sliding
load, associated with change from plowing friction to scratch friction. The paper presents relevant illustration
in the same.

SE-P5
EFFECT OF TEMPERATURE ON RUN-IN PERIOD
OF Ni BASED HARDFACING ALLOY DEPOSITED
BY PLASMA TRANSFERRED ARC WELDING
Kesavan D. and Kamaraj M.
Indian Institute of Technology Madras,Chennai
The investigation attempts to understand the effect of temperature on run-in period in friction plot of
Ni based (Colmonoy 5) hardfacing alloy deposited by plasma transferred arc welding (PTAW).
Characterization of the deposits was carried out using with optical microscopy, SEM-EDAX, TEM, XRD
and Vicker’s microhardness tester. Dry sliding wear tests of deposits were carried out at room temperature
(RT), 3000C and 550qC in air atmosphere for a fixed sliding velocity of 0.25m/s and at a constant load of
60N using high temperature pin-on-disc machine.Microstructure of the deposit consists of dendrites of J –
nickel solid solution phase and eutectic interdendritic consistutents. TEM micrograph reveals the fine globular
and needle like precipitates less than 100nm in sizes. The X ray diffraction pattern of deposits showed that
the various phases and precipitates of J – Ni, Chromium carbide Cr7C3 , Chromium boride Cr5B3 , Nickel
carbide Ni3C , Nickel boride Ni3B , and Nickel silicide Ni3Si . The hardness of the deposits is around 420
VHN whereas substrate is about 170 VHN.The co-efficient of friction (COF) at RT was found to be between
0.3 - 0.4, whereas at 300qC and 550qC it was hovering between 0.25 – 0.35 and 0.2 – 0.3, respectively. It has
been observed that steady state in COF values after run-in period for all the tests. High COF was observed
upto a run-in period of 200m at room temperature tests, whereas at 300qC it was observed up to 150m and
at 550qC, run-in period was almost negligible. Change in a COF value and run-in period are associated with
establishment of compacted layer of oxides and partially oxidized debris on the sliding surfaces. Mechanisms
involved at RT tests are pure abrasion, delamination and ploughing whereas at high temperatures mild
abrasion, adhesion and oxidation were responsible.
ISRS-2008 101

SE-P6
STUDIES ON FRICTION SURFACING OF AUSTENITIC
STAINLESS STEEL ON MILD STEEL
Khalid Rafi H., Janakiram G.D., Phanikumar G., Prasad Rao K.
Dept. of Metallurgical and Materials Engg. IIT Madras, Chennai-36
Single-bead coatings of AISI 310 stainless steel were deposited on mild steel substrates using friction
surfacing. Friction surfacing process parameters were optimized based on statistically deigned experiments.
The coatings were found to be metallurgically bonded to the substrate with good interfacial characteristics.
A well defined heat affected zone existed underneath the coatings, whose microstructure and hardness were
found to vary significantly with process parameters. Fully martensitic and hard HAZs typically resulted under
conditions of high heat input. It has been shown that, with careful choice of parameters, good coatings with
smaller/softer HAZs can be produced. The coatings showed fine equiaxed grains, indicative of dynamic
recrystallization. Preliminary microstructural studies showed no undesirable phases in coatings. EDAX
linescan studies confirmed that there was practically no dilution, demonstrating the superiority of friction
surfacing over conventional fusion welding based surfacing processes.

SE-P7
SYNTHESIS AND CHARACTERIZATION OF TERNARY
ELECTROLESS Ni-W-P COATINGS USING A BATH CONTAINING
MIXED COMPLEXING AGENTS
Logavenkatesh S., Seshadri S.K., Prathap Haridoss
Dept. of Metallurgical and Materials Engg. IIT Madras, Chennai-36
Electroless plating is a technique in which the redox reactions among chemicals are used to deposit
metal on an object without passing external electrical energy. Generally complexing agents are used in the
bath to control the free nickel ion concentration and to maintain pH level during electroless process. In this
investigation a bath to produce ternary electroless Ni-W-P using two complexing agents namely sodium
tricitrate and glycine was formulated, and plating rates estimated by using weight gain method. The bath
containing 10 g/l and 15 g/l of sodium tricitrate and glycine respectively shows the maximum plating rate.
Coatings with different composition were produced by altering the amount of sodium tungstate in the bath.
The chemical composition was determined by EDAX analysis. The structural analysis was conducted using
X-ray diffraction and TEM for as plated and heat-treated coatings, which shows the coatings to be nano
crystalline even after heat treatment. Surface morphology of the coatings was studied using SEM and shows
nodular structure. Mild steel was chosen as substrate for coatings and hardness was determined using Vickers
micro hardness testing, for both as plated and heat treated samples.
Key words: electroless nickel; mixed complexing agent; ternary alloys.
102 ISRS-2008

