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A XII-A CONFERIN DE TIINA I

INGINERIA MATERIALELOR OXIDICE

12th CONFERENCE ON SCIENCE AND


ENGINEERING OF OXIDE MATERIALS

CONSILOX
Sinaia, ROMNIA, 16-20 Septembrie 2016

REZUMATE
Abstracts

-2016-
1
Cuprins/Content

Pag.
1. Industria silicailor i a compuilor oxidici din Romnia n
contextul integrrii europene
Industry of silicates and oxidic compounds of Romania in the 11
context of European integration
Doru Vladimir Pucau, Maria Georgescu, Jenica Paceagiu
2. Ultra-reactive ash: a new concept of fly ash leading to the
production of durable and cheap eco-concrete 12
Angel Palomo, Olga Maltseva and Ana Fernandez-Jimenez
3. Liani cu activare alcalin pe baz de deeuri de sticl
sinteza i proprieti
Alkali activated inorganic polymers based on waste glass -
synthesis and properties 13
Alina Bdnoiu, Taha H.Abood Al Saadi, Georgeta Voicu,
tefania Stoleriu
4. Pumice composite binders activated with Portland cement and
calcium sulphate 14
K.Cabrera-Luna, Erick Edgar Maldonado-Bandala, Demetrio
Nieves-Mendoza, Jose Ivan Escalante Garca
5. Demersuri experimentale de obinere a unor materiale
compozite autoreparante cu matrici pe baz de ciment
Experimental issues regarding obtaining of self-healing
composite materials with cementitious matrix 15
Constantin Dorinel Voinichi, Adrian Volceanov, Viviana Tufan,
Alexandru Prvan, Radu Voinichi
6. Procesul de ntrire n sistemul ciment superplastifiant
Flubet
Hardening process in the cement Flubet superplasticizer 16
system
Marcela Muntean, Ovidiu Dumitrescu
7. Alkaline aluminosilicate adhesives for gluing concrete and
ceramic 17
Pavel Krivenko, Oleg Petropavlovskii, Hryhorii Vozniuk
8. Instalaia WHPG la Fabrica Fieni un nou proiect finalizat cu
succes de ctre HeidelbergCement Romnia
The WHPG installation in Fieni Plant a new project 18
successfully completed by HeidelbergCement Romania
Florin George Bernea, Doru Vladimir Pucau
9. Senzori inteligeni de temperaturi inalte, pe carbur de siliciu,
pentru aplicaii n medii ostile
High temperature SiC smart sensors in hostile environments 19-20
applications
Gheorghe Brezeanu, Adriana Pribeanu, Doru Vladimir Pucau,
Florin Drghici, Mihai Bdil, Gheorghe Pristavu, Rzvan Pascu,

2
Florin Crciunoiu, Ion Rusu, Florin George Bernea
10. Structural, electrical and optical properties of sprayed NdF
codoped ZnO thin films 21
Amina El Fakir
11. Compozite tip beton realizate prin valorificarea unor deeuri
Concrete type composites obtained by some wastes valorisation 22
Carmen Munteanu, Maria Georgescu
12. Betoane realizate cu agregate provenite din anvelope uzate
Concrete made with used tire aggregate
Viorel Crciun, Alina Bdnoiu, Dorinel Voinichi, Radu
Voinichi 23

13. Studii privind utilizarea agregatelor reciclate din beton n


betonul permeabil
Study regarding the use of recycled concrete aggregate in 24
pervious concrete
Radu Voinichi, Alina Bdnoiu, Dorinel Voinichi, Viorel
Crciun
14. Determinri experimentale pentru evaluarea rspunsului
dinamic al betonului proaspt n procesul de compactare
Experimental measurements in order to assess the dynamic 25
response of fresh concrete
Ramona Pinoi
15. Procese dinamice de consolidare a terenurilor de fundare
folosind stabilizatori ecologici
Dynamic processes for the consolidation of foundation ground 26
using ecological stabilizers
Cornelia Dobrescu
16. Performane de rezisten a pmnturilor stabilizate cu
enzime, n procesul de compactare prin vibraii
Resistance performances of stabilized grounds with enzymes, in 27
the compaction process by vibration
Polidor Bratu, Eugen Brgu
17. Studiul compactrii betonului proaspt n regim de vibraii
forate 28
Fresh concrete compaction study in forced vibrations regime
Polidor Bratu, Ruslan Bordos
18. Influena aditivilor polimerici asupra performanelor
mortarelor de tencuial aplicate pentru sistemele compozite de
termoizolare exterioar (ETICS) 29
Polymer additives influence on the plaster mortars performance
for external thermal insulation composite systems (ETICS)
Daniela Fiat
19. Efectul aditivilor asupra caracteristicilor mortarelor pe baz
de var 30
Effect of the additives on the characteristics of the mortars based
3
on lime
Ileana Mohanu, Dan Mohanu, Ionela Petre, Mariana Coarn
20. Influena adaosului de fibre de celuloz i polietilen asupra
proprietilor tencuielilor decorative pe baz de liani organici
The influence of cellulose and polyethylene fibers admixtures on 31
the renders properties based on organic binders
Mirela Lazr
21. Evaluarea caracteristicilor mortarelor de var armate cu fibre
de cnep
Evaluation of the characteristics of lime mortars reinforced with 32
fibers of hemp
Ileana Mohanu, Dan Mohanu, Ioana Gomoiu, Adriana Moan,
Liliana Radu, Cristina Serendan
22. Mortare pe baz de nanomateriale vs. mortare tradiionale
pentru conservarea faadelor de construcii
Nanomaterials-based mortars vs. traditional mortars for building
faades preservation 33-35
Rodica-Mariana Ion, Mihaela-Lucia Ion, Raluca-Ioana Suica-
Bunghez, Radu-Claudiu Fierscu, Irina Fierscu, Sofia
Teodorescu
23. Colonizarea mortarelor de ctre bacterii i fungi
The colonization of mortars by bacteria and fungi 36-37
Ioana Gomoiu, Mdlin Enache, Ileana Mohanu, Roxana Cojoc,
Simona Neagu, Dan Mohanu
24. Nanomagnetism: superparamagnetism in iron doped
Ce(Fe2+/Fe3+)O2 nanocrystals 38
Zoran V. Popovi
25. Pulberi de ZnAl2O4 obinute prin metoda combustiei i
proprietile lor adsorbante
ZnAl2O4 powders prepared by combustion synthesis and their 39
adsorbent properties
Robert Iano, Radu Lazu, Roxana Istratie, Roxana Bbu,
Cornelia Pcurariu, Cristina Butaciu
26. Nanoporous mayenite (12 CaO7Al2O3): from insulator to
electride 40
Branko Matovic
27. Compozite ceramice uoare pe baz de cenui de
termocentral romneti obinute n cmp de microunde
Porous ceramic composites from Romanian coal-firing power 41-42
stations waste by using microwaves field technique
Enik Volceanov, Carmen Plapcianu, Marco Truccato, Simona
Badea, Adrian Volceanov
28. Study of ceramic substrates from fly ashes, coated with TiO2 slurry
for environmental application 43
Eleni Katsika, Angeliki Moutsatsou, Vayos Karayannis, Maria
Volioti, Dimitrios Tsoukleris
29. Pigmeni termoreflexivi pe baz de Zn1-XCoXAl2O4 obinut 44-45
prin metoda combustiei
4
Thermoreflective blue pigments based on combustion
synthesized Zn1-xCoxAl2O4
Robert Iano, Eliza Muntean, Cornelia Pcurariu, Radu Lazu,
Cornelia Bandas
30. Studiu comparativ asupra structurii i proprieti fotocatalitice a
nanoparticulelor de TiO2 obinute prin metoda hidrotermal
asistat de microunde i poliol
Comparison study of structures and photocatalytic activity of TiO2 46-47
nanoparticles prepared via microwave assisted hydrothermal and
polyol methods
Alberto Ion, Rzvan State, Adrian Volceanov
31. Precipitarea bacterian a carbonatului de calciumetod
alternativ de tratament a betoanelor
Bacterial calcium carbonate precipitation as an alternative
concrete treatment 48-49
Victor Fruth, Jeanina Pandele-Cusu, Irina Atkinson, Luminia
Predoan, Adriana Rusu, Iuliana Raut, Mihaela Doni, Luiza Jecu,
David Vasilescu, Alina Bdnoiu
32. Evaluarea calitii de izolare termic a produselor din vat
mineral prin metoda conductivitii termice
Thermal insulation quality assessment of mineral wool products 50
by thermal conductivity method
Marinela Ghi
33. Materiale termoizolatoare pe baz de polipropilen i
materiale silicioase
Thermal insulation materials based on polypropylene and
siliceous materials 51
Jenica Paceagiu, Zina Vuluga, Marina Martin, Liliana Radu,
Michaela Iorga, Valentin Apostol, Horaiu Pop
34. Caracteristicile mortarelor compozite termoizolante
Characteristics of thermal insulation composite mortars
Virgil Marinescu, Georgeta Velciu, Gabriela Sbrcea, Adriana 52
Moan, Mirela Menicu, Constantin Dorinel Voinichi, Gheorghe
Ghe. Ioni
35. Materiale neconvenionale pe baz de fibre vegetale utilizate n
construcii
Unconventional materials based on vegetables fibres use in 53
constructions
Cristina Dima, Adrian abrea
36. Caracterizarea fizico-mecanic a unor materiale compozite
fonoabsorbante cu diverse deeuri
Physico-mecanical characterization of some sound-absorbing 54
composite materials with various wastes
Mihai Bratu, Ovidiu Dumitrescu, Ovidiu Vasile, Ileana Nicolescu,
Luoana Florentina Pascu
37. Industria cimentului i betonului - parte integrant a
economiei circulare 55-56
Cement and concrete industry integrant part of circular economy

5
Mihai Rohan
38. GB chemistry of silicon nitride based ceramics implications
to the ceramics properties 57
Pavol Sajgalik
39. Metode combinate de mbuntirea proprietilor fizice i
chimice ale produselor industriale din sticl 58-59
Combined methods, used to improve physical and chemical
properties of industrial glassware
Vasile aragov
40. Sticle boro-fosfatice dopate, sub form de sticle de volum,
pulberi i straturi subiri obinere, structur i proprieti
Doped boro-phosphate glasses as bulk, powders and thin layers
obtaining, structure and properties 60-61
Bogdan Alexandru Sava, Lucica Boroica, Mihail Elisa, Regina
C.C. Monteiro, Olga Shikimaka, Victor Kuncser, Ionu Feraru,
Raluca Iordnescu, Zinaida Barbos, Mihaela Popa, Mihaela
Filipescu, Gabriel Socol
41. Investigation of the structural, Optical and Electrical
properties of Sb doped SnO2 thin films deposited by Spray 62
Pyrolysis
Chourouk Nassiri, Adil Hadri, Mustapha Rouchdi, Abderrahim El
hat, Boubker Fares, Larbi Laanab, Ahmed Mzerd
42. Noi matrici ceramic-vitroase pentru imobilizarea unor deeuri
de crom
New glass-ceramic matrix for the chromium wastes 63-64
immobilization
Cosmin Vancea, Giannin Mooarc, Adina Laia, Romul Marius
Jurca
43. Studiul soluiilor solide de tipul La1-xSrxCoO3 cu structur
pseudo-perovskitic (x=0,4 i 0,5)
The study of the solid solutions La1-xSrxCoO3 with 65-66
pseudoperovskite structure (x=0,4 and 0,5)
Maria Preda, Georgeta Velciu, Alina Melinescu, Virgil
Marinescu, Victor Fruth, Cristina Hornoiu
44. Creterea straturilor subiri de titanat zirconat de plumb
(PZT) pentru aplicaii n detectorii de infrarou
Growth of lead zirconium titanate (PZT) thin films for infra-red 67-68
detectors applications
Jenica Neamu, Alina Iulia Dumitru, Virgil Marinescu
45. Effect of Cu on the physical properties of ZnO synthesized by
spray pyrolysis technique 69
Abderrahim El Hat, Mustapha Rouchdi, Adil Hadri, Chourouk Nassiri,
Fatima Zahra Chafi, Boubker Fares, Najem Hassanain, Larbi Laanab,
Ahmed Mzerd
46. Structura, microstructura i comportarea electric a unor
produse ceramice sol-gel Ba1-xSrxTiO3 pentru aplicaii 70
piroelectrice
Structure, microstructure and electrical behaviour of some
6
sol-gel Ba1-xSrxTiO3 ceramics for pyroelectric applications
Adelina Ianculescu, Ioana Pintilie, Lucian Pintilie, Ctlina
Andreea Vasilescu, Alina Melinescu, Mihaela Botea, Alin Iuga,
Nicolae Drgan, Dorel Crian
47. Development of transparent conductive tin doped ZnO thin
films: Effect of tin concentration and post annealing 71
Adil Hadri, Mhamed Taibi, Ahmed Mzerd
48.
Investigation of structural, optical and electrical properties of In
doped SnO2 thin films deposited by spray pyrolysis
72
Adil Hadri, Fares Boubker, Mohammed Loghmarti, Chourouk,
Ahmed Mzerd
49. Influena condiiilor de obinere asupra caracteristicilor
aerogelurilor din SiO2
The influence of obtaining parameters upon the characteristics 73
of SiO2 aerogels
Adrian Dnu-ugui, tefania Stoleriu
50. Sinteza i proprietile unor liani cu activare alcalin de tip
borosilicatic
Synthesis and properties of alkali activated borosilicate 74
inorganic polymers
Adrian Nicoar, Taha H.Abood Al Saadi, Alina Bdnoiu,
Georgeta Voicu, tefania Stoleriu
51. Filtre ceramice aluminoase cu suprafa activ
Alumina filter ceramics with active surface 75
Adrian Tbcaru, tefania Stoleriu
52. Analiza de monitorizare a temperaturii n industria cimentului
alternativ carbur de siliciu
Temperature monitoring analysis in the cement industry the Silicon
Carbide alternative 76-77
Adriana Graiela Pribeanu, Doru Vladimir Pucau, Florin
Bernea, Gheorghe Brezeanu, Florin Drghici, Gheorghe Pristavu,
Rzvan Pascu
53. Materiale compozite destinate proteciei mpotriva radiaiilor
gamma
Composite materials used for gamma radiation shielding 78-79
Adriana Moan, Viorel Fugaru, Maria Gheorghe, Ionela Petre,
Mariana Coarn, Lidia Radu, Nastasia Saca, Eugeniu Vasile,
Roxana Truc
54. Vitroceramici n sistemul Na2O-CaO-P2O5-SiO2 pentru
ingineria tisular
Glass-ceramics in Na2O-CaO-P2O5-SiO2 system for tissue 80-81
engineering
Andreea Cristina Vjan, tefania Stoleriu
55. Modification of GFRC to increase the persistence of the fibers 82
Aleksey Kharitonov, Nina Shangina, Antonina Ryabova
56. Comportamentul materialelor de legtur dintr-un sistem de 83
7
Bariere Termice la temperaturi nalte
High temperature oxidation behaviour of alternative Bond Coat
materials as part of a TBC system
Amalia Soare, Ioana Csaki, Cristina Oprea, Sorin Soare, Cristian
Predescu
57. Effect of Nd and Tm co-doping on structural, optical and
electrical properties of ZnO thin films 84
Amina El Fakir
58. Influena fineii argilei asupra reciclrii nmolurilor de
epurare ntr-o matrice ceramic
The influence of clay fineness upon sludge recycling in a 85
ceramix matrix
Anna-Mria Szke, Marcela Muntean
59. Comportarea crmizilor refractare bazice n timpul
funcionrii cuptorului de clincher 86
The behavior of the refractory basic bricks during operation of a
clinker kiln
Bogdan Ctlin Marin, Georgeta Voicu, tefania Stoleriu
60. Evaluarea nano-pulberilor de hidroxiapatit obinute in
condiii de laborator, pentru ndeprtarea ionilor de plumb
din soluiile lor apoase
Evaluation of lab scale nano-hydroxyapatites for lead ions 87-88
removal from aqueous solutions
Christu rdei, Claudia Maria Simonescu, Cristian Onose,
Bogdan Alexandru Sava, Lucica Boroica, Dorinel Tlpeanu,
Gabriela Sbrcea
61. Hidroxiapatit substituit cu magneziu i silice pentru aplicaii
medicale
Magnesium and silicon substitution of hydroxyapatite for 89
medical application
Costel Cristian Ion, tefania Stoleriu
62. Influena sulfoaluminatului de calciu asupra proprietilor
liante ale compuilor nalt refractari din cimenturile
superaluminoase 90-91
The influence of calcium sulphoaluminate on binder properties
of the high refractory mineralogical compounds from high
alumina cements
Cristina Stancu
63. Polimorfismul principalelor faze ale clincherului de ciment
Portland raportate la ionii strini 92
Main Portland cement clinker phases polymorphism related to
foreign ions
Daniela Nstac, Luminia Predoan, Cornel Munteanu, Victor
Fruth
64. Senzori de gaze toxice i inflamabile bazai pe capacitoare
MOS pe SiC 93-94
Toxic and inflammable gas sensors based on SiC MOS
capacitors
8
Doru Vladimir Pucau, Adriana Graiela Pribeanu, Rzvan
Pascu, Florea Crciunoiu, Gheorghe Brezeanu, Florin Drghici,
Gheorghe Pristavu, Gherghina Ciortan
65. Morfologia i compoziia microsferelor anorganice utilizate n
mortare
Morphology and composition of inorganic microspheres used in
thermo insulating mortars 95
Georgeta Velciu, Virgil Marinescu, Christu rdei, Gabriela
Sbrcea, Adriana Moan, Mirela Menicu, Constantin Dorinel
Voinichi, Gheorghe Ghe. Ioni
66. Metodologii de optimizare a proceselor analitice.Modelul
matematic al sistemului optimizat.
Methodologies of optimization for analytical processes. 96-97
Mathematic model of optimized system.
Gherghina Ciortan
67. Impact of the river aggregate particle size distribution on the
quantity of cement and admixtures required for making of
concrete mixes of the same properties 98
Gordana Toplii-uri, Duan Grdi, Nenad Risti, Zoran
Grdi
68. Aspecte de mediu la stabilizarea zgurilor metalurgice (LF)
utilizate n agricultura sustenabil
Environmental aspects of the use of stabilised metallurgical ladle 99-100
furnace (LS) slags in sustainable agriculture
Lavinia Gabriela Popescu, Eniko Volceanov, Florian Zaman,
Valerica Slavescu, Ildiko Anger, Ecaterina Matei
69. Evoluia emisiilor de metale grele din fabricile de ciment n
anii 2014 i 2015 n raport cu limitrile legii
The evolution of heavy metals emissions from cement plants in 101
the years 2014 and 2015 in relation to limitation of law
Marina Martin
70. Inertizarea unui deeu industrial cu coninut de crom ntr-o
matrice liant anorganic
Inertization of an industrial waste containing chromium in a 102-103
inorganic binder matrix
Marius Prvan, Carmen Oproiu, Georgeta Voicu, Alina Bdnoiu,
Roxana Truc, Simina tefan
71. Caracterizarea fizico-morfologic a unor vitroceramici din
deeuri de sticl CRT
Physical and morphological characterisation of some glass- 104
ceramics from CRT glass wastes
Mihai Eftimie, Alina Melinescu, Eduard Marinescu
72. Synthesis and magnetic properties of Mg doped ZnO thin
films: experimental and AB-Initio study
Mustapha Rouchdi, El mehdi Salmani, Abderrahim El hat, 105
Chourouk Nassiri, Adil Hadri, Boubker Fares, Najem Hassain,
Ahmed Mzerd
73. Corelaii structur bazicitate proprieti pentru sticle din 106
9
sistemul Al2O3 NaPO3
Structure basicity properties correlations for glasses from
Al2O3 NaPO3 system
Ovidiu Dumitrescu, Dorel Radu
74. Proprieti magnetice i magneto-optice ale sticlei
aluminofosfatice dopate cu Bi i Pb
Magnetic and magneto-optical properties of Bi and Pb-doped
aluminophosphate glass 107-108
Raluca Iordnescu, Mihail Elisa, Cristina Vasiliu, Bogdan
Alexandru Sava, Lucica Boroica, Mihaela Vleanu, Victor
Kuncser, Adrian Volceanov, Mihai Eftimie, Alina Melinescu, Anca
Beldiceanu
75. Mineralogical composition of the SEN internal build-up 109
Sneana Devi, Mira Coci
76. Determinarea grosimii stratului dezalcalinizat de sticl i a
gradului de dezalcalinizare prin metoda HF- secionrii
Determination of the thickness of dealkalized layer of glass the 110-111
degree of dealkalization using the method of the section etching
by HF solution
Vasile aragov, Svetlana Raifura, Galina Curicheru
77. Intensificarea procesului de dezalcalinizare a sticlelor
industriale cu gaze acide
Intensification of the dealkalization process of industrial glasses 112-113
with acid gases
Vasile aragov, Gheorghe Duca, Ion Burcovschi
78. Sinteza i caracterizarea compozitelor de tip hidroxiapatit -
titanat de bariu pentru ingineria tisular osoas
Synthesis and characterization of hydroxyapatite - barium 114
titanate composites for bone tissue engineering
Victor Badea, Anamaria Puia, tefania Stoleriu
79. Corelaii ntre compoziie, condiiile de procesare i
microstructura clincherului portland prin utilizarea analizei
multivariate 115-116
Correlations between composition, processing conditions and
microstructure of Portland clinker using multivariate analysis
Zeno Ghizdve, Daniela Nstac, Mihai Eftimie, Adrian Volceanov

10
INDUSTRIA SILICAILOR I A COMPUILOR OXIDICI DIN ROMNIA N
CONTEXTUL INTEGRRII EUROPENE
INDUSTRY OF SILICATES AND OXIDIC COMPOUNDS OF ROMANIA IN
THE CONTEXT OF EUROPEAN INTEGRATION
Doru Vladimir Pucau1, Maria Georgescu2, Jenica Paceagiu1
1Ceprocim S.A., Bucureti, Romnia
2Academia de tiine Tehnice din Romnia

Materialul se dorete o poziionare a industriei silicailor i a compuilor oxidici din


Romnia n cadrul Uniunii Europene n care sunt prezentai principalii indicatori economici
realizai de aceast industrie n Uniunea Europeana i n Romnia. Se prezint de
asemenea nivelul atins n Romnia de principalele ramuri ale acestui domeniu (sticla,
ceramic, ciment) comparativ cu situaia din Europa. n ultima parte este redat succint o
diagnoz a industriei silicailor i a compuilor oxidici din Romnia, insistndu-se pe
punctele tari i cele slabe ale acesteia dar i pe oportunitile oferite de aceast industrie.

The paper presents the current position occupied by the industry of silicates and oxidic
compounds in Romania within the European Union as well as the main economic
indicators made by this industry in the European Union and in Romania. Also, it presents
the level attained in Romania by the main branches of this domain (glass, ceramic,
cement), as compared to the situation in Europe. The final part makes a brief diagnostic
presentation of the silicates and oxidic compounds industry in Romania, insisting upon its
strengths and weaknesses as well as the opportunities offered by this industry.

11
ULTRA-REACTIVE ASH: A NEW CONCEPT OF FLY ASH LEADING TO
THE PRODUCTION OF DURABLE AND CHEAP ECO-CONCRETE
Angel Palomo1, Olga Maltseva1, Ana Fernandez-Jimenez1
1Instituto Eduardo Torroja (CSIC), Madrid, Spain

Coal fly ash can be subject to large variations in characteristics as a function of the type of
coal burned, the operation status of the coal power plant and the ash separation
technology employed. Good quality fly ash is in demand in the cement industry (and in the
concrete plants) due to its ability to partially substitute some Portland cement (typically
between 10% and 25%).
On the other hand, coal bottom ash, due to its coarser nature, it is generally considered as
a low value by-product that may at best be used as a partial replacement for aggregates in
concretes or as geotechnical fill material. In this paper authors propose a procedure
(mechanical-chemical combined procedure) by which to transform regular coal combustion
products (fly ashes and/or bottom ashes) into Ultra-Reactive Ashes (URA).
URA is a product with very interesting cementitious characteristics which can become the
most important component of a new family of extra-durable and cheap ecoconcretes.

12
LIANI CU ACTIVARE ALCALIN PE BAZ DE DEEURI DE STICL
SINTEZ I PROPRIETI
ALKALI ACTIVATED INORGANIC POLYMERS BASED ON WASTE
GLASS - SYNTHESIS AND PROPERTIES
Alina Bdnoiu1, Taha H.Abood Al Saadi1,2, Georgeta Voicu 1, tefania Stoleriu1
1Universitatea Politehnica din Bucureti, Romnia
2 Foundation of Technical Education-Technical College-Baghdad, Iraq

n aceast lucrare se prezint sinteza i proprietile unor polimeri anorganici


(geopolimeri), obinui prin activarea alcalin a deeurilor de sticl. Aceste materiale se
obin prin amestecarea pulberii de sticl (rezultat prin mcinarea cioburilor de sticl
provenite dintr-o staie de reciclare) cu o soluie activatoare alcalin pe baz de hidroxid de
sodiu. Rezistena la compresiune a acestor liani poate atinge valori de pn la 40 MPa n
funcie de natura i dozajul pulberii de sticl folosit ca precursor i a timpului de ntrire la
60oC. Se constat existena unei bune corelaii ntre valorile rezistenei la compresiune i
microstructura pastelor/mortarelor pe baz de astfel de liani. De asemenea, in lucrare sunt
prezentate i proprietile intumescente ale acestui tip de material. Tratamentul termic al
probelor de mortar/past determin i o mbuntire a stabilitii hidrolitice a acestor
materiale.

The paper presents the synthesis and properties of inorganic polymers obtained by the
alkali activation of cullet glass powder. These materials where obtained by the mixing of
waste glass powder (produced by the grinding of cullet from a recycling facility) and an
alkaline solution based on sodium hydroxide. The compressive strength of these materials
can reach up to 40 MPa depending on the nature of waste glass used as precursor, as well
as the curing time at 60oC. A good correlation can be established between the
compressive strength values and the microstructure of alkali activated inorganic polymers
(AAIP) mortars/pastes, assessed by Scanning Electron Microscopy. The intumescent
behavior AAIP is also reported in this paper. The hydrolytic stability of these materials is
improved by the thermal treatment.

13
PUMICE COMPOSITE BINDERS ACTIVATED WITH
PORTLAND CEMENT AND CALCIUM SULPHATE
K. Cabrera-Luna1, Erick Edgar Maldonado-Bandala1, Demetrio Nieves-Mendoza,
Jose Ivan Escalante Garca2
1 Facultad de Mecnica, Campus Xalapa, Universidad Veracruzana, Xalapa, Veracruz,
Mxico
2 Centro de Investigacin y de Estudios Avanzados del IPN, Unidad Saltillo, Mxico

Research efforts worldwide have focused on developing alternative binders that would help
to reduce the greenhouse gas emissions associated to the production of Portland cement.
Various raw materials, natural or byproducts, have been studied for the development of
several types of binders. One of those greener cements are the so called supersulphated,
which are commonly formulated using about 80% blastfurnace slag and a source calcium
sulphate and an alkaline activator that is commonly clinker of Portland cement.
This paper presents results from an investigation on a novel supersulphated-type binder
which contains at least 60% volcanic pumice; the sulphatic activators were hemihydrate
and waste anhydrite, while the alkaline activator was Portland cement (PC). The Taguchi
method was used for the experimental design, which included variation in the composition
of the binder and curing temperatures within the range of 20 to 60C; a selection of 4
factors using 2 and 3 levels led to an orthogonal array L18 (21x33). The compressive
strength was the response variable. After 28 days, the optimal composition showed 20.16
MPa for a paste made of 70%pumice-20%PC-10%Anhydrite cured for 22 h at 60C then at
20C. In general, the pastes showed a trend towards higher strengths. The effect of higher
curing temperatures and higher PC content were favorable for the strength. The
microstructures showed that the pumice reacted although not very actively. Thermal
analysis evidenced the formation of C-S-H, ettringite and gypsum. Some of mortars were
cured under water and showed strength stability, which further evidenced the formation of
C-S-H. A general discussion on the effects of the experimental parameters on strength
and reaction products will be discussed.
Keywords: supersulphated cements, volcanic materials, sulphatic activation, new alkaline binders.

14
DEMERSURI EXPERIMENTALE DE OBINERE A UNOR
MATERIALE COMPOZITE AUTOREPARANTE CU MATRICI PE BAZ DE
CIMENT
EXPERIMENTAL ISSUES REGARDING OBTAINING OF SELF-
HEALING COMPOSITE MATERIALS WITH CEMENTITIOUS MATRIX
Constantin Dorinel Voinichi 1, Adrian Volceanov 2, Viviana Tufan 1, Alexandru
Prvan1, Radu Voinichi 1
1 Universitatea Tehnic de Construcii, Bucureti, Romnia
2 Universitatea Politehnica din Bucureti, Romnia

n prezenta lucrare se discut despre obinerea unor materiale compozite auto-reparante


cu matrice de ciment.
n acest sens, se dorete utilizarea ca reparant al structurii a unui adaos de clincher tratat
pentru meninerea n stare nehidratat.
Odat fisurile produse n matrice acestea vor traversa i granulele de material reparant i
vor determina hidratarea acestora cu consecine n auto-repararea structurii n timp.
Eficiena aciunii de autoreparare se evalueaz prin cantitatea de cloruri ce traverseaz
zona cu fisura i o zon sntoas dintr-un beton autoreparant mbtrnit artificial. Aceast
determinare s-a fcut dup prevederile standardului ASTM C 1202.
Rezultatele obinute au confirmat aciunea autoreparant a granulelor de clincher tratate.

This paper discusses about obtaining self-healing composite materials with cementitious
matrix.
In this respect, it is desired to use as healing of the structure an admixture of treated
clinker for keeping in unhydrated state.
Once the stress cracks are produced in the matrix these will cross the unhydrated granules
and will determine their hydration with consequences for self-healing structure in time.
The effectiveness of self-healing action is assessed by the amount of chlorides crossing
the crack area and healthy area of a self-healing artificially aged concrete. This
determination was made according to ASTM C 1202.
The results confirmed the self-healing action of treated clinker granules.

15
PROCESUL DE NTRIRE N SISTEMUL CIMENT
SUPERPLASTIFIANT FLUBET
HARDENING PROCESS IN THE CEMENT - FLUBET SUPERPLASTICIZER
SYSTEM
Marcela Muntean1, Ovidiu Dumitrescu1
1Universitatea Politehnica din Bucureti, Romnia

Lucrarea prezint studiul influenei unui superplastifiant romnesc Flubet asupra procesului
de ntrire al cimentului Portland. Flubet este o sare de sodiu i/sau de amoniu a
produsului de condensare a sulfonat naftalinei i formaldehidei. Au fost utilizate diferite
proporii de Flubet (1 3%). Pentru comparaie, s-au folosit pastele de ciment care conin
ca aditiv superplastifianii Disan (un amestec de lignosulfonat i alchil aril sulfonai). Gradul
de hidratare a permis determinarea concentraiei optime a superplastifianilor n pasta de
ciment. Prezena unei proporii optime de superplastifiani Flubet n pastele de ciment are
o influen pozitiv asupra procesului de ntrire al cimentului.

The present paper presents the study of the influence of some Romanian superplasticizer
Flubet on the cement Portland hardening process. Flubet is a sodium or/and NH4 salt of
the condensation product of naphthalene sulphonate and formaldehyde. Different
proportions of Flubet (1 3 %) were used. For comparison, the cement pastes containing
as additive Disan superplasticizers (a mixture of lignosulphonate and alkyl aryl
sulphonates) were used. Thus, we determined the optimum concentration of
superplasticizers in the cement paste by its hydration degree. The presence of an optimum
proportion of Flubet superplasticizers in the cement pastes has a positive influence upon
the hardened cement system.

16
ALKALINE ALUMINOSILICATE ADHESIVES FOR GLUING
CONCRETE AND CERAMIC
Pavel Krivenko1, Oleg Petropavlovskii1, Hryhorii Vozniuk1
1Kyiv National University of Civil Engineering and Architecture, Scientific Research
Institute for Binders and Materials, Ukraine

At present, a tendency to substitute hazardous organic adhesives in the majority of


building materials is clearly observed. This is connected with the more strict than before
requirements for health safety, fire safety and durability. The most important task is
substitution of organic binders, traditionally used as adhesives for gluing concrete, brick
and ceramics with non-hazardous inorganic binders. To solve this problem an adhesive
for concrete, brick and ceramics based on ecologically friendly alkaline aluminosilicate
binder (geocement) has been developed. This binder is itself an inorganic polymer, which
combines properties of inorganic substances (high strength and frost resistance) and
those of organic substances (elasticity, adhesion to various materials etc.) and is
analogue to alkaline aluminosilicate materials occurring in nature: zeolites, feldspathoids,
etc. Bonding strength of the geocement-based adhesives to various surfaces is higher
than 1 MPa. With taking into account high pH of the geocement stone a proper choice of
fillera and additives is important. The purpose of the study was to reveal influence of the
geocement - based adhesive composition on properties and, accordingly, on structure of
the interfacial transition zones: "concrete-concrete", "concrete-ceramics", "ceramics-
ceramics".