BH=C74B8B0=3?A>24BB8=6
SP-O1
SURFACE TREATMENT OF POLYESTER WITH GLOW
DISCHARGE PLASMA IN AIR AT LOW PRESSURE
Inbakumar S. and Anu kaliani* A.
PG and Research department of Physics,Kongunadu arts & Science College, Coimbatore-641029, Tamilnadu, India.

In order to increase the hydrophilicities and to improve dyeability, polyester fabrics were treated in
low pressure - glow discharge plasma. Different plasma parameters like pressure, exposure time and voltage
were variables in the process. Morphological changes as a result of plasma treatment were observed using
scanning electron microscopy (SEM). When treated, these fibres showed a new lamellar crystallization, as
shown by a new melting peak using differential scanning calorimetry (DSC). X-ray photoelectron
spectroscopy (XPS) has been used to study the chemical effect of low pressure glow discharge plasma
treatments of a PET surface. The capillary method was applied to evaluate the improvement in water uptake
of polyester fabrics.

SP-O2
GROWTH AND SINGLE CRYSTAL STRUCTURE
SOLUTION OF Fe1.97Bi0.03O3
Sathiyakumar S., Anbarasu V., Manigandan A.
Anna University, Chennai.

The title compound crystallizes in Rhombohedral system with unit cell values a = 5.0244(3) Å, c =
13.7233(8) Å and space group R3c. The percentage occupancy of Bi in Fe site was obtained by site occupancy
parameters as a variable in the least square refinement of the structure. There is a merohedral twinning of the
system about the c axis. The structure is essentially coincident with that of Fe2O3.

SP-O3
SYNTHESIS OF ZnO MICROSTRUCTURES FROM METALLIC Zn
Shubra Singh and Ramachandra Rao M.S.
Indian Institute of Technology Madras, Chennai

ZnO is one of the most important functional oxides with direct wide band gap (3.37 eV) and large
exciton binding energy (60 meV), exhibiting many interesting properties including near-UV emission,
transparent conductivity, and piezoelectricity. In recent years, a variety of ZnO nano-/ micromaterials have
been synthesized, such as nanowires, nanobelts, nanospring, nanoneedles, walls, tubes, nanobidges,
nanonails, sea urchin-like ZnO structures, etc.[1-4]. These complex ZnO structures have a particular
significance in the realization of advanced electronic and optoelectronic devices. In the present work different
morphologies of ZnO have been realized by vapour synthesis technique, using metallic Zn flakes. The growth
takes place at 800qC without employing any metal catalysts that are conventionally used in vapour deposition
technique. The as prepared sample consisted of fork and broom like structures. It exhibits visible green
emission (around 510 nm) on UV excitation. EDX data point towards oxygen deficiency in the sample.
Photoluminescence spectra confirm the presence of defects and a poor crystal quality of the as prepared
ISRS-2008 103

sample. The sharp tips and high surface area of these unique structures make them a potential candidate for
field emission, ultra-sensitive gas sensing, catalysts and filtering. A simple growth mechanism has been
proposed to explain the formation of such structures.