17
INSTALAIA WHPG LA FABRICA FIENI UN NOU PROIECT FINALIZAT
CU SUCCES DE CTRE HEIDELBERGCEMENT ROMNIA

THE WHPG INSTALLATION IN FIENI PLANT A NEW PROJECT


SUCCESSFULLY COMPLETED BY HEIDELBERGCEMENT ROMANIA
Florin George Bernea1, Doru Vladimir Pucau 2
1 HeidelbergCementRomnia S.A
2 Ceprocim S.A, Bucureti, Romnia

Procesul de fabricare a cimentului are ca efect secundar generarea de energie termic


rezidual care, n prezent, este folosit n principal pentru uscarea amestecului de materii
prime n instalaiile de mcinare sau pentru uscarea adaosurilor la mcinarea clincherului
n usctoare speciale.
ncepnd cu anul 1980 energia termic rezidual a nceput s fie folosit i pentru a
produce energie electric prin intermediul unei instalaii speciale WHPG (Waste Heat
Power Generator).
Comunicarea prezint soluia tehnic i rezultatele obinute cu o instalaie WHPG la
HeidelbergeCement Romania Fabrica de ciment Fieni.
Aceast instalaie are la baz tehnologia ORC (Organic Rankine Cycle) i realizeaz
conversia cldurii reziduale prin intermediul unui sistem ulei termal special ciclopentan in
energie electric.
Realizarea acestui proiect va conduce la scderea cu cca.25% a achiziiei de energie
electric a fabricii i va realiza n mod indirect reducerea emisiilor de CO2 contribuind
astfel la protejarea mediului inconjurtor.

A secondary effect of the cement manufacturing process is the generation of waste heat
which is currently used mainly for the drying of the raw materials mix in grinding
installations or for the drying of clinker grinding additives inside special dryers.
As of 1980, the waste heat started to be used also for the production of electrical energy by
means of a special installation WHPG (Waste Heat Power Generator).
This paper presents the technical solution and the results obtained with a WHPG at
HeidelbergCement Romania Fieni Cement Plant.
The installation is based on the ORC technology (Organic Rankine Cycle) and performs
the conversion of waste heat into electrical energy by means of a special thermal oil
system cyclopentane.
The implementation of this project will result in a ca. 25% decrease of the plants electrical
energy purchase and will indirectly achieve also the reduction of CO2 emissions, helping
thus protect the environment.

18
SENZORI INTELIGENI DE TEMPERATURI INALTE, PE CARBUR DE
SILICIU, PENTRU APLICAII N MEDII OSTILE
HIGH TEMPERATURE SIC SMART SENSORS IN HOSTILE
ENVIRONMENTS APPLICATIONS
Gheorghe Brezeanu1, Adriana Graiela Pribeanu2, Doru Vladimir Pucau2,
Florin Drghici1, Mihai Bdil1 Gheorghe Pristavu1
Rzvan Pascu3, Florin Crciunoiu3, Ion Rusu1, Florin Bernea4
1 Universitatea Politehnica din Bucureti, Romnia
2 CEPROCIM S.A., Bucureti,Romnia
3 Institutul Naional de Cercetare Dezvoltare in Microtehnologie, IMT- Bucureti, Romnia
4 HeidelbergCement, Romnia S.A, Romnia

Carbura de Siliciu (SiC) este un semiconductor de band interzis larg, folosit pentru
dispozitive electronice din structura echipamentelor de detecie ce funcioneaz n condiii
speciale. Dispozitivele comerciale pe SiC sunt folosite in prezent, datorit preului ridicat,
numai ca senzori care opereaz la temperaturi peste 200C i in medii ostile unde
utilizarea dispozitivelor pe Si este imposibil. De exemplu utilizarea, n conditii extreme, a
sondelor de temperatur ridicat, echipate cu senzori pe carbur de siliciu, poate duce la
eficientizarea costurilor i creterea fiabilitii.
Senzori de temperatur i gaz sunt adesea necesari n procese industriale. Detecia
temperaturii se poate efectua cu precizie cu diode Schottky. Cnd sunt polarizate la curent
constant, aceste dispozitive prezint o caracteristic tensiune (direct) - temperatura
liniar, doar dac parametrii electrici principali (factorul de idealitate i bariera Schottky)
sunt independeni de temperatur i au o dispersie tehnologica redus.
Lucrarea de fa investigheaz senzori de nalt temperatur, bazai pe diode Schottky pe
SiC cu parametrii precis controlai, destinai echipamentelor din industria cimentului. Se
evideniaz performanele senzorilor de temperatur pe SiC, cu accent pe posibilitatea de
operare pana la 600C, n condiii extreme, dar i pe dificultile tehnologice de fabricaie i
costurile ridicate. Pentru diodele senzor s-a proiectat un layout-ul inovator cu dispozitive de
diferite arii i terminaie cu profil rampa de oxid. Caracteristicile curent-tensiune ale
diodelor fabricate au fost msurate la diverse temperaturi pn la 450C. Variaia curentului
direct respect legea emisiei termionice pe mai multe ordine de mrime, pn la 1mA.
Astfel se demonstreaz posibilitarea integrrii acestor dispozitive n sonde inteligente de
temperatur.
Sonda mai are in componen un circuit electronic special conceput pentru conversia i
controlul precis al semnalului de la ieirea diodei senzor.
Sonda realizat cu diode senzor pe SiC a fost testat n condiii reale, ntr-o fabric de
ciment, pentru monitorizarea temperaturilor in gama 100-400C. S-a reuit urmrirea
permanent, timp de peste 10 luni, a temperaturii pe mai multe instalaii. Rezultatele
investigrii unui proces cu o temperatur in jurul valorii de 290C au fost comparate cu
datele nregistrate de o sond standard, amplasat n vecintatea senzorului pe SiC.
Diferenele de temperatur ntre sonda inteligent i cea standard au fost sub 5% pe
ntreaga perioada de testare.

19
Silicon carbide (SiC) is a promising semiconductor for harsh environment sensing
applications due to its excellent electrical and physical properties. The commercial
applications of SiC are mostly in the sensor domain.
The cost premium for SiC devices compared to their traditional semiconductor
counterparts, such as Si, will limit the usage of these devices to applications where the
material properties offer exclusive advantages.
Therefore, the main research focus in Silicon Carbide technology becomes obtaining
devices which are capable of high-temperature, harsh-environment operation. For example,
if used within temperature probes, they can reduce the cost and enhance the reliability.
The essential types of detection required in industry processes include temperature and
gas sensing as the top contenders. Accurate temperature sensors can be obtained using
SiC-Schottky barrier diodes (SBDs). When biased at constant current, these devices
exhibit linear voltage-temperature dependence provided their electrical parameters,
particularly Schottky barrier height and ideality factor, are reproducible and temperature
independent.
The paper is focused on a smart high temperature sensor, based on SiC SBDs and used in
the cement industry. The advancement status of SiC temperature sensors, with emphasis
on current difficulties and future opportunities for progress is evinced. A novel layout was
employed for fabricating the sensors. The devices have an oxide ramp field plate
termination. The forward current-voltage characteristics of the fabricated SiC SBDs have
been measured at several temperatures up to 450C. The current obeys the thermionic
emission law over many orders of magnitude, up to 1mA. This enables the use of SBDs as
high temperature sensors.
The harsh environment temperature sensor based on SiC Schottky diode is connected with
a signal procesing electronic circuit, in order to obtain a smart temperature probe.
The temperature probe was tested in a cement factory, for monitoring temperature in the
100-400C range inside different facilities. Full time tests, for several months, at
temperatures around 290C have proven differences lower than 5% between temperature
given by factory standard thermocouple-based sensors and the proposed smart-probe.

20
STRUCTURAL, ELECTRICAL AND OPTICAL PROPERTIES OF SPRAYED
NdF CODOPED ZnO THIN FILMS
Amina El Fakir
University of Mohammed V-Materials Physics Laboratory, Faculty of Sciences, Morocco

Undoped ZnO, Nd doped ZnO (NZO), and NdF co-doped ZnO (NFZO) thin films were
prepared at 350 C on glass substrates by chemical spray pyrolysis method. The effect of
cationic and anionic elements (Nd and F) on the structural, optical and electrical properties
was studied. X ray diffraction analysis indicated that all the films were polycrystalline with
hexagonal wurtzite crystal structure and that the nature of the doping atom has a strong
influence on the preferential growth direction. No sensitive evolution of the band gap is
observed upon doping. Photoluminescence measurements showed that all the films have a
strong emission band at around 380 nm and that Nd ions are optically activated. In
addition, energy transfer from the matrix to Nd3+ ions is demonstrated by excitation
photoluminescence. Layers with electrical resistivity values as low as 4.0 9 10-2 X cm were
obtained.

21
COMPOZITE TIP BETON
REALIZATE PRIN VALORIFICAREA UNOR DEEURI
CONCRETE TYPE COMPOSITES
OBTAINED BY SOME WASTES VALORISATION
Carmen Munteanu1, Maria Georgescu2
1 Universitatea Politehnica din Bucureti, Romnia
2 Academia de tiine Tehnice, Romnia

Lucrarea aduce informaii obinuite prin cercetri proprii, referitoare la prepararea i


caracterizarea unor betoane n care liantul a constat din ciment portland cu coninut variabil
de cenu de termocentral (20-70%), iar ca agregat, s-a utilizat beton vechi, concasat,
care a substituit parial sau integral, agregatul de balastier, convenional. Betoanele au
fost aditivate cu 0,9% superplastifiant policarboxilic.
Pe baza datelor experimentale, se pot stabili corelaii utile compoziie proprieti
(rezisten mecanic, impermeabilitate, rezisten la nghe-dezghe). Pe baza acestora, se
poate aprecia c este posibil valorificarea simultan a cenuii de termocentral i a
betonului vechi (concasat), prin obinerea unor betoane care, pentru anumite caracteristici
compoziionale, prezint proprieti (rezisten mecanic, impermeabilitate, rezisten la
nghe-dezghe) apropiate de ale unui beton de referin, preparat cu materiale
convenionale. O astfel de valorificare a deeurilor menionate are, desigur, implicaii
favorabile asupra mediului.

The paper brings information obtained by own researches regarding manufacture and
characterization of some concretes in which the binder was Portland cement with variable
content of fly ash (20-70%). As aggregate, an old crushed concrete was used which
substituted partial or total the conventional aggregate (of ballast-pit). A polycarboxilic type
superplasticiser (dosed as 0.9% relative the cement content) was used for all the
concretes.
On the experimental data basis some useful correlations compositions properties
(mechanical strength, impermeability, and freeze-thaw resistance) could be established.
These allow the assessment that it is possible the manufacture of some concretes by
simultaneous use of the fly ash and recycled concrete, without significant change in the
principal properties (mechanical strength, impermeability, freeze-thaw resistance). Such
waste valorization has favorable influences on the environment.

22
BETOANE REALIZATE CU AGREGATE PROVENITE DIN ANVELOPE
UZATE
CONCRETE MADE WITH USED TIRE AGGREGATE
Viorel Crciun1, Alina Bdnoiu2, Dorinel Voinichi1, Radu Voinichi1
1 Universitatea Tehnic de Construcii, Bucureti, Romnia
2 Universitatea Politehnica din Bucureti, Romnia

Problemele legate de reciclarea anvelopelor uzate au condus la dezvoltarea de diverse


utilizri pentru aceste deeuri industriale. Caracteristicile mecanice ale betoanelor realizate
cu aceste tipuri de deeuri au fost studiate ncepnd cu anii 1990. Betoanele realizate cu
deeuri provenite din anvelope au fost realizate pentru utilizarea lor n lucrri care s
absoarb ocuri (capete de pod, acoperirea separatoarelor de sens etc.)
n aceast lucrare au fost realizate probe din beton cu agregate reciclate din anvelope
cu/fr fibre, fiind evaluate rezultatele rezistenei la compresiune, densitii, modulului
static de elasticitate i rezistenei la ngh-dezghe. De asemenea, s-au efectuat teste
pentru determinarea energiei absorbite la rupere.

The problems related to the dumping used tires have led to the development of various
recycling methods for this industrial waste. The performance of concrete that contains
rubber aggregate made from used (waste) tires has been studied since early 1990s.
Concrete with waste tire were used as shock absorber materials for bridgeheads, covering
sense separators etc.
In this paper we present results regarding the preparation and properties of concrete with
recycled aggregate from used tires with/without fibers. The main properties assessed for
this type of concrete were: compressive strength, density, static modulus of elasticity and
freeze-thaw resistance. Also, tests were conducted to determine the energy absorbed at
rupture.

23
STUDII PRIVIND UTILIZAREA AGREGATELOR RECICLATE DIN BETON
N BETONUL PERMEABIL
STUDY REGARDING THE USE OF RECYCLED CONCRETE AGGREGATE
IN PERVIOUS CONCRETE

Radu Voinichi1, Alina Bdnoiu2, Dorinel Voinichi1, Viorel Crciun1


1 Universitatea Tehnic de Construcii Bucureti, Romnia
2 Universitatea Politehnica din Bucureti, Romnia

Betonul permeabil este un tip de beton cu un coninut redus sau zero de particule fine.
ntruct amestecul de beton conine o cantitate redus de parte fin, acesta prezint o
structur foarte poroas ceea ce permite apei s curg direct prin el. n ultimul timp,
interesul pentru betonul permeabil a crescut, dar totui exist nc lips de cunotine cu
privire la modul cnd i unde betonul permeabil este necesar.
n lucrare sunt prezentate rezultatele n ceea ce privete utilizarea de agregate provenite
din beton reciclat (RCA) utilizate n compoziia betonului permeabil, n special efectele
asupra densitii, rezistenei la compresiune, permeabilitii i rezistenei la nghe-dezghe.
Au fost realizate probe cilindrice din beton permeabil cu agregate reciclate grosiere sort 4/8
mm i 8/16 mm. Rezultatele obinute au fost comparate cu rezultatele obinute pe betonul
de referin - beton cu permeabilitate ridicat realizat doar cu agregate naturale sort 4/8
mm i 8/16 mm.

Pervious concrete is a form of concrete that uses a small amount or no sand in the mix.
This concrete becomes highly porous to the point that water can flow directly through it.
Recently was noticed an increase of the scientific and practical interests in pervious
concrete, but there is still a lack of knowledge on how and when pervious concrete is
appropriate to be used.
In this paper we present results regarding the use of recycled concrete aggregate (RCA) in
pervious concrete; this study focuses on the RCA effects on the density, compressive
strength, permeability and freeze-thaw resistance of concrete.
Cylindrical specimens of pervious concrete with different percentage of RCA (4/8 mm and
8/16 mm sorts) were cast and tested after different periods of time. The results were
compared with the result obtained on the reference concrete - pervious concrete made only
with natural aggregates (NA) - 4/8 mm and 8/16 mm sorts.

24
DETERMINRI EXPERIMENTALE PENTRU EVALUAREA
RSPUNSULUI DINAMIC AL BETONULUI PROASPT N PROCESUL DE
COMPACTARE
EXPERIMENTAL MEASUREMENTS IN ORDER TO ASSESS THE
DYNAMIC RESPONSE OF FRESH CONCRETE
Ramona Pinoi
Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii ICECON S.A.,
Romnia

Stabilirea duratei optime de compactare prin vibrare pe cale experimental reprezint un


obiectiv major pentru evaluarea rezistenei betonului.
n acest context, durata optim de vibrare a fost corelat cu durata de malaxare pentru
aceeai clas de beton i regim de vibrare.
Se constat c mrirea duratei de vibrare, peste limita optim, poate duce la micorarea
rezistenei betonului sub valoarea iniial a betonului nevibrat.

Establishing the optimal vibratory compaction duration using experiment means is a major
goal for the concrete compressive strength assessment.
In this context, the optimal vibratory compaction duration is correlated with the mixing time
for the same concrete class and vibrating regime.
It is determined that increasing vibratory compaction duration, over the optimum limit, may
cause a decrease of the concrete compressive strength below the initial value of the non-
vibrate concrete.

25
PROCESE DINAMICE DE CONSOLIDARE A TERENURILOR
DE FUNDARE FOLOSIND STABILIZATORI ECOLOGICI
DYNAMIC PROCESSES FOR THE CONSOLIDATION OF FOUNDATION
GROUNDS USING ECOLOGICAL STABILIZERS
Cornelia Dobrescu
Institutul Naional de Cercetare-Dezvoltare n Construcii, Urbanism i Dezvoltare
Teritorial Durabil -INCD URBAN INCERC, Romnia

Lucrarea prezint efectul vibraiilor transmise terenului de fundare tratat cu stabilizatori


ecologici n vederea consolidrii.
Soluiile tehnice sunt utilizate n procesul dinamic al consolidrii i stabilizrii pmnturilor
cu portan redus pentru realizarea fundaiilor de construcii.

The paper presents the effect of vibration transmitted to soil foundation treated with organic
stabilizers for the purpose of consolidation.
Technical solutions are used in the dynamic process of consolidation and stabilization
applied to soils with reduced bearing capacity in order to perform building foundations.

26
PERFORMANE DE REZISTEN A PMNTURILOR STABILIZATE
CU ENZIME, N PROCESUL DE COMPACTARE PRIN VIBRAII

RESISTANCE PERFORMANCES OF STABILIZED GROUNDS WITH


ENZYMES, IN THE COMPACTION PROCESS BY VIBRATION

Polidor Bratu1, Eugen Brgu2


1 Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii ICECON S.A.,
Romnia
2 Universitatea Dunrea de Jos, Galai, Romnia

Se prezint rezultatele experimentale i efectele de mrire a modulului de elasticitate


longitudinal pentru pmnturile argiloase stabilizate cu enzime.
Astfel, se evideniaz comportarea pmnturilor argiloase naturale sau stabilizate sub
influena regimului de vibraii.

The paper presents the experimental results and the effects of increasing the longitudinal
elasticity modulus for clay grounds stabilized with enzymes.
Thus, it highlights the behavior of natural or stabilized clay grounds under the influence of
the vibration regime.

27
STUDIUL COMPACTRII BETONULUI PROASPT
N REGIM DE VIBRAII FORATE
FRESH CONCRETE COMPACTION STUDY
IN FORCED VIBRATIONS REGIME

Polidor Bratu1, Ruslan Bordos2


1 Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii ICECON S.A.,
Romnia
2 Universitatea Dunrea de Jos, Galai, Romnia

n lucrare se prezint rezultatul studiilor analitice i experimentale efectuate pentru


optimizarea compactrii betonului proaspt, pus n oper.
Astfel pe baza modelelelor compuse de tip Voigt-Kelvin sau Maxwell a fost stabilit
rspunsul dinamic, energia disipat i curbele histeretice pentru diverse regimuri de vibraii
forate.

The paper presents the results of the analytical studies and experiments performed for the
optimization of the fresh concrete compaction process.
Thus, based on the Voigt-Kelvin or Maxwell composed models there were established the
dynamic response, the energy dissipation and the hysteretic curves for different regimes of
forced vibration.

28
INFLUENA ADITIVILOR POLIMERICI ASUPRA PERFORMANELOR
MORTARELOR DE TENCUIAL APLICATE PENTRU SISTEMELE
COMPOZITE DE TERMOIZOLARE EXTERIOAR (ETICS)

POLYMER ADDITIVES INFLUENCE ON THE PLASTER MORTARS


PERFORMANCE FOR EXTERNAL THERMAL INSULATION COMPOSITE
SYSTEMS (ETICS)
Daniela Fiat
Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii ICECON S.A.,
Romnia

n prezenta lucrare a fost studiat influena pulberilor redispersabile i a eterilor de celuloz


n tencuielile minerale aplicate ca ultim strat n sisteme de izolare termic la exterior.
Pornind de la reete tradiionale, utiliznd aditivi polimerici specifici pentru sistemele ETICS
au fost concepute compoziii originale n care s-a modificat concentraia de aditiv polimeric
(pulbere redispersabil) cu impact pe studiul influenei caracteristicilor fizico-mecanice.

The paper presents the results of the studies performed on the influence of redispersible
powders and of the cellulose ethers in mineral plasters applied as the last layer in exterior
thermal insulation composite systems.
Starting from traditional recipes, using polymeric additives specific for ETICS, there were
developed original composition in which the polymer additive (redispersible powder)
concentration was modified and it was studied the impact of the concentration influence on
physical and mechanical characteristics.

29
EFECTUL ADITIVILOR ASUPRA CARACTERISTICILOR MORTARELOR
PE BAZ DE VAR
EFFECT OF THE ADDITIVES ON THE CHARACTERISTICS OF
THE MORTARS BASED ON LIME

Ileana Mohanu1, Dan Mohanu2, Ionela Petre1, Mariana Coarn1

1 CEPROCIM S.A., Bucureti, Romnia


2 UniversitateaNaional de Arte, Bucureti, Romnia

n lucrrile de conservare restaurare se urmrete utilizarea unor materiale compatibile cu


elementele constitutive ale monumentelor istorice asupra crora se intervine. n cazul
monumentelor istorice construite pn n secolul XIX sunt recomandate mortarele pe baz
de var.
Cercetrile, ale cror rezultate sunt prezentate n aceast lucrare, au avut ca scop
obinerea unor mortare pe baz de var care s permit realizarea unor operaiuni de
conservare-restaurare mai durabile. n acest sens, au fost utilizate trei tipuri de aditivi
(antrenor de aer, hidrofobizant, retenie ap) pentru a observa n ce msur sunt
influenate proprietile n stare ntrit i de durabilitate ale mortarelor de var.
Caracteristicile evaluate au fost: densitate aparent, absorbie ap prin capilaritate,
permeabilitate la vapori de ap, rezistena la ncovoiere i compresiune, rezistena la
nghe-dezghe, rezistena la imersare n soluie de sulfat de sodiu. S-a constatat o
mbuntire a rezistenelor mecanice n cazul utilizrii aditivilor antrenor de aer i
hidrofobizant i creterea rezistenei la nghe-dezghe, n cazul utilizrii aditivului antrenor
de aer.

In the works of preservation-restoration it is followed the using of some materials


compatible with constitutive elements of historical monuments on which is intervened. In
case of historical monuments constructed until the XIX-th century, mortars based on lime
are recommended.
The researches, on which the results are presented in this paper, had as scope obtaining
of some mortars based on lime that allow performing of some operations of preservation-
restoration more durable. In this way, were used three types of additives (air entraining,
water-repellent, water retention) in order to remark in what measure the properties in
hardened state and of durability of lime mortars are influenced. Evaluated characteristics
were: apparent density, water absorption through capillarity, water vapor permeability,
flexural and compressive strength, resistance at freezing-thawing, resistance at immersion
in solution of sodium sulphate. An improvement of mechanical resistance was stated in
case of using the additives of air entraining and water-repellent and increase of the
resistance at freezing-thawing, in case of using the additive of air entraining.

30
INFLUENA ADAOSULUI DE FIBRE DE CELULOZ I POLIETILEN
ASUPRA PROPRIETILOR TENCUIELILOR DECORATIVE PE BAZ DE
LIANI ORGANICI
THE INFLUENCE OF CELLULOSE AND POLYETHYLENE FIBERS
ADMIXTURES ON THE RENDERS PROPERTIES BASED ON ORGANIC
BINDERS

Mirela Lazr
Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii-ICECON S.A,
Romnia
.
n lucrare se prezint rezultatele referitoare la proprietile unor tencuieli decorative pe
baz de liani organici (acrilici, siliconici) cu/fr adaos de fibre de celuloz i polietilen.
Proprietile tencuielilor decorative care au fost determinate sunt: permeabilitatea la ap,
permeabilitatea la vaporii de ap, aderena la suport, durabilitatea la nghe/dezghe.
Rezultatele evideniaz tencuielile decorative pe baz de liani organici cu adaos de fibre
de celuloz i polietilen care prezint o cretere cu 200% a valorilor aderenei la suport
att iniiale ct i dup nghe/dezghe raportat la aderena la suport a tencuielilor
decorative fr adaos de fibre precum i mbuntirea proprietilor de permeabilitate la
ap i vaporii de ap. Fibrele de celuloz i polietilen nglobate n masa tencuielilor lichide
prezint rol de armare datorit coeziunii mai bune ntre particulele de liant organic i
materialele de umplutur anorganice.

The paper presents the tests results concerning the influence of cellulose and polyethylene
fibers admixtures, on the properties of renderings based on organic binders (acrylic,
silicone). The decorative renderings properties that were determined are: water
permeability, water vapor permeability, adhesion to the support, the resistance to freeze /
thaw. The results highlight the performances decorative renderings based on organic
binders with cellulose and polyethylene fibers admixtures, showing a 200% increase values
of adherence to support both initially and after freeze / thaw test compared with the
adherence to the support of decorative renderings without cellulose and polyethylene fibers
admixtures. At the same time, the water permeability, water vapor permeability proprieties
were improved. The cellulose and polyethylene fibers contained in the mass of the
renderings are reinforcing elements, due to the better cohesion between the organic binder
particles and inorganic filler materials.

31
EVALUAREA CARACTERISTICILOR MORTARELOR DE VAR ARMATE
CU FIBRE DE CNEP
EVALUATION OF THE CHARACTERISTICS OF LIME MORTARS
REINFORCED WITH FIBERS OF HEMP
Ileana Mohanu1, Dan Mohanu2, Ioana Gomoiu3, Adriana Moan1, Liliana Radu1,
Cristina Serendan2
1 CEPROCIM S.A., Bucureti, Romnia
2Universitatea Naional de Arte, Bucureti, Romnia
3 Institutul de Biologie, Academia Romn, Bucureti, Romnia

Bisericile de lemn pictate in fresc, prezente exclusiv n zona de sud a Romniei,


reprezint o categorie restrns, prea puin explorat i, n plus, ameninat cu dispariia.
Principala problem de conservare o reprezint refacerea aderenei frescei la suportul de
lemn.
Aceast lucrare prezint rezultatele primelor cercetri privind obinerea unor materiale care
s serveasc n procesul de consolidare a picturilor murale pe suport de lemn. n acest
scop au fost realizate o serie de mortare pe baz de var hidratat, nisip de ru i fibre de
cnep. Pentru mbuntirea aderenei a fost adugat un aditiv acrilic. Au fost evaluate
diferite caracteristici ale mortarelor n stare ntrit, cum ar fi: densitate aparent, absorbie
de ap prin capilaritate, permeabilitate la vapori de ap, rezisten la ncovoiere i
compresiune, rezistena la fenomenul de biodegradare. Aderena a fost verificat prin
aplicarea mortarelor pe plcue confecionate din lemn de stejar. S-a constatat o
mbuntire a aderenei la suportul de lemn n cazul mortarelor n care a fost adugat un
aditiv acrilic.
Mulumiri: Aceast lucrare a fost realizat prin programul Parteneriate n domenii prioritare PN
II, derulat cu sprijinul MEN UEFISCDI, proiect nr. PNIIPTPCCA201341311.

The churches of wood painted in fresco, present exclusively in south zone of Romania,
represents a limited category, very little explored and, additional, threaten with
disappearance. The main problem of preservation is represented by remaking of the
adherence of fresco at wood support.
This paper presents the results of the first researches regarding the obtaining of some
materials which will serve in the process of consolidation of mural pictures on wood
support. For this purpose were performed a series of mortars based on hydrated lime, river
sand and fibers of hemp. For improvement of the adherence and acrylic additive was
added. Different characteristics of mortars in hardened state were evaluated, such as:
apparent density, absorption of water by capillarity, water vapor permeability, flexural and
compressive strength, resistance at the phenomenon of biodegradation. The adherence as
checked by application of the mortars on plates made from wood of oak. It was stated an
improvement of the adherence at wood support in the case of the mortars in which an
acrylic additive was added.

32
Acknowledgments: This research was carried out with financial support of the National Research
Program Partnerships in priority areas PN II, MEN UEFISCDI, Project no. PNIIPTPCCA
201341311.

MORTARE PE BAZ DE NANOMATERIALE VS. MORTARE


TRADIIONALE PENTRU CONSERVAREA FAADELOR DE
CONSTRUCII
NANOMATERIALS-BASED MORTARS VS. TRADITIONAL MORTARS
FOR BUILDING FAADES PRESERVATION
Rodica-Mariana Ion1, 2, Mihaela-Lucia Ion3, Raluca-Ioana Suica-Bunghez1,
Radu-Claudiu Fierscu1, Irina Fierscu1, Sofia Teodorescu4
1 Institutul Naional de Cercetare i Dezvoltare pentru Chimie si Petrochimie - ICECHIM,
Bucureti, Romnia
2 Universitatea Valahia, Departamentul Materiale, Trgovite, Romnia
3 Universitatea Valahia, Facultatea de Istorie, Trgovite, Romnia
4 Institutul de Cercetare tiinific i Tehnologic Multidisciplinar, Universitatea Valahia

din Trgovite, Romnia

Mortarul este esenial n conservarea patrimoniului cultural. Cel mai important aspect este
compatibilitatea noului mortar cu cel existent. Pentru cldirile cu un mortar de var,
aplicarea unui mortar din ciment, implic un proces de degradare din cauza prezenei de
gips i substane alcaline, care vor provoca reacii de sulfatare i alcalin-silicatice. De
asemenea poate avea loc deteriorarea ireversibil fie la suprafee i n structurile tratate.
Exist unele efecte importante induse de prezena varului liber. Cristalizeaza n goluri, cu
reducerea dimensiunii acestora i creterea aciunii lor capilare. Evaporarea apei cu
apariia de micro-fisuri contracie-, ce este cauzat de un control inadecvat al adsorbiei
umiditii de ctre zidrie. De aceea mortarul este lipsit de apa necesar pentru hidratare i
ca rezultat mortarul devine friabil. Oxidul de calciu nu este hidraulic i are nevoie de
contact cu aerul pentru a re-absorbi CO2 i a reconstitui CaCO3 sau calcar (carbonatare),
ntr-un timp foarte lung. Din cauza fineii sale, varul induce un necesar de ap, crete
capilaritatea prin cristalizarea n golurile existente, i pentru a reduce dimensiunea
golurilor, care afecteaz rezistena la nghe, peretele devine din ce n ce mai sensibil la
nghe. Varul este higroscopic, atrage apa i absoarbe srurile, ambele responsabile
pentru ndeprtarea mortarului.
n domeniul diagnosticului de restaurare arhitectural, sunt studiate materialele vechi i
dezintegrarea n medii agresive, prin intermediul unor studii de caz (faad de arhitectura
veche din Romnia). Anumite proprieti (capilaritatea, porozitatea, rezistena la nghe-
dezghe, sruri) sunt testate la diferite suprafee de faad, n scopul de a identifica
materialele existente i pentru a selecta materialele potrivite utile pentru restaurare.
Studiile de microscopie permit observarea prezenei principalelor semne de alterare
(alterarea cromatic, alveolizarea, formarea de vezicule, dezagregare diferenial,
eflorescene, decoeziunea, exfolierea i detaarea, fisurile, exfolierea, dezagregarea i
pierderile de mas), EDXRF i ICP-AES permit determinarea compoziiei elementare a

33
eantionului, n timp ce GC-MS ne permit, identificarea rinii de conifere din adezivul
folosit pentru a lega vopseaua la suportul de perete.

Compoziia n compui i mbtrnirea au fost analizate prin spectroscopie FTIR i Raman.


Prezena acizilor grai, diacizi, hidroxi acizi, alcooli cu caten lung i modele de
alcanispecifice a evideniat prezena uleiurilor vegetale i rainii de conifere. De asemenea,
parametrii de culoare CIELAB constituie o dovad a procesului de alterare n timp.
Mai mult dect att noile materiale pentru o restaurare compatibil i durabil a
materialelor antice sunt investigate ca materiale anorganice (consolidani fosfatici,
nanomateriale oxidice, etc.) i mortare de reparaii pentru cldiri vechi.
Nanoparticulele consolidanti anorganici ofer instrumente versatile i extrem de eficiente
pentru a stopa procesele de degradare ce altereaz suprafeele, sunt foarte stabile chimic
i favorizeaz conservarea suprafeele pereilor, asigurnd o durat lung a efectelor de
consolidare, fr efecte secundare.
Referinte
1. R.M. Ion, et al., Applied Surface Science, 358, part B, 2015, pp. 612-618.
2. RM Ion, et al., Key Engineering Materials, 660(2015), pp. 383-388

Mulumiri: Aceast lucrare a fost elaborat cu suportul financiar al proiectelor PN II 261/2014, PNII 222/2012
i PN 16.31.02.04.

The mortar is essential for the preservation of cultural heritage. The most important aspect
is the compatibility of the new mortar with the existing one. For the buildings with a lime
mortar, the application of cement mortar involves a decay process due to the presence of
gypsum and alkalis that will cause sulphate and alkali-silica reactions. Irreversible damage
can occur either at surfaces and in structures, too. There are some important effects
induced by the presence of free lime. It crystallises in the voids, reducing their size and
increasing their capillary action. The evaporation of this water leaves micro cracks in the
mortar shrinkage-, which is caused by an inadequate suction control of the masonry units.
The mortar is therefore deprived of the water necessary for its hydration and as result the
mortar becomes friable. Free lime is not hydraulic and needs contact with air to re-absorb
CO2 and reconstitute itself to CaCO3 or limestone (carbonation) through a very long time.
Due to its fineness, lime increase water demand in the mortar, increases capillarity by
crystallising in the voids, and reduce the voids size, affecting the frost resistance, the wall
becoming more susceptible to frost damage. Lime is hygroscopic, attracts water and
absorbs salts, both responsible for mortar removing.
In the field of diagnostics for architectural restoration, ancient materials and their decay in
aggressive environments are studied, through case-histories (ancient architecture faade
in Romania). Some properties (capillarity, porosity, freese-thaw resistence, salts) are
tested on different faade surfaces, in order to identify the existing materials and to select
the proper materials useful for restoration. Microscopy studies allows to observe the
presence of the main weathering signs (chromatic alteration, alveolization, blistering,
differential disaggregation, efflorescence, decohesion, exfoliation and detachment,

34
cracking, delamination, disaggregation, flaking, loss), EDXRF and ICP-AES allow
elemental composition of sample, while GC-MS allow us, the identification of the coniferous
resin from the glue used to link the paint to the wall support.

The composition and aging compounds found have been analyzed by FTIR and Raman
spectroscopy.The presence of fatty acids, diacids, hydroxy-acids, long chain alcohols and
specific alkane patterns highlighted the presence of plant oils and pine resin. Also, the
CIELAB color parameters are a proof of the weathering process in time.