SP-O4
A STUDY ON THE HEAT CAPACITY BEHAVIOUR OF INDIGENOUSLY
DEVELOPED REDUCED ACTIVATION FERRITIC MARTENSITIC
(RAFM) STEEL BY DSC
Jeyaganesh* B., Arun Kumar Rai, Mythili R., Raju S., Saroja S., Mohandas E.,
Vijayalakshmi M. and Bhanu Sankara Rao K.
Indira Gandhi Centre for Atomic Research, Kalpakkam.
Reduced activation ferritic – martensitic steels (RAFM) are rather recent additions to the
well-established family of high chromium, low carbon, low swelling ferritic alloys. Currently these steels
are under active consideration as candidate material for the plasma facing first wall and tritium breeder blanket
components in emerging fusion reactor design (ITER and DEMO). In applications related to nuclear fusion,
the structural candidate must posses a higher degree of swell resistance against neutrons of higher energy
than encountered in a fast reactor, besides good high temperature creep strength at temperatures upwards of
600qC. Above all, they must pose a highly reduced radioactive hazard at the waste disposal end as otherwise
the high induced radioactivity would demand deep underground burial for prolonged periods of time. It is
by the way of mitigating this important problem, truly reduced activation ferritic martensitic steels have come
into existence. These steels are basically designed after modified 9Cr variety with the important caveat that
the concentration of Nb, Mo, Cu, Ti, Al, Sb, P, S etc are reduced to below ppb levels. Thus Mo is replaced
by W + V and Nb is replaced by Ta and by controlling the impurity content by making use of very pure
starting material, it is possible to design a RA FM . One such composition, namely
9Cr-1W-0.226V-0.003Mo-0.063Ta-0.0039Nb-0.026N-0.005Cu-0.05Si-0.0036Al (all in wt.%) has been
melted in MIDHANI and this has been taken up for detailed physical, metallurgical and mechanical
characterization in IGCAR. As a part of this study, we have measured the temperature variation of heat
capacity Cp using a high temperature heat flux differential scanning calorimetry. The measurements have
been made on various samples with different base microstructure, like the as received, quenched / normalized
(980, 1180, 1280qC / 0.5 to 2h) and tempered (780qC – 2 and 5 hour) conditions. The heat flux signal from
the calorimeter has been calibrated using pure iron (Fe-80ppm C, Aldrich Chemicals) in the temperature
range 200 1200qC. Highly reproducible and consistent results have been obtained for heat capacity of RAFM.
These data were compared critically with our own earlier measurements on other 9Cr-Mo based steels
including Eurofer –97 and also with literature information. As a result, a critically assessed lower and upper
bound Cp estimates are arrived for generic 9Cr-steel, including RAFM. As a by product of this study, accurate
values for the various phase transformation arrest points have also been determined for RAFM.
104 ISRS-2008

SP-O5
ROLE OF 12-PHOSPHOTUNGSTIC ACID SUPPORTED
MESOPOROUS MATERIALS INVOLVING ORGANIC
TRANSFORMATION REACTIONS – A LEACHING STUDY
Karthikeyan G., Pandurangan* A.
ICPT, A.C. Tech, Anna University, Chennai-25, India
The drive towards healthy solid acid catalysts associated with recyclability lead to the preparation of
HPWA/MCM-41 mesoporous molecular sieves of appropriate ratios by loading phosphotungstic acid on
siliceous MCM-41 by wet impregnation method. The prepared HPWA/MCM-41 materials were
characterized by X-ray Diffraction analysis (XRD), BET surface area method, FT-IR measurements and 31P
NMR. The morphology of mesoporous materials was studied by TEM technique. The catalytic activity of
the above materials was tested over single step organic transformation reactions and the diminishing load of
HPWA for every cycle was measured by ICP-AES technique in terms of tungsten percentage. The effect of
large pore pass-through for bulk molecules with high range acidity and the dissolution of synthetically
prepared HPWA/MCM-41 in various solvents with regard to tungsten content and complete achievement of
the loading were observed. The effects of process parameters such as concentration of loading, temperature,
nature of solvents, time on the dissolution rate of HPWA from the support and negligible leaching point
deciding the reusability were investigated.
Key words: Tungsten, Heteropoly acid, Leaching, Organic transformation reactions