Moreover new materials for a compatible and durable restoration of ancient materials are
investigated as inorganic consolidating materials (phosphatic consolidants, oxide
nanomaterials, etc.) and repair mortars for ancient building. Inorganic consolidants
nanoparticles offer versatile and highly efficient tools to invert the degradation processes
altering surfaces and are highly chemically stable and preserve the wall surfaces, ensuring
long-lasting consolidation effects without the side effects.

References
1. R.M. Ion, et al., Applied Surface Science, 358, part B, 2015, pp. 612-618.
2. RM Ion, et al., Key Engineering Materials, 660(2015), pp. 383-388

Acknowledgements: This paper has been prepared with the financial support of the projects PN II
261/2014, PNII 222/2012 and PN 16.31.02.04

35
COLONIZAREA MORTARELOR DE CTRE BACTERII I FUNGI
THE COLONIZATION OF MORTARS BY BACTERIA AND FUNGI
Ioana Gomoiu1, Mdlin Enache2, Ileana Mohanu3, Roxana Cojoc2, Simona Neagu2,
Dan Mohanu1
1Universitatea Naional de Arte, Bucureti, Romnia
2 Institutul de Biologie, Academia Romn, Bucureti, Romnia
3 CEPROCIM S.A., Bucureti Romnia

Structura poroas a mortarelor i depunerile organice sunt favorabile pentru


microbiodeteriogeni deoarece pot fi ni ecologic pentru microorganismele autotrofe sau
att ni ecologic precum i substrat nutritiv pentru microorganismele heterotrofe.
Colonizarea de origine microbian i biodeteriorarea picturilor murale au ca rezultat
deteriorri structurale i estetice datorit degradrii lianilor organici, biomineralizrii,
biofilmelor colorate i decolorrii. Este un proces complex care demonstreaz interaciunea
microorganismelor cu substratul i mediul nconjurtor; are un impact major n elaborarea
strategiei de restaurare i stabilirea metodelor de prevenie. Mortarul original i cel de
intervenie din trapeza complexului monastic Hurezi din Romnia s-au analizat din punct
de vedere structural i microbiologic. Analiza efectuat in situ pe peretele de nord i pe cel
de vest, a pus n eviden: fisuri, zone mici i extinse colorate n roz la nivelul stratului
pictural, mortarului original i de intervenie, zone mici de culoare neagr pe mortarul de
intervenie i eflorescene albe i roz n special pe mortarul de intervenie. Observaiile la
microscopul optic (efectuate in situ), cele la microscopul optic i microscopul electronic cu
baleiaj (efectuate n laborator) au confirmat originea microbian a acestora: bacterii n
zonele colorate n roz i fungi n cele colorate n negru. Peste suportul picturii murale
format din dou straturi (arriccio i intonaco) s-a aplicat stratul pictural n stil bizantin.
Aceeai structur s-a identificat i la mortarul de intervenie folosit pentru a acoperi
lacunele din partea inferioar i median a pereilor. Stratul de arriccio s-a aplicat pe
crmid i conine var carbonatat ca liant, respectiv nisip de ru n proporie de 65% ca
agregat. Stratul de intonaco conine var carbonatat ca liant, 6-5% nisip de ru ca agregat
mineral i fibre de cnep tiate cu rol de armare. Difracia de raze X i microscopia optic
efectuate pe seciuni subiri obinute din probe recoltate de pe peretele de nord i vest au
confirmat prezena calcitului ca liant i a nisipului de ru ca agregat n stratul de arriccio. In
probele de sfrmturi (proba 6NM) s-a identificat o sare a carbonatului de sodiu
(Na3H(CO3)22H2O - throne). Caracteristicile mortarelor susin aderarea bacteriilor i a
fungilor, iar depozitele organice reprezint sursa nutritiv pentru multiplicarea
biodeteriogenilor concretizat prin colonizarea substratului.

Aceast lucrare a fost realizat prin programul Parteneriate n domenii prioritare PN II, derulat cu
sprijinul MEN UEFISCDI, proiect nr. PN-II-PT-PCCA-2013-4-0660.

36
The porous structure of mortars and organic deposits make them to act as host to
microbiodeterigens, offering either only ecological niche for autotrophic microorganisms or
both niche and nutrients for heterotrophic microorganisms. Microbial colonization and
biodeterioration of mural paintings in historical monuments have as result structural and
aesthetic damages due to degradation of organic binders, biomineralization, colored
biofilms and discoloration. It is a complex process that illustrates the interaction of
microorganisms with the substratum and environment having a major impact for
establishing prevention and restoration strategies. The original and infilling mortar from
refectory of Hurezi monastic complex-Romania was analyzed from structural point of view
as well as from microbiological point of view. Visual inspection performed in situ on the
northern and western walls revealed: cracks, small and large pink areas on the pictorial
layer, original and infilling mortar, small black areas on the infilling mortar and white and
pink efflorescences appearing mostly on the infilling mortar. Microscopical observation
performed both in situ and in laboratory (Optical Microscope and Scanning Electron
Microscope) revealed a pink biofilm and small black colonies. Microbiological analysis
confirmed the bacterial origin of the pink biofilm and fungal origin of black colonies. The
support of the painting mural painting is composed of two distinct layers of mortar on which
paint layers were applied following the Byzantine painting style. The same structure of the
plaster was used by the restorers for the infilling mortar of large areas of lacunae at the
bottom and at the middle of the walls. The original plaster and the infillings have two layers
structure. The arriccio, applied on brick masonry, consists of calcium carbonate (calcite) as
binder and river sand (quartz, potassic feldspar, muscovite) in proportion of about 65 % as
mineral aggregate. The intonaco, consists of calcium carbonate as binder, 6-5 % river sand
as mineral aggregate and short cut fibres of hemp as vegetal aggregate for reinforcement
of the mortars. In both layers the calcium carbonate originates from carbonated lime.
Analyze of diffraction with X-rays performed on samples taken from Northern wall (compact
samples and chippings), put into evidence for arriccio layer compounds of binder lime
(calcite) and of aggregate river sand (quartz, potassium feldspar, muscovite). In the
samples of debris (for example 6NH) was put into evidence the presence of a salt of
sodium carbonate (Na3H(CO3)2 2H2O - throne). The characteristics of the mortars sustain
adhesion of the bacteria and fungi and organic deposits their multiplication which is
reflected in colonization of the substrate.

Acknowledgments: This research was carried out with financial support of the National Research
Program Partnerships in priority areas PN II, MEN UEFISCDI, grant no.PN-II-PT-PCCA-2013-4-0660.

37
NANOMAGNETISM: SUPERPARAMAGNETISM IN IRON DOPED
Ce(Fe2+/Fe3+)O2 NANOCRYSTALS
Zoran V. Popovi
Center for Solid State Physics and New Materials,
Institute of Physics, The University of Belgrade, Serbia

We have measured the magnetization of undoped and Fe2+(3+) doped CeO2-y


nanocrystals at various temperatures and magnetic fields. In the case of Fe-doped
samples, the magnetization versus magnetic field dependence is well fitted with a weighted
Langevin function. A blocking temperature of about 20 K is obtained both from the ZFC/FC
curves and from the coercive field against temperature dependence. The temperature and
field dependence of the magnetization clearly shows the presence of nanosized particles
which exhibit superparamagnetic behavior.

38
PULBERI DE ZnAl2O4 OBINUTE PRIN METODA COMBUSTIEI I
PROPRIETILE LOR ADSORBANTE
ZnAl2O4 POWDERS PREPARED BY COMBUSTION SYNTHESIS AND
THEIR ADSORBENT PROPERTIES
Robert Iano*, Radu Lazu, Roxana Istratie, Roxana Bbu, Cornelia Pcurariu,
Cristina Butaciu

Universitatea Politehnica Timioara, Facultatea de Chimie Industrial i Ingineria Mediului,


Timioara, Romnia

Diferite pulberi de aluminat de zinc, ZnAl2O4, s-au obinut prin metoda combustiei, pornind
de la soluii apoase de acetat de zinc (sau azotat de zinc), azotat de aluminiu, uree,
asparagin i azotat de amoniu. Iniierea reaciilor de combustie auto-propagate s-a
realizat prin nclzirea rapid a soluiilor precursoare la 450 C ntr-un cuptor electric
prenclzit. Probele rezultate au fost caracterizate din punct de vedere compoziiei fazale,
dimensiunii cristalitelor, suprafeei specifice i morfologiei particulelor. n ncercarea de a
explica formarea pulberilor de aluminat zinc i proprietile acestora, s-au luat n
considerare cantitatea total de gaze eliberate n timpul reaciilor de combustie i
aspectele de natur termodinamic (entalpia standard de reacie i energia liber Gibbs
standard). Capacitatea de adsorbie a pulberilor aluminat de zinc n raport cu metil orange
i albastru de metilen a fost investigat i discutat n legtur cu suprafa specific,
ncrcarea suprafeei i condiiile de sintez.

Various zinc aluminate, ZnAl2O4, powders were prepared by combustion synthesis, starting
from aqueous solutions of zinc acetate (or zinc nitrate), aluminium nitrate, urea, asparagine
and ammonium nitrate. The self-propagating combustion reactions were ignited by rapidly
heating the precursor solutions at 450 C inside a preheated electric furnace. The resulted
samples were characterized in terms of phase composition, crystallite size, specific surface
area and particle morphology. The total amount of gases released during combustion
reactions and thermodynamic aspects (standard heat of reaction and standard Gibbs free
energy) were considered in an attempt to explain the formation of zinc aluminate powders
and properties thereof. The adsorption capacity of zinc aluminate powders with respect to
methyl orange and methylene blue was investigated and discussed in relation to specific
surface area, surface charges and synthesis conditions.

39
NANOPOROUS MAYENITE (12CaO7Al2O3):
FROM INSULATOR TO ELECTRIDE
Branko Matovic
Institute for nuclear sciences Vinca, Belgrade University, Serbia

Room-temperature stable Electride [Ca24Al28O64]4+ (e-)4 was obtained from insulator


powder with composition corresponding to mineral Mayenite (12CaO7Al2O3) by heating in
reducing atmosphere. Starting Mayenite was synthesized by self-propagating combustion
method at 1100 C in an ambient atmosphere. The chemical formula of the unit cell
Mayenite compound can be expressed by [Ca24Al28O64]4+ (O2-)2. The free oxygen ions (O2-)
can be removed via appropriate reduction treatments. In this work, the sample powder was
set in a carbon crucible and was heated at 900 C in a flowing N2 atmosphere. The thermal
treatment caused the color change from white to dark green. The reduction process was
replaced free O2- ions with electrons converting insulating phase (12CaO7Al2O3) into
conductor. The powder X-ray diffraction confirmed that the both insulating and conductor
mayenite phase are the same indicating that the reduction treatment does not change the
crystal structure. The obtained powders were characterized by Scanning electron
microscopy (SEM), Raman spectroscopy at room temperature, Electron paramagnetic
resonance (EPR) at 196 C and NMR spectra using the "magic angle spinning" (MAS)
technique at 196 C.

40
COMPOZITE CERAMICE UOARE PE BAZ DE CENUI DE
TERMOCENTRAL ROMNETI OBINUTE N CMP DE MICROUNDE
POROUS CERAMIC COMPOSITES FROM ROMANIAN COAL-FIRING
POWER STATIONS WASTE BY USING MICROWAVES FIELD
TECHNIQUE
Enik Volceanov1, Carmen Plapcianu2, Marco Truccato3,
Simona Badea4, Adrian Volceanov5
1Universitatea Politehnica Bucureti, Centrul pentru tiina Suprafeei i Nanotehnologie,
Romnia
2Universitatea Politehnica Bucureti, Facultatea de Chimie Aplicat i tiina Materialelor,

Romnia
3Universitatea din Torino, Departamentul de Fizic, Italia
4Institutul pentru Fizica Materialelor, Departamentul de Magnetism i Supraconductibilitate,

Bucureti Mgurele, Romnia


5 Centrul de Cercetare tiinific pentru Aprare CBRN i Ecologie, Bucureti, Romnia

Cenua de termocentral rezultat la arderea crbunilor reprezint una dintre cele mai
importante deeuri care sunt produse n lume, inclusiv n Romnia, iar valorificarea
acesteia din haldele istorice sau a celei generate curent a devenit o real provocare pentru
cercettori. Generarea masiv de cenu la arderea crbunilor din centralele termice
implic probleme de mediu i economice, n msura n care depozitarea acestor deeuri a
devenit recent mai strict din cauza reglementrilor de mediu, precum i a costurilor
ridicate legate de depozitarea deeurilor. Proprietile fizice i chimice ale cenuii depind n
mod evident de tipul de crbune utilizat i de condiiile de ardere. Cenuile de
termocentral conin oxizi valoroi, cum ar fi: SiO2, Al2O3, CaO, Fe2O3 i ali oxizi; avnd
compoziia, densitatea, textura, porozitatea i capacitatea de absorbie a apei variabile. n
acelai timp, cenuile au granulaia foarte fin, astfel nct acestea pot fi utilizate direct n
producia de ceramici uoare, fr nici un tratament mecanic. Scopul acestei cercetri este
de a examina posibilitatea dezvoltrii unui nou mod de utilizare a deeurilor abundente de
cenu de la arderea crbunilor obinerea unor compozite ceramice prin tratament termic
rapid. Au fost investigate tipuri de cenui provenite de la dou termocentrale din Romnia:
1) o cenu de clasa F din arderea crbunelui bituminos i respectiv o cenu de clasa C
din arderea lignitului, care n prezena unui adaos de bentonit au fost sinterizate la 950-
1200 oC n cmp de microunde la intervale variabile de timp cuprinse ntre 5 30 minute.
Au fost determinate proprietile ceramice i caracteristicile morfologico-structurale ale
cenuilor de termocentral dup tratamentul termic n cmp de microunde, iar acestea par
a fi promitoare in condiiile aplicrii unei arderi rapide in microunde la 1000 oC timp de 20
minute pentru cenua zburtoare de clasa C, respectiv de la 1050 oC timp de 30 minute
pentru cenua (bottom ash) de clasa F. Au fost nregistrate date in timp real prin
microscopie de temperatur nalt - cnd probele au fost tratate intr-un cuptor electric
convenional - i s-a pus n eviden faptul c cenua de tip C se nmoaie mai uor dect
cea de tip C. Proprietile chimice ale probelor de cenu din arderea crbunilor relev
caracteristici adecvate, fiind comparabile cu cele ale materiilor prime ceramice utilizate n
mod obinuit n industria ceramic.
41
Concluzii: Rezultatele arat c pot fi dezvoltate ceramici uoare din ambele cenui de
termocentral investigate i prin condiii adecvate de tratament termic in cmp de
microunde la frecvena de 2.45 GHz, cu proprieti ceramice ce le recomand ca agregate
uoare spre exemplu, pentru aplicaii n sectorul de construcii. Pe termen mediu, utilizarea
agregatelor uoare n industria construciilor este de ateptat s creasc lund n
considerare avantajele tehnice i economice: materii prime cu costuri reduse, procesarea
rapid i protecia mediului.

Coal fly ash is one of the major wastes which are produced in the world, including
Romania. The massive production of coal fly ash from thermal power plants involve
environmental and economical problems as far as storage of this waste has recently
become more stringent because of increasing laws regulations and the high costs of
landfill. The physical and chemical properties of fly ash depend obviously on the type of
coal used and the combustion conditions. Fly ash contains valuable oxides such as SiO2,
Al2O3, CaO, Fe2O3, and other oxides which vary as composition, density, texture, porosity
and water absorption capacity.
At the same time, fly ash has a very fine size so it can be directly used in the production of
lightweight ceramics, without any mechanical treatment. In the medium term perspective
the use of lightweight aggregates in construction industry will increase taking into account
the technical and economical advantages: raw material low cost and the environment
protection.
The aim of this research is to examine the possibility to develop a new way to utilize the
abundant waste fly ash by providing preliminary information of converting it into ceramic
composites. Two series of kaolin- fly ash ceramics cured at 950-1200oC in microwave field
were developed by using coal fly ash from the combustion of bituminous coal and lignite in
two thermal power plants in Romania. Thermomechanical properties as well as the
morphological feature of the ceramic samples developed from clay and fly ash in different
amounts give an optimistic forecast in incorporating a waste material in the ceramic
samples followed by fast thermal curing.

Conclusions
1. Chemical properties of fly ash samples reveal adequate characteristics in comparison
with those of the ceramic raw materials usually used in the ceramic industry.
2. Mechanical strengths of samples increase with the growing of fly ash in the batch. The
best mechanical properties were obtained with the % 20-30% fly ash additions.
3. Density of sample decrease with the increasing of fly ash in the batch, up to 1.95 g/cm3
for 50% fly ash addition.
4. The results show that lightweight ceramics can be developed from clay and fly ash
mixtures and provide the best conditions to obtain porous products with desirable
properties suitable for construction sector.

42
STUDY OF CERAMIC SUBSTRATES FROM FLY ASHES,
COATED WITH TIO2 SLURRY FOR ENVIRONMENTAL APPLICATION
Eleni Katsika1, Angeliki Moutsatsou1, Vayos Karayannis2, Maria Volioti1,
Dimitrios Tsoukleris3
1Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering,
National Technical University of Athens (NTUA), Zografou Campus, Athens, Greece
2 Department of Environmental Engineering, echnological Education Institute of Western

Macedonia, Kozani, Greece


3 Laboratory of General Chemistry, School of Chemical Engineering, National Technical

University of Athens (NTUA), Zografou Campus, Athens, Greece

Several industrial solid wastes containing SiO2, Al2O3 and CaO as the predominant oxides
have already been used in construction applications, such as ceramics, glass-ceramics
and cement-based materials including geopolymers. Actually, the valorization of fly ashes,
slags etc. in the elaboration of value-added materials represents a challenge with important
environmental, technological and economic aspects.
This study aims at the utilization of calcareous and siliceous lignite ashes, the by-products
of lignite combustion in power plants, towards the development of new materials with
environmental benefits, by investigating the possibility to modify ceramic substrates made
of lignite fly ashes (calcareous or siliceous) with i2 (anatase and rutile), a photocatalytic
material. The chemical, mineralogical and morphological characteristics of lignite ashes
promote their application in the field of ceramics production for their further use as
substrates of heterogeneous photocatalysts.
For that purpose, a series of disc-shaped specimens were formed by cold pressing of fly
ash samples (calcareous or siliceous). Compaction pressure was optimized to achieve
sufficient density and strength of the compacts for their subsequent treatment. All
specimens were sintered at 1000oC for 2 hours in air in a controlled laboratory chamber
furnace and finally gradually cooled to ambient temperature in the furnace. Then the
specimen surfaces were coated with TiO2 slurry and studied for drying and sintering
conditions. The obtained microstructures were thoroughly examined by XRD and SEM-
EDAX.
Main advantage of this process is that the immobilization of titania onto a cheap porous
substrate can provide an additional solution to the photocatalytic treatment of liquid wastes.
The experiments ended up to encouraging results using both visible and the UV irradiation
during photocatalysis, due to a synergistic effect between lignite fly ashes and i2. It
must, also, be mentioned that the substrates maintain their ability in heavy metals retention
from wastewaters, as further tests verified.

43
PIGMENI TERMOREFLEXIVI PE BAZ DE Zn1-XCoXAl2O4 OBINUT
PRIN METODA COMBUSTIEI

THERMOREFLECTIVE BLUE PIGMENTS BASED ON COMBUSTION


SYNTHESIZED Zn1-XCoXAl2O4
Robert Iano1, Eliza Muntean1, Cornelia Pcurariu1, Radu Lazu1*, Cornelia Bandas2

1Universitatea Politehnica Timioara, Facultatea de Chimie Industrial i


Ingineria Mediului, Timioara, Romnia
2 Institutul Naional de Cercetare-Dezvoltare pentru Electrochimie i Materie Condensat,

Departamentul de Materie Condensat, Timioara, Romnia

Temperatura acoperiurilor i faadelor cldirilor crete n timpul verii din cauza absorbiei
radiaiilor din domeniul infra-rou apropiat (NIR), ceea ce conduce la creterea
semnificativ a consumului de energie necesar pentru funcionarea aerului condiionat.
Una dintre abordrile curente pentru reducerea temperaturii suprafeelor se bazeaz pe
utilizarea pigmenilor cu reflexie n infra-rou, care absorb selectiv radiaia din domeniul
vizibil genernd culoarea dorit i n acelai timp reflect radiaia din zona NIR a spectrului
solar responsabil cu supranclzirea zonelor urbane.

n cadrul lucrrii au fost obinui prin metoda combustiei pigmeni albatri pe baz de
Zn1-xCoxAl2O4 (x = 0 0.3) avnd reflexie ridicat n infra-rou apropiat. S-a pornit de la
soluii apoase de azotai metalici, uree i glicin. Aceste soluii au fost nclzite la
450 C, ceea ce a condus la iniierea unor reacii autopropagate, puternic exoterme de
combustie. Temperatura maxim generat n timpul unui astfel de proces a depit 1400
C n cazul de fa.

Pulberile obinute const n Zn1-xCoxAl2O4 nanocristalin, fr a mai fi necesar o etap


suplimentar de tratament termic. Soluiile solide rezultate au avut dimensiuni medii ale
cristalitelor de 23-32 nm. Suprafaa specific a variat ntre 6 i 8 m2/g.
Odat cu creterea coninutului de cobalt nuana albastr a pigmenilor obinui (valoarea
parametrului b*) s-a intensificat de la -39 (pentru x = 0,1) pn la -49 (pentru x = 0,3), n
timp ce reflectana solar total a sczut de la 58 % (pentru x = 0,1) la 48 % (pentru x =
0,3).

n comparaie cu alte abordri, sinteza prin metoda combustiei este foarte rapid i
eficient energetic, permind obinerea rapid a pigmenilor albatri pe baz de
Zn1-xCoxAl2O4 cu bune proprieti termoreflexive.

44
During summer the roof and facade temperature of the buildings increases because of
near infrared (NIR) radiation absorption, causing a significant increase in the electricity
needed for air conditioning. One approach for decreasing the surface temperature relies on
using NIR reflective pigments, which selectively absorb radiation in the visible range
generating the desired colour, and at the same time reflect the NIR radiation responsible
for overheating.

Zn1-xCoxAl2O4 (x = 0 0.3) NIR-reflective blue pigments were prepared via combustion


synthesis, starting from aqueous solutions of metal nitrates, urea and glycine. The aqueous
solutions were heated at 450 C, triggering the ignition of fast and exothermic self-
propagating combustion reactions. The maximum temperature measured by infrared
thermal imaging during the process exceeded1400 C.

The obtained powders consisted of nanocrystalline Zn1-xCoxAl2O4 and no additional


annealing was required. The resulted solid solutions had average crystallite size of 23-32
nm. The specific surface areas ranged between 6 and 8 m2/g. As the amount of cobalt
increased, the blue shade (b* value) intensified from -39 (x = 0.1) to -49 (x = 0.3), whilst the
total solar reflectance decreased from 58 % (x = 0.1) to 48 % (x = 0.3).

Compared to other approaches, combustion synthesis is time-effective and energy-


efficient, allowing the fast preparation of blueZn1-xCoxAl2O4 pigments with good NIR
reflective properties.

45
STUDIU COMPARATIV ASUPRA STRUCTURII I PROPRIETI
FOTOCATALITICE A NANOPARTICULELOR DE TIO2 OBINUTE PRIN
METODA HIDROTERMAL ASISTATA DE MICROUNDE I POLIOL
COMPARISON STUDY OF STRUCTURES AND PHOTOCATALYTIC
ACTIVITY OF TIO2 NANOPARTICLES PREPARED VIA MICROWAVE
ASSISTED HYDROTHERMAL AND POLYOL METHODS
Alberto Ion1, Rzvan State2, Adrian Volceanov1
1 Universitatea Politehnica din Bucureti, Departament tiina i Ingineria
Materialelor Oxidice i Nanomateriale, Romnia
2 Institutul de Chimie Fizic Ilie Murgulescu al Academiei Romne, Bucureti, Romnia

n ultimul deceniu interesul pentru materialele fotocatalitice a crescut exponenial. Cele mai
multe nanomateriale testate, precum fotocatalizatori, au fost cele bazate pe dioxid de titan
(TiO2), oxid de zinc (ZnO), alumina Al2O3. Datorit activitii fotocatalitice ridicate, a
stabilitii chimice i a netoxicitii, unul dintre cele mai studiate materiale n fotocataliz
este TiO2.

Scopul acestei lucrri este corelarea sintez structur proprieti fotocalitice a


nanoparticulelor de TiO2 obinute prin 2 metode - hidrotermal asistat de microunde i
metoda poliol. Pulberile astfel obinute au fost analizate prin diferite metode de
caracterizare i anume analiza termic diferenial i termogravimetrie (TGA/TG), difracie
de raze X (XRD), granulometrie laser, microscopie electronic de baleiaj i microscopie
electronic de transmisie (SEM/TEM) i determinarea suprafeei specifice (BET).

(a) (b)
Figura 1. Imagini SEM ale pulberilor obinute prin (a) metoda poliol i (b) metoda sol-gel

Pentru a se observa eficiena materialelor obinute n degradarea unor compui toxici au


fost efectuate teste fotocatalitice n care a fost folosit un simulator solar pentru a se
reproduce ct mai real condiiile de mediu.

46
In the last decade the interest for photocatalytic materials has increased exponentially. The
most tested nanomaterials, such as photocatalysts, were based on titanium dioxide (TiO2),
zinc oxide (ZnO) or alumina (Al2O3). Due to high photocatalytic activity, chemical stability
and non-toxicity the research has been extensively focused on TiO2 as most promising
material for photocatalysis.

The aim of present work is concerned to correlate syntesis, structure, and photocatalytic
properties of TiO2 nanoparticles prepared by two methods, namely: microwave assisted
hydrothermal and polyol method. The powders obtained by these methods were analysed
through several characterization techniques such as complex thermal analysis (DTA), X-
ray diffraction (XRD), laser granulometry, scanning and transmission electron microscopy
(SEM/TEM) and specific surface area determination (BET), as well.

In order to estimate the efficiency of the obtained materials for degradation of some toxic
compounds there were performed photocatalytic tests where a solar simulator was
involved in order to reproduce real environmental conditions.

47
PRECIPITAREA BACTERIAN A CARBONATULUI DE CALCIU
METOD ALTERNATIV DE TRATAMENT AL BETOANELOR
BACTERIAL CALCIUM CARBONATE PRECIPITATION AS AN
ALTERNATIVE CONCRETE TREATMENT
Victor Fruth1, Jeanina Pandele-Cusu1, Irina Atkinson1, Luminia Predoan1, Adriana Rusu1,
Iuliana Raut2, Mihaela Doni2, Luiza Jecu2, D. Vasilescu3, Alina Bdnoiu3
1 Institutul de Chimie Fizic Ilie Murgulescu al Academiei Romne, Bucureti, Romnia
2 Institutul Naional pentru Cercetare-Dezvoltare pentru Chimie i Petrochimie ICECHIM,
Bucureti, Romnia
3 Universitatea Politehnica din Bucureti, Romnia

Multe microorganisme bacteriene dezvolt activiti metabolice cu producerea enzimei


ureaz ceea ce conduce la precipitarea carbonatului de calciu. Producerea formelor
polimorfe ale carbonatului de calciu cristalin depinde de mediile de cultur i tipul tulpinii
bacteriene. Aceast proprietate are multe aplicaii n consolidarea nisipurilor, remedierea
structurilor deteriorate, ca pietre ornamentale i umplerea fisurilor i golurilor [1, 2]. Stratul
de carbonat produs pe suprafaa materialului reprezint o abordare inovatoare pentru
mbuntirea durabilitii betonului la aciunea apei i a altor ageni distructivi, prin
scderea porozittii materialului. Ureaza microbian catalizeaz hidroliza ureei i produce
CO2 i NH3. Creterea valorilor pH i suprasaturaia n CO2 n prezena ionilor Ca+2
determin depunerea ulterioar de carbonat de calciu. Precipitarea depinde de tipul de
microorganism, concentraia de carbon anorganic dizolvat, valorile pH, concentraia ionilor
de calciu i prezena centrelor de cristalizare. De asemenea, sunt implicate condiiile de
mediu [3].

Prezentul studiu investigheaz potenialul a dou tulpini bacteriene comune ce urmeaz s


fie utilizate pentru producia biologic de minerale pe baz de carbonat de calciu. Tulpinile
au fost crescute n mediu coninnd uree solid i lichid i ioni de Ca+2. Capacitatea
microorganismului de a induce precipitarea CaCO3 a fost evideniat cu testul de culoare
cu alizarin. Spectroscopia n infrarou (FTIR), difracia de raze X (XRD) i microscopia
electronic de baleiaj (SEM) au fost utilizate pentru a confirma prezena carbonatului de
calciu din precipitat. Datele experimentale prezint rezultate promitoare i studii
suplimentare vor fi efectuate pentru a pune n aplicare, pe o scar mai mare, acest
tratament biologic eco-friendly.

Many bacterial microorganisms are developing metabolic activities with the production of
urease enzyme which leads to the precipitation of calcium carbonate. The production of the
crystal polymorphs of calcium carbonate depends on growing environments and bacterial
strains. This property has many applications in sand consolidation, remediation of
damaged structured, as ornamental stones and filling of cracks and holes [1, 2]. The
carbonate layer produced on material surface represents an innovative approach for a
concrete with improved durability as water and other destructive agents protection by
decreasing the material porosity. Microbial urease catalyzes the hydrolysis of urea and
produces carbonate and ammonium. The increase of pH values and supersaturation of
48
carbonate in the presence of Ca+2 ions promote subsequently the deposition of calcium
carbonate. The precipitation depends on type of microorganism, concentration of dissolved
inorganic carbon, pH values, concentration of calcium ions and presence of nucleation
sites. Also, environmental conditions are involved [3].
The present study investigates the potential of two bacterial common strains to be used for
the biological production of calcium carbonate based minerals. The strains were grown in
solid and liquid medium containing urea and Ca+2 ions. The microorganism ability of
inducing CaCO3 precipitation was evidenced with alizarin coloration test. Fourier transform
infrared (FTIR) spectroscopy, X-ray diffraction (XRD) analyses, and scanning electron
microscopy (SEM) were performed in order to confirm the presence of calcium carbonate
in the precipitate. One isolate presents promising results and further studies will be
performed to implement on a larger scale this eco-friendly biological treatment.

Acknowledgments. The researches were financially supported by project PN-II-PT-PCCA-2013-4-


1709/085/2014 (BIO-THERM).

References
[1] Vahabi A., Ramezanianpour A. A., Sharafi H., Zahiri H. S., Vali H., Noghabi K. A. 2015, Calcium
carbonate precipitation by strain Bacillus licheniformis AK01, newly isolated from loamy soil: a promising
alternative for sealing cement-based materials, Journal of Basic Microbiology, 55, 105111.
[2] Rodriguez-Navarro C., Jroundi F., Schiro M., Ruiz-Agudo E., Gonzlez-Muoz M. T., 2012, Influence of
substrate mineralogy on bacterial mineralization of calcium carbonate: Implications for stone conservation.
Applied and Environmental Microbiology. 78, 4017-4029.
[3] De Muynck W., Verbekenc K., De Beliea N., Verstraeteb W., 2010, Influence of urea and calcium dosage
on the effectiveness of bacterially induced carbonate precipitation on limestone, Ecological Engineering, 36,
99111.

49
EVALUAREA CALITII DE IZOLARE TERMIC A PRODUSELOR DIN
VAT MINERAL PRIN METODA CONDUCTIVITII TERMICE
THERMAL INSULATION QUALITY ASSESSMENT OF MINERAL WOOL
PRODUCTS BY THERMAL CONDUCTIVITY METHOD
Marinela Ghi
Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii-ICECON S.A,
Romnia

Produsele din vat mineral se utilizeaz n principal pentru realizarea izolaiei termice la
exteriorul ct i la interiorul cldirilor pentru meninerea unei temperaturi interioare
acceptabile prin nclzire sau rcire.
n lucrare se vor prezenta metodele de determinare a performanelor de rezisten termic
pentru produsele de vat de sticl i rezultatele obinute n urma ncercrilor utiliznd
echipamentul HESTO-LAMBDA-CONTROL A90 conform standardului SR EN 12667
Performana termic a materialelor i produselor de construcie. Determinarea rezistenei
termice prin metoda cu termofluxmetru. Produse cu rezisten termic mare i medie.

Metodele de ncercare i nivelurile de performan pentru produsele din vat mineral sunt
impuse prin respectarea standardului de produs SR EN 13162 Produse termoizolante
pentru cldiri. Produse fabricate din vat mineral (MW). Specificaie.
Evaluarea performanelor termice ale saltelelor de vat mineral se realizeaz prin
determinarea rezistenei termice i a conductivitii termice pe epruvete extrase din rulouri,
saletele sau plci de vat mineral care se pregtesc n prealabil pentru aceasta
operaiune deoarece structura pufoas poate fi afectat prin manipulare sau transport
conducnd la rezultate eronate.

Mineral wool products are mainly used for the internal and external thermal insulation of
buildings, in order to maintain an acceptable inside temperature by heating or cooling.
The paper presents the methods for determining the thermal resistance performances of
glass wool products and the results of the tests obtained using the HESTO-LAMBDA-
CONTROL A90 equipment, according to SR EN 12667 Thermal performance of building
materials and products. Determination of thermal resistance by means of heat flow meter
method. Products of high and medium thermal resistance.