SP-P1
AUTOMATION OF HOME MADE SPRAY PYROLYSIS UNIT
AND DEPOSITION OF CuFe2O4 THIN FILMS
Paul Joseph D. and Venkateswaran C.
University of Madras, Chennai.
The home made spray pyrolysis unit has been automated for horizontal rastering of the spray gun and
for controlled spray with constant interval in order to achieve homogenous coating over a large area. The
various components used in the automation of the unit are discussed with the help of a block diagram. In
order to check the performance of the automated unit, CuFe2O4 thin films were deposited onto a quartz
substrate at 500qC with constant rastering of the spray gun. The structural, microstructural, optical and
magnetic properties of the post annealed (800qC/1h in air) CuFe2O4 thin film are presented and discussed.
ISRS-2008 105

SP-P2

GROWTH AND CHARACTERIZATION OF PURE


AND 1,10 PHENANTHRLAINE DOPED POTASSIUM
PENTA BORATE (KB5) SINGLE CRYSTALS
Prabhaa K., Rajeshkumara T., Dennish Christya P., Ramesh babub M., Nirmala Jothia N.S.,
Chenc H. and Sagayaraja* P.
Loyola College, Madras Univeristy, Chennai, India

Borate crystals are often employed for high-power UV generation because of their relatively high
tolerance to laser-induced damage, large optical nonlinear coefficients, and greater transparency in the UV
region. KB5 appears to be superior to ammonium penta borate NH4B5O8.4H2O in most essential properties
relevant for use in nonlinear optical devices. For example at 222.2 nm KB5 generated more than ten times as
much radiation as the NH4B5O8.4H2O sample. We concentrate the low temperature slow solvent evaporation
method and characterization of 1,10 phenanthraline doped KB5 and describe its potential as a non-linear
optical material. The grown crystal has been subjected to single crystal X-ray diffraction analysis to identify
the unit cell parameters and crystal systems. The presence of carbon, hydrogen and oxygen content were
confirmed by CHN analysis. The Kurtz’s-Perry powder SHG efficiency was found to be for Pure and 1,10
phenanthraline doped KB5 crystals 1.6 and 2.2 times than that of pure KDP. Functional groups of the
compounds were confirmed by FT-IR studies. Surface morphology of the pure and doped KB5 crystals has
been found to be Scanning Electron Microscopic technique (SEM).

SP-P3

HIGH SPEED MACHINING (TURNING) OF SUPERALLOY INCONEL 718


Thakur D.G., Ramamoorthy B., Vijayaraghavan L.
Mechanical Engineering Department, Indian Institute of Technology Madras, Chennai-600 036 TN (India)

Nickel and Nickel based alloys especially, superalloy Inconel 718 has found its niche in many
industries, owing to its unique properties such as high oxidation resistance, corrosion resistance even at very
high temperatures and it retains a high mechanical strength under these conditions as well. Thus, it is often
used in extreme conditions, such as aircraft engine parts, chemical processing, pressure vessels, steam turbine
power plants, space vehicles, marine applications, automotive sector etc. As a result of these properties and
potential applications, a great necessity exists to understand the problems/questions associated with the
machining of such a superior material. However, Inconel 718 is considered to have poor machinability due
to its peculiar characteristics like low thermal conductivity, work hardening, presence of abrasive carbide
particles, hardness, affinity to react with tool material etc. which makes it difficult to machine. Hence, Inconel
718 is classified as the “difficult-to-cut materials”. Success in machining Inconel 718 depends largely on
overcoming several of the inherent properties of the metal such as workhardening, its tendency to weld to
the tool, intense heat generation due to low thermal conductivity, shorter tool life due to stresses and
temperature etc. Considering all the above facts, an attempt has been made in this work to understand the
machinability of superalloy Inconel 718 with respect to cutting forces, acoustic emission, and microstructural
alteration while high speed turning. The experimental investigations were carried out and the results are
presented and analyzed in this paper.
106 ISRS-2008

SP-P4

INFLUENCE OF MILLING TIME AND ATMOSPHERE


ON THE PRODUCTION OF LEADED BRASS IN THE PRESENCE
OF GRAPHITE USING MECHANOCHEMICAL MET
Farahbakhsh, Tabaian S.H., Vahdati J.
Iran University of Science and Technology.

Mechanochemical process was applied for brass alloy production using oxide powders. Alpha brass
was produced when CuO, ZnO and PbO were milled under argon atmosphere in the presence of graphite (as
reducing agent). Concurrent reduction of zinc, copper and lead oxides took place in the argon atmosphere,
whereas the reduction reactions did not proceed well in the closed chamber filled with air. These reactions
were promoted by milling time up to 100 hours. The amount of reduction tends to decrease for longer times.