The testing methods and the performance levels for the mineral wool products are imposed
by the product standard SR EN 13162 Thermal insulation products for buildings - Factory
made mineral wool (MW) products - Specification.
The thermal performance assessment of the mineral wool mattress is performed by
determining the thermal resistance and conductivity on specimens sampled from mineral
wool rolls, mattress or slabs that are prepared in advance for the tests due to their loose
structure that may be affected by handling or transport, causing incorrect results.

50
MATERIALE TERMOIZOLATOARE PE BAZ DE POLIPROPILEN I
MATERIALE SILICIOASE
THERMAL INSULATION MATERIALS BASED ON POLYPROPYLENE
AND SILICEOUS MATERIALS
Jenica Paceagiu1, Zina Vuluga2, Marina Martin1, Liliana Radu1, Michaela Iorga2, Valentin
Apostol3, Horatiu Pop3
1CEPROCIM S.A., Bucuresti, Romnia
2Institutul Naional pentru Cercetare-Dezvoltare pentru Chimie i Petrochimie ICECHIM,
Bucureti, Romnia
3 Universitatea Politehnica din Bucureti, Romnia

Scopul acestei lucrri este de a obine un nou material compozit destinat utilizrii ca
material termoizolant n construcii.
n prezenta lucrare s-au preparat materiale compozite pe baz polipropilen (PP) umplute
cu diferite materiale silicioase, utiliznd procedeul de extrudare i turnare prin injecie prin
prelucrare prin topire dinamic.
S-au evaluat efectele coninutului de umplutur asupra proprietilor termice, cum ar fi
rezistena termic, conductivitate termic i stabilitate termic (evaluat prin analiz
termogravimetric) i asupra rezistenei la traciune ale compozitelor. De asemenea,
morfologia compozitelor a fost evaluat prin microscopie electronic de baleiaj (SEM) i
spectroscopie cu dispersie a energiei razelor X (EDS).
Rezultatele au artat c materialul silicios a mbuntit stabilitatea termic a materialelor
compozite pe baz de PP; efectul este destul de diferit n funcie de tipul sursei de material
silicios. De asemenea s-a observat un uor efect pozitiv asupra rezistenei la traciune.
Mulumiri: Acest studiu este realizat cu sprijinul Ministerului Educaie Naionale i Cercetrii
tiinifice-UEFISCDI, in cadrul proiectului PN-II-PT-PCCA-2013-4-1709 (BIO-THERM-contract
85/2014).

The aim of this study is to obtain a new material composite intended to use as thermal
insulation material in building constructions.
In the present work polypropylene (PP) based composites filled with different siliceous
materials were prepared using the extrusion compounding and injection molding by
dynamical melt processing.
The effects of filler content on the thermal properties such as thermal resistance, thermal
conductivity and thermal stability (evaluated by thermogravimetry analysis) and on the
tensile strength of the composites were evaluated. Also, the morphology of the composites
was evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray
spectroscopy (EDS).
The results showed that the siliceous material improved the thermal stability of composites
based on PP; the effect is quite different depending on type of siliceous source. A slight
positive effect was noticed on the tensile strength, too.
Acknowledgements: This material is based upon work supported by the Ministry of National
Education and Research Activity- UEFISCDI, in the frame of the project number PN-II-PT-PCCA-
2013-4-1709 (BIO-THERM, grant no 85/2014).

51
CARACTERISTICILE MORTARELOR COMPOZITE TERMOIZOLANTE
CHARACTERISTICS OF THERMAL INSULATION COMPOSITE MORTARS
Virgil Marinescu1,4, Georgeta Velciu1, Gabriela Sbrcea1, Adriana Moan2,
Mirela Menicu2, Constantin Dorinel Voinichi3, Gheorghe Ghe. Ioni4
1Institutul Naional de Cercetare-Dezvoltare pentru Inginerie Electric ICPE-CA,
Bucureti, Romnia
2 CEPROCIM SA, Bucureti, Romnia
3 Universitatea Tehnic de Construcii Bucureti, Romnia
4Universitatea Valahia din Trgovite, Romnia

Utilizarea materialelor compozite cu diverse adaosuri i filere sunt frecvent utilizate n


domeniul construciilor, prezentnd o serie de avantaje fa de materialele
standardizate. Microsferele ceramice si microsferele de cenu de termocentral sunt
utilizate n mortare n vederea mbuntirii proprietilor termoizolante.

Au fost investigate compoziii de mortar n a cror reete s-a utilizat microsfere de


cenu de termocentral n proporii variind ntre 10 i 30%. Microsferele utilizate, a
cror distribuie granulometric a fost sub 32m, au fost obinute prin clasarea cenuii
brute. Analizele structurale realizate prin difracie de raze X, efectuate pe probele de
mortar, evideniaz formarea hidrosilicailor i prezena fazelor cristaline. Caracterizarea
microstructural (SEM) a probelor de mortar la termenul de 28 zile au artat o distribuie
relativ uniform a microsferelor din cenua de termocentral n masa mortarului. De
asemenea, se evideniaz prezena ca faze hidratate a hidrosilicailor de calciu gelici,
slab structurai cu forme neregulate sau bine cristalizai.
Caracteristicile structurale i microstructurale influeneaz proprietile mecanice i
termice ale mortarelor.

Using of composites materials with different fillers and additives are frequently used in
building materials domain, with a lot of advantages from standard materials. Ceramic
microspheres and fly ash microspheres from coal plants are used like filler in mortars for
improve thermo-insulation properties.

We investigate mortars compositions and their recipes who implicated ash coal plant
microspheres in proportion of 10 and 30% filler. A used microsphere, with granulometric
distribution was under 32 m, was obtained by ranking of raw fly ash. Structural
analysis done by X-Ray diffraction, on the mortars highlights hydro-silicates forming and
crystalline phases presence. Micro-structural investigations done by SEM of mortars
samples after 28 days showed a uniform relative distribution of ash fly microspheres
additives in the whole mortars mass. Also it is shown the presence of hydrated phases
of gel hydro-silicates, weak structured with irregular shapes but also the presence of the
same compound very well crystallized.

Acknowledgments: This research was carried out with financial support of the National Research
Program Partnerships in priority areas PN II, MEN UEFISCDI, grant no. PN-II-PT-PCCA-2013-4-0945

52
MATERIALE NECONVENIONALE PE BAZ DE FIBRE VEGETALE
UTILIZATE N CONSTRUCII
UNCONVENTIONAL MATERIALS BASED ON VEGETABLES FIBRES USE
IN CONSTRUCTIONS
Cristina Dima1, Adrian abrea2
1 Universitatea Politehnica din Bucureti, Institutul de Cercetri pentru Echipamente i
Tehnologii n Construcii ICECON S.A., Bucureti, Romnia
2 Institutul de Cercetri pentru Echipamente i Tehnologii n Construcii ICECON S.A.,

Bucureti, Romnia

Folosirea n construcii a fibrelor vegetale provenite din surse naturale (stuf, papur) sau
deeuri agricole (paie, tulpini de floarea soarelui) a nceput cu multe secole n urm.
Datorit cerinelor privind mediul nconjurtor, utilizarea fibrelor vegetale ca material
neconvenional de izolare termic i acustic a fcut subiectul multor studii n ultimele
decenii.

Prezenta lucrare s-a axat pe studiul proprietilor termice i mecanice ale unor panouri
termoizolante realizate termoizolante realizate din tulpini de stuf uscat, precum i
modalitile de punere n oper a acestor produse. Valorile obinute pentru conductivitatea
termic ( = 0,060 W/mK) i indicele de izolare la zgomot aerian (14-18 dB) demonstreaz
faptul c materialele pe baz de fibre vegetale (stuf) pot fi folosite ca material de izolare
termic i fonic n domeniul construciilor.

The use of vegetable fibers from natural sources (reed, rushes) or agricultural waste
(straw, sun flower haulms) in construction has a long history. In the last decades, the
vegetable fibers thermal and sound insulation properties were extended studied due to the
environmental impact requirements.

The paper presents the studies performed in order to determine the mechanical and
thermal properties for thermal insulation panels based dried reddstalks, as well as the
manufacturing and installation process. The values obtained for the thermal conductivity
( = 0,060 W/mK) and the index noise transmission (14-18 dB) demonstrates that
vegetable fibers based materials (reeds) can be used as thermal and sound insulation
material in construction.

53
CARACTERIZAREA FIZICO-MECANIC A UNOR MATERIALE
COMPOZITE FONOABSORBANTE CU DIVERSE DEEURI
PHYSICO-MECANICAL CHARACTERIZATION OF SOME SOUND-
ABSORBING COMPOSITE MATERIALS WITH VARIOUS WASTES

Mihai Bratu1, Ovidiu Dumitrescu2, Ovidiu Vasile3,


Ileana Nicolescu1, Luoana Florentina Pascu1

Naional de Cercetare & Dezvoltare Ecologie Industrial ECOIND,


1 Institutul

Bucureti, Romnia
2 Universitatea Politehnic din Bucureti, Facultatea de Chimie Aplicat i tiina

Materialelor, Dep. tiina Materialelor Oxidice & Inginerie i Nanomateriale, Bucureti,


Romnia
3Universitatea Politehnica din Bucureti, Departamentul de Mecanic, Bucureti, Romnia

Poluarea, sub toate aspectele ei actuale, reprezint o preocupare permanent i actual a


cercettorilor. De aceea, realizarea de materiale fono-absorbante care s nglobeze
deeuri este o abordare foarte util.
Lucrarea prezint cercetri privind obinerea unor materiale compozite cu matrice oxidic
ce conin ca material de armare diverse deeuri care pot afecta mediul nconjurtor.
Este descris procedeul de obinere i compoziiile efective ale acestor materiale.

Au fost msurate o serie de proprieti fizico-mecanice pentru caracterizarea acestor


materiale compozite: distribuie granulometric, rezisten mecanic la compresiune,
rezisten mecanic la ncovoiere precum i capacitatea de absorbie a undelor sonore.
Pe baza analizelor microstructurale (SEM si EDAX) se prezint corelaiile structur
proprieti ale acestor materiale compozite cu diverse deeuri.

Pollution, in all its current views, its a permanent concern of the researchers. Therefore,
achieving phono-absorbent materials that encompass waste is a very useful approach.
The paper presents the researches on obtaining of some oxide matrix composites
containing as reinforcing material, various wastes that may affect the environment.

It is described the process for preparing these kind of materials and their effective
compositions. In order to characterise these composite materials a number of physico-
mechanical properties were measured: particle size distribution, compressive strength,
flexural strength and their sound absorbing ability.

The correlations between the structure and the properties of such of composites materials
containing various wastes, are based on microstructural analyses (SEM and EDAX).

54
INDUSTRIA CIMENTULUI I BETONULUI PARTE INTEGRANT A
ECONOMIEI CIRCULARE
CEMENT AND CONCRETE INDUSTRY INTEGRANT PART OF
CIRCULAR ECONOMY
Mihai Rohan
Patronatul din Industria Cimentului i altor produse minerale penrtru construcii din
Romnia -CIROM, Romnia

Conceptul Economiei Circulare este unul foarte simplu: un principiu de baz al fizicii i
chimiei clasice nimic nu se pierde, totul se transform este aplicat economiei actuale n
care resursele naturale sunt din ce n ce mai limitate i se transpune n deeurile trebuie
s devin o resurs, iar coninutul lor material i energetic s fie recuperat i s intre
ntr-un nou ciclu economic, reprezentnd un aport de materii prime alternative i
combustibili alternativi.
n Romania exist mai multe industrii care deja aplic acest concept al economiei circulare.
De exemplu, industria cimentului/betonului care transform deeurile n resurse alternative
de materii prime i energie i valorific deja cantiti semnificative de deeuri provenind din
alte industrii precum i deeuri menajere sortate.
Co-procesarea deeurilor n industria cimentului este o metod de valorificare a deeurilor,
recunoscut drept una dintre cele mai bune practici de eficientizare a utilizrii resurselor.
Prin co-procesare are loc simultan att reciclarea coninutului mineral al deeurilor, ct
recuperarea energiei acestora, ceea ce conduce la reducerea emisiilor indirecte de CO2.
De asemenea, produsul de larg consum al acestei industrii - betonul din ciment - poate fi
reciclat 100% drept agregate alternative utilizate la construirea infrastructurii de transport
sau pentru obinerea unui nou beton.
Astfel industria cimentului/betonului contribuie la conservarea resurselor naturale prin
nlocuirea lor cu resurse alternative provenite din deeuri i devine parte integrant a
economiei circulare - deziderat european pentru eficientizarea utilizrii resurselor i
asigurarea securitii energetice.

The Circular Economy concept is a very simple one: a basic principle of classic physics
and chemistry "nothing is lost, everything is transformed" is also applied to the current
economy, where natural resources are becoming increasingly limited, and it is translated
into "waste must become a resource" , and their material and energetic content to be
recovered and to enter into a new economic cycle, representing a contribution of
alternative raw materials and alternative fuels.
In Romania, there are several industries that already apply the concept of circular
economy. For example, cement/concrete industry that turns waste into alternative sources
of raw materials and energy and already recovers significant amounts of waste from other
industries as well as sorted household waste.

55
Waste co-processing in cement industry is a waste recovery method, recognized as being
one of the best practices for an efficient use of resources. By co-processing take place
simultaneously, both the recycling of waste mineral content as well as their energy
recovery, which leads to the reduction of indirect CO2 emissions.
Also, the product of wide consume of this industry cement concrete can be 100%
recycled as alternative aggregates used in building the transport infrastructure or getting a
new concrete.
Thus, the cement/concrete industry contributes to the conservation of natural resources by
replacing them with alternative resources from waste, and becomes an integrant part of the
circular economy - European goal for an efficient use of resources and ensuring energy
security.

56
GB CHEMISTRY OF SILICON NITRIDE BASED CERAMICS
IMPLICATIONS TO THE CERAMICS PROPERTIES
Pavol Sajgalik
Slovak Academy of Sciences, Bratislava, Slovakia

Six different sintering aids (Lu2O3, Yb2O3, Y2O3, Sm2O3, Nd2O3 and La2O3) were used for
the processing of dense Si3N4/SiC micro/nano composites. Formation of SiC nano
inclusions was achieved by in situ carbothermal reduction of SiO2 by C during the sintering
process. Room temperature fracture toughness, hardness and strength showed increasing
tendency when the used rare-earth element in the oxide additive changes from a large to
a small rare-earth cation (i.e. from La3+ to Lu3+). Besides the highest hardness and
reasonably high fracture toughness and strength of composite material with Lu2O3 sintering
additive. The first principle calculations were used for the explanation of the fracture
behaviour of the composites depending on the rare earth additive. The energy of fracture
was calculated with respect to the chemical composition of GB. The experimental and
theoretical results will be discussed.
Besides mechanical properties composites the thermal shock resistance, wear resistance
and oxidation resistance are discussed.
Thermal shock resistance: A critical temperature difference increased with an increasing
ionic radius of RE3+ for both the composites and the monoliths.
Wear behavior: The friction coefficient as well as the specific wear rate decreased with a
decreasing ionic radius of rare-earth elements in both the monoliths and the composites.
High bonding strength and the high fracture toughness are the reasons why the ceramics
doped by Lu exhibited the best wear resistance.
Oxidation resistance: Composites exhibited predominately parabolic oxidation behaviour
indicated diffusion as the rate limiting mechanism. Exception was only the Si3N4-SiC
composite sintered with Lu2O3. In this case diffusion of cation has been strongly
suppressed because of the beneficial effect of stable grain boundary phase and the
presence of the SiC particles predominately located at the grain boundaries of Si3N4.

57
METODE COMBINATE DE MBUNTIREA PROPRIETILOR FIZICE I
CHIMICE ALE PRODUSELOR INDUSTRIALE DIN STICL
COMBINED METHODS, USED TO IMPROVE PHYSICAL AND
CHEMICAL PROPERTIES OF INDUSTRIAL GLASSWARE
Vasile aragov
Universitatea de Stat Alecu Russo din Bli, Republica Moldova

Se analizeaz i generalizeaz rezultatele cercetrilor complexe pentru determinarea


stabilitii chimice, rezistenei mecanice, microduritii i stabilitii termice a produselor
industriale din sticl, tratate cu reageni dediferit natur. Experimentele au fost efectuate
n condiii de producere la cteva Fabrici de Sticl.

Rezultate importante au fost obinute la combinarea tratrii termochimice (TTC) cu tratare


termomagnetic (TTM) al produselor industriale din sticl. Sunt posibile trei variante de
tratare combinat: 1) TTM al produselor din sticl, apoi TTC; 2) TTC al produselor din
sticl, apoi TTM; 3) tratarea concomitent a produselor din sticl cu gaze i cu cmpuri
electromagnetice.