SP-P5

EFFECT OF SURFACE ROUGHNESS ON SURFACE


HEAT FLUX DURING IMMERSION QUENCHING
OF STAINLESS STEEL PROBES IN WATER
Babu K. and Prasanna Kumar T.S.
Indian Institute of Technology Madras, Chennai.

During quenching, if the properties like thermal stresses, thermal strains, residual stresses and
microstructure of the steel are to be simulated using numerical methods, it is obligatory to give an accurate
boundary condition. The surface heat-transfer coefficients or heat fluxes between specimen and the quenchant
are regarded as key parameters for numerical simulation of the quenching process. Heat transfer during
quenching is very complex and is affected by parameters like surface temperature, surface condition of the
specimen, fluid properties such as viscosity, density, specific heat and all thermal physical properties of the
solid and quenchant agitation. In this paper, the effect of surface texture on the heat flux during quenching
of stainless steel probes in water has been studied. Stainless steel probes of diameter 20 mm and 50 mm long
were prepared from 304L which has no transformations during quenching. Three quench probes were
machined to different surface finish with its roughness (Ra) being . The estimation of heat flux at the P and
2.196 P, 1.289 P 0.210 quenched surface was based on Inverse Heat Conduction Problem (IHCP).
Thermocouples were inserted at the holes drilled at 2 mm below the cylindrical surface of the quench probes.
Using a computer assisted data acquisition system, the time-temperature data were recorded during quenching
of these probes in water. The IHCP algorithm gives the surface temperature of the probe along with the heat
flux using the measured temperature data as input. The results of the computation showed that the peak heat
flux increased with increase in surface roughness of the specimen. The slope of different regimes like
transition boiling, nucleate boiling and convective boiling in the cooling curve remained same. However,
there is a appreciable change in the magnitude of peak heat flux values but its corresponding surface
temperature did not vary much.
ISRS-2008 107

SP-P6
ANALYSIS AND IDENTIFICATION OF NATURAL COPPER ORE
Puthilibai a,* G. Vasudhevan b S. and Athapan c P.R.
a
Department of Chemistry, SriSairam Engineering College, West Tambaram, Chennai - 600 044, India.
b
Department of Chemistry, K.V.,Central Leather Research Institute, Adyar, Chennai - 600 020, India.
c
Department of Inorganic Chemistry, School of Chemistry, Madurai Kamaraj University, Madurai - 625 021, India.
The natural Copper ore obtained for the present project was collected from Antipatti Hill area, near
Vaigai Dam, Madurai District, situated in the state of Tamil Nadu, India. The appearance of the ore was a
mixture of deposits of blue, violet, ash and green colours. In total, the ore look like greenishblue in colour.
The present work is aimed at collecting and estimating the individual metals and anlysing the nature of the
ore and its constituents by various physicochemical methods (UV-Vis spectra, FTIR spectra, Cyclic
voltametric and Crystallographic studies). Based on the results of physicochemical studies the ore is
confirmed as a carbonate and oxide based Malachite [Cu(OH)2.CuCO3] with varying degree of Cuprite. This
study may open up a new chapter in industrial development in TamilNadu by bringing up a new industry for
processing the newly identified Copper ore.

SP-P7
MESOPOROUS Al- KIT-6 CATALYSTS FOR THE PREPARATION OF
FINE CHEMICALS: SYNTHESIS OF JASMINALDEHYDE
Prabhu A., Kumaresan L., Palanichamy M. and Murugesan* V.
Anna Univrsity, Chennai
The discovery of silica-based and metal-substituted mesoporous materials M41S has attracted intense
interest due to their high surface area, uniform pore size distribution, large pore size, and highly valuable
potential applications in catalysis, separation, adsorption, nano devices, and nanostructured materials. Many
mesoporous siliceous materials, such as MCM-48, MCM-41, SBA-15 and KIT-6, have been prepared by the
self-assembly method using long-chain surfactants as templates over the past decade.The mesoporous silica
KIT-6 was reported by Kleitz et .al[1]. The incorporation of Al into KIT-6 mesostructure was carried out by
direct synthesis method using Aluminium isopropoxide as Al source. Mesoporous aluminosilicate Al-KIT-6
was synthesized from assembly of polymer surfactant micelle as a template in strong acidic media. In the
typical synthesis of Al-KIT-6, Triblock copolymer (Pluronic P123) was used as the structure-directing
template. Mesoporous Al-KIT-6 molecular sieves with Si/Al ratios 20, 50,100 and 150 were synthesized
hydrothermally and characterized by XRD, FT-IR, BET, SEM and HR-TEM. Mesoporous Al-KIT-6 was
good phase purity from XRD analysis. The surface area of the catalysts was found to be varying from 699
to 887m2/g. The HR-TEM picture of Al-KIT-6(50) showed formation of particles of cubic morphology.
D-n-Amylcinnamaldehyde (Jasminaldehyde) has been prepared with high selectivity and using low ratios of
benzaldehyde/heptanal by means of mesoporous Al-KIT-6 molecular sieves. The synthesis of
jasminaldehyde, a compound used in the flavor industry, is not only a reaction of commercial interest, but is
also an interesting test reaction to assess the selectivity of the catalyst.The products were confirmed by GC
and GC-MS analysis.
ISRS-2008 109

Participating Institutes in ISRS 2008

Indian Universities

x Indian Institute of Technology Madras


x Indian Institute of Technology Kanpur
x Indian Institute of Technology Kharagpur
x Indian Institute of Technology Bombay
x Indian Institute of Technology Delhi
x Indian Institute of Science Bangalore
x NIT Trichy
x NIT Surathkal
x NIT Calicut
x NIT Rourkela
x VNIT Nagpur
x Anna University
x NIIST Trivandrum CSIR
x AMPRI(Formerly RRL) CSIR Bhopal
x IGCAR
x NAL Bangalore
x DMRL Hyderabad
x Central Glass & Ceramic Reasearch Institute , Kolkata
x University of Madras
x University of Calcutta
x Osmania University
x Mysore University
x ITBHU
x JNTU Hyderabad
x University of Kerala
x MGIT Hyderabad
x Cochin university
x Gauhathi University
x Loyola college, Chennai
x Jiwaji University
x G. B. Pant University
x Bharathidhasan University
x Bharathiyar University
x Kakatiya University
x Panjab University
x Presidency College Chennai
x PSG Tech Coimbathore
x Kongu Engineering College
x R V College
110 ISRS-2008

x Pt. Ravishankar Shukla University


x Sathyabama University
x SRM University
x St Joseph College
x Thiagarajar College of Engineering
x Auden Technology and Management Academy, Bangalore
x University BDT College of Engineering
x Sagar Institute of Research and Technology, Bhopal

International Universities

x Univ. of Central Florida, USA


x Univ. Teknologi MARA Malaysia
x University of California Santa Barbara, USA
x Universiti Tenaga Nasional, Malaysia
x Universität Bayreuth, Germany
x Nagaoka University of Technology, Nagaoka, Japan
x Iran University of Science and Technology, Iran
x Dalian University of Technology, China
x Delft University of Technology, Netherlands
x Technical University Darmstadt, Germany
x Shahid Bahonar University of Kerman
x Ryerson University, Canada
ISRS-2008 111

List of Sponsors

x All India Council for Technical Education (AICTE)


x Board of Research in Nuclear Sciences (BRNS)
x Department of Science and Technology (DST)
x Defense Research and Development Organisation (DRDO)
x Atomic Energy Regulatory Board (AERB)
x Council of Scientific and Industrial Research (CSIR)
x Department of Mathematics, IIT Madras
x Department of Management Studies, IIT Madras
x Department of Physics, IIT Madras
112 ISRS-2008

List of Advertisers

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x PerkinElmer (India) Pvt. Ltd.
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x Toshniwal Brothers (SR) Private Limited
x India Pistons Ltd.
x Karthik Steels Limited
x Lakshmi Technology and Engineering Industries Ltd.
x Madras Metallurgical Service Pvt. Ltd.
x Techscience Services Pvt. Ltd.
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