Efectul maxim n sporirea proprietilor mecanice, stabilitii termice i chimice a sticlei de


ambalaj s-a obinut n timpul tratrii concomitente al produselor din sticl cu gaze active i
cmpuri electromagnetice.

n condiii de producere s-au aprobat diferite combinaii ale metodelor de mbuntire a


proprietilor de exploatare a produselor din sticla industrial, i anume: 1) TTC cu gaze,
apoi depunerea acoperirilor de protecie organice, silicoorganice i oxido-metalice; 2)
depunerea acoperirilor de protecie organice, silicoorganice i oxido-metalice, urmat de
TTC cu gaze; 3) TTC cu gaze, apoi schimb ionic cu reageni n faz solid; 4) schimb ionic
cu reageni n faz solid, urmat de TTC cu gaze; 5) TTM, apoi depunerea acoperirilor de
protecie organice, silicoorganice i oxido-metalice; 6) depunerea acoperirilor de protecie
organice, silicoorganice i oxido-metalice, urmat de TTM.

n unele experimente s-au utilizat trei metode de tratare a produselor din sticl: 1) TTC cu
gaze, depunerea acoperirilor de protecie organice, silicoorganice i oxido-metalice, urmat
de TTM; 2) TTC cu gaze, TTM i depunerea acoperirilor organice, silicoorganice i oxido-
metalice.

Efectul maxim la mbuntirea proprietilor de exploatare a produselor din sticl a fost


atins cu ajutorul combinrii celor trei metode de tratare. Ins, n acest caz considerabil se
complic deservirea liniilor tehnologice pentru fabricarea ambalajului din sticl.

58
The article offers an analysis and a generalization of the results of complex research
carried out to determine the chemical stability, mechanical strength, microhardness and
thermal stability of industrial glassware treated with reagents of different nature.
Experiments were carried out in manufacturing conditions at several glass factories.

Important results have been obtained by combining thermochemical treatment (TCT) with
acid gases and thermomagnetic treatment (TMT) of industrial glassware. There are three
possible variants of combined treatment: 1) TMT of glassware, then TCT; 2) TCT of
glassware, then TMT; 3) simultaneous treatment of glassware with acid gases and
electromagnetic fields.

The greatest effect in increasing the mechanical, thermal and chemical stability of glass
containers was obtained as a result of simultaneous treatment of glassware with acid
gases and electromagnetic fields.

Various combinations of methods to improve physical and chemical properties of the


industrial glassware were tested in manufacturing conditions, namely: 1) TCT with acid
gases, and then deposition of organic, organosilicon and metal oxide protective coatings;
2) deposition of organic, organosilicon and metal oxide protective coatings, followed by the
TCT with acid gases; 3) TCT with acid gases, and then ion-exchange with solid phase
reagents; 4) ion-exchange with solid phase reagents, followed by TCT with acid gases; 5)
TMT, then deposition of organic, organosilicon and metal oxide protective coatings; 6)
deposition of organic, organosilicon and metal oxide protective coatings, followed by TMT.
In some experiments, three methods of glassware treatment were used: 1) TCT with acid
gases, deposition of organic, organosilicon and metal oxide protective coatings, followed
by TMT; 2) TCT with acid gases, TMT and deposition of organic, organosilicon and metal
oxide protective coatings.

The maximum effect in improving the physical and chemical properties of the industrial
glassware has been achieved by combining the three methods of treatment. But in this
case, it considerably complicates the servicing of technological lines for glass container
manufacturing.

59
STICLE BORO-FOSFATICE DOPATE, SUB FORMA DE STICLE DE
VOLUM, PULBERI i STRATURI SUBIRI OBINERE, STRUCTUR I
PROPRIETI
DOPED BORO-PHOSPHATE GLASSES AS BULK, POWDERS AND
THIN LAYERS OBTAINING, STRUCTURE AND PROPERTIES
Bogdan Alexandru Sava1, Lucica Boroica1, Mihail Elisa2, Regina C.C. Monteiro3,
Olga Shikimaka4, Victor Kuncser5, Ionu Feraru2, Raluca Iordnescu2*,
Zinaida Barbos4, Mihaela Popa4, Mihaela Filipescu1, Gabriel Socol1
1Institutul Naional de Fizica Laserilor, Plasmei i Radiaiei, Mgurele-Bucureti, Romnia
2Institutul Naional de Cercetare i Dezvoltare pentru Optoelectronic, INOE 2000,
Mgurele-Bucureti, Romnia
3Universidade Nova de Lisboa, Departamentul de tiinta Materialelor, CENIMAT/I3N,

Facultatea de tiine i Tehnologie, Lisabona, Portugalia


4Institutul de Fizic Aplicat, Academia de tiinte a Moldovei, Chiinu, Republica Moldova
5Institutul Naional de Fizica Materialelor, Mgurele-Bucureti, Romnia

Au fost obinute materiale sub form de sticl de volum, pulberi i filme subtiri, prin
metodele sol-gel, magnetron sputtering - MS i depunere cu laser cu pulsaii PLD, din
sisteme boro-fosfatice co-dopate cu ioni de Bi-Pb si Dy-Tb. A fost investigat influena
precursorilor, pH-ului, temperaturii i timpului asupra procesului sol-gel, precum i a
parametrilor de proces ai MS i PLD asupra proprietilor filmelor.
Au fost analizate structura i proprietile probelor obinute utiliznd spectroscopia Raman,
FTIR i UV-Vis i analiza termic, precum i comportamentul mecanic la nano- i
microscar, prin aplicarea sarcinii concentrate [1]. Corelaia structur proprieti a fost
studiat utiliznd msuratori de XRD, XRF, SEM + EDS, EDAX i AFM. Proprietile
magneto-optice au fost analizate cu ajutorul unui dispozitiv Kerr modificat [2].
Spectrele Raman pentru sticla bloc permit identificarea vibraiilor simetrice i asimetrice ale
legturii (POP) n uniti Q2 i Q1, mpreuna cu (PO2) simetric i asimetric n uniti Q2
i (PO3)2- n uniti Q1. Prezena legturilor BOB n uniti Q2 i Q1 este de asemenea
evideniat.
Rugozitatea depunerilor PLD crete de la 60 la 150 nm la 400 C, respectiv de la 20 la 50
nm la 600 C (temperatur substrat) atunci cnd numrul de pulsuri crete de la 12500 la
25000. Au fost cercetate particularitile de deformare a sticlelor la nano- i micro-
indentare n dependen de condiiile de deformare. S-a stabilit c sticlele borofosfatice au
proprieti mecanice mbuntite, comparativ cu cele aluminofosfatice. Curbele DSC
pentru sticlele de volum au artat un efect endoterm, corespunznd Tg i unul sau dou
efecte exoterme, corespunznd cristalizrii sticlei. Pentru probele dopate cu pmnturi rare
se observ rotiri semnificative Faraday (mergnd pn la 0.17 min/cm/Oe la 400 nm).
Mulumiri: Autorii sunt recunosctori UEFISCDI, Romania, pentru suportul financiar n cadrul proiectului
M-ERA.NET 7-081/2013, Parteneriate 186/2012 i Bilateralului Romno-Moldav 695/2013 i
13.820.05.20/RoF/2013 i proiectului CSTD ASM nr. 15.817.02.06A. Aceast cercetare a fost finanat i de
proiectul M-ERA.NET/0010/2012 i de fonduri FEDER prin programul COMPETE 2020 i naionale prin FCT
Fundaia Portughez de tiina i Tehnologie prin proiectul nr. POCI-01-0145-FEDER-007688, ref.
UID/CTM/50025.

60
Bibliografie
1. O. Shikimaka, D. Grabco, B.A. Sava, M. Elisa, L. Boroica, E. Harea, C. Pyrtsac, A. Prisacaru, Z. Barbos.,
Journal of Materials Science, 2015, 51(3), 1409-1417 (2016)
2. M. Valeanu, M. Sofronie, A.C. Galca, F. Tolea, M. Elisa, B.A. Sava, L. Boroica, V. Kuncser, Journal of
Physics D: Applied Physics, 49 (2016) 075001

Bulk glasses, powders and thin films were obtained by sol-gel, magnetron sputtering - MS
and pulsed laser deposition - PLD methods from Bi-Pb and Dy-Tb ions co-doped boro-
phosphate systems. The influence of precursors, pH, temperature, time, on the sol-gel
process, and also the MS and PLD process parameters influence on films properties were
investigated. The structure and properties of the obtained samples were analyzed by using
Raman, FTIR and UV-Vis spectroscopy, thermal analysis and mechanical behavior at
nano- and micro - scale under concentrated load action [1]. The structure - properties
correlation was studied by using XRD, XRF, SEM-EDS, and AFM measurements. The
magneto- optical properties were analyzed using a modified Kerr device [2]. The Raman
spectra for the bulk glass permitted the identification of symmetric and asymmetric
vibrations of (POP) bond in Q2 and Q1 units, together with symmetric and asymmetric
(PO2) in Q2 and (PO3)2- in Q1 units. The presence of (BOB) bonds in Q2 and Q1 units is
also evidenced.

The roughness of PLD films increased from 60 to 150 nm at 400 C, and from 20 to 50 nm
at 600 C (substrate temperature) when the number of pulses increased from 12500 to
25000, respectively. The features of glasses deformation at nano- and micro- indentation
were studied depending on the deformation conditions. It was established that the boro-
phosphate glasses have improved mechanical properties in comparison with alumino-
phosphate ones. The DSC curves for bulk glasses showed one endothermic effect,
corresponding to Tg, and one or two exothermic effects corresponding to glass
crystallization. For the rare earth doped samples, an important Faraday rotation was
observed (up to 0.17 min/cm/Oe at 400 nm).

Acknowledgements: The authors are grateful to the UEFISCDI (Executive Unity for Financing of Higher
Education, Research and Innovation), Romania, for the financial support in the frame of 7-081/2013 M-
ERA.NET project, 186/2012 project from Partnership Program and Bilateral Romanian-Moldavian project
695/2013 and 13.820.05.20/RoF/2013 and CSTD ASM project nr. 15.817.02.06A. This work was also
supported by M-ERA.NET/0010/2012 project and by FEDER funds through the COMPETE 2020 Programme
and National Funds through FCT - Portuguese Foundation for Science and Technology under the project
number POCI-01-0145-FEDER-007688, ref. UID/CTM/50025.

References:
1. O. Shikimaka, D. Grabco, B.A. Sava, M. Elisa, L. Boroica, E. Harea, C. Pyrtsac, A. Prisacaru, Z. Barbos.,
Journal of Materials Science, 2015, 51(3), 1409-1417 (2016)
2. M. Valeanu, M. Sofronie, A.C. Galca, F. Tolea, M. Elisa, B.A. Sava, L. Boroica, V. Kuncser, Journal of
Physics D: Applied Physics, 49 (2016) 075001

61
INVESTIGATION OF THE STRUCTURAL, OPTICAL AND
ELECTRICAL PROPERTIES OF Sb DOPED SnO2 THIN FILMS
DEPOSITED BY SPRAY PYROLYSIS
Chourouk Nassiri1, Adil Hadri1, Mustapha Rouchdi1, Abderrahim El hat1, Boubker
Fares1, Larbi Laanab2 and Ahmed Mzerd1*
1 LPM, Faculty of Science, Mohammed V University, Rabat- Morocco
2 LCS, Faculty of Science, Mohammed V University, Rabat- Morocco

SnO2 and Sb-doped SnO2 (ATO) thin films were deposited on glass substrate at 400 C by
chemical spray pyrolysis. The structural, optical and electrical properties were investigated
as a function of dopant concentration, which was varied between 0 and 5 at % of Antimony
by using XRD, AFM, UV-visible spectrophotometry and Hall effect measurement
techniques. It is found that the films are polycrystalline in nature with a tetragonal crystal
structure with a preferential orientation along [110] direction. All the ATO films exhibit a
transmittance between 75 and 85 % in the visible range. The ATO films were n-type
degenerate semiconductor with a lowest electrical resistivity of about 6.010-3 .cm.

Keywords: Spray pyrolysis, Thin films, Sb-doped SnO2, Characterization.

62
NOI MATRICI CERAMIC-VITROASE PENTRU IMOBILIZAREA UNOR
DEEURI DE CROM
NEW GLASS-CERAMIC MATRIX FOR THE CHROMIUM WASTES
IMMOBILIZATION
Cosmin Vancea*, Giannin Mooarc, Adina Laia, Romul Marius Jurca
Universitatea Politehnica Timioara, Facultatea de Chimie Industrial i Ingineria Mediului,
Timioara, Romnia

Lucrarea de fa propune o alternativ de reciclare a dou deeuri de sticl comune: geam


i partea conic a tubului cinescop, mpreun cu caolinul de Bojidar sub forma unei matrici
ceramic-vitroase pentru fixarea unor deeuri de crom. Caolinul a fost n prealabil utilizat ca
mediu adsorbant pentru reinerea Cr6+ solubil dintr-o ap rezidual uzat. Pentru sinteza
probelor au fost folosite trei rapoarte gravimetrice deeu de sticl:caolin (60:40, 70:30 i
respectiv 80:20). Materiile prime pulverulente (fraciunea granulometric sub 0,1 mm) au
fost omogenizate mpreun i apoi presate sub form cilindric avnd diametrul i
nlimea de cca. 35 mm. Tratamentul termic s-a realizat la trei temperaturi diferite (900,
1000 i 1100C), timp de 60 minute. Compactitatea probelor obinute a fost caracterizat
pe baza porozitii aparente i respectiv a densitii aparente. Acestea variaz ntre
0-22,93% n cazul porozitii aparente i respective ntre 1.93-2.25 g/cm3 pentru densitatea
aparent, n funcie de tipul deeului de sticl utilizat i de temperatura de tratament termic.

Structura microporoas a probelor a fost ilustrat folosind imagini SEM. Compoziia fazal
a materialelor obinute, stabilit prin difractometrie RX a pus n eviden ca faze cristaline
principale cristobalitul, diopsidul, tridimitul i wollastonitul. Rezistena la compresiune a fost
corelat cu temperatura de sintez, cele mai bune valori, ntre 136-175 N/mm2,
corespunznd probelor obinute la 1000C. Stabilitatea hidrolitic i chimic i respectiv
capacitatea de imobilizare a cromului au fost determinate pe baza American Extraction
Procedure Toxicity Test, ISO 719/1985 i DIN 12116/2001. Toate probele sintetizate au
imobilizat complet ionii de crom astfel c nu au fost identificate pierderi de crom, indiferent
de pH soluiilor de extracie. Rezultatele obinute sugereaz c imobilizarea unor deeuri
de crom adsorbite pe caolin sub forma unor matrici ceramic-vitroase reprezint o soluie
viabil cu multiple avantaje economice.

The present paper propose an alternative recycling method for two common glass wastes:
window panes and funnel CRT glass, together with Bojidar kaolin as new glass matrix for
chromium waste immobilization. The kaolin was previously used as adsorption support for
the soluble Cr6+ waste from residual waters. Tree different weight ratios glass waste:kaolin
(60:40, 70:30 and 80:20) were used for the glass-ceramic synthesis. The raw materials as
powders (granulometric fraction under 0.1 mm) were mixed together and then pressed into
cylinders having the diameter and height around 35 mm. The heat treatment was
conducted at three different temperatures 900, 1000 and 1100C respectively for 60
minutes.

63
The compactness of the obtained glass-ceramic samples was characterized using their
apparent porosity and apparent density. The obtained values range from 0 to 22.93% for
the apparent porosity and from 1.93 to 2.25 g/cm3 for the apparent density respectively,
depending on the glass waste type and heat treatment temperature. The microporous
structure was illustrated using SEM. The phase composition of the studied samples was
established by RX diffraction, cristobalite, diopside, tridymite and wollastonite being the
main crystalline phases. The compressive strength of the obtained glass-ceramic products
was measured and correlated with the heat treatment temperature. The highest values
range from 136 to 175 N/mm2, corresponding to the samples obtained at 1000C. The
hydrolytically and chemical stability, and chromium leechability were determined according
to the American Extraction Procedure Toxicity Test, ISO 719/1985 and DIN 12116/2001
respectively. All the studied samples completely immobilized the chromium ions in the
glass-ceramic matrix so that no chromium extraction was recorded, regardless the pH of
the leeching solution. The obtained results suggest that the immobilization of the chromium
wastes adsorbed on kaolin in glass ceramic matrix is a viable solution having multiple
economic advantages.

64
STUDIUL SOLUIILOR SOLIDE DE TIPUL La1-XSrXCoO3 CU STRUCTUR
PSEUDO-PEROVSKITIC (x=0,4 i 0,5)
THE STUDY OF THE SOLID SOLUTIONS La1-XSrXCoO3
WITH PSEUDOPEROVSKITE STRUCTURE (x = 0.4 and 0.5)
Maria Preda1, Georgeta Velciu2, Alina Melinescu1, Virgil Marinescu2, Victor Fruth3,
Cristian Hornoiu3
1Universitatea Politehnica din Bucureti, Romnia
2InstitutulNaional de Cercetare Dezvoltare pentru Inginerie Electric ICPE-CA Bucureti,
Romnia
3Institutul de Chimie Fizic Ilie Murgulescu al Academiei Romne, Bucureti, Romnia

S-au sintetizat La0,6Sr0,4CoO3 i La0,5Sr0,5CoO3 folosindu-se ca materii prime La2O3, SrCO3


i Co3O4. Prepararea amestecului de materii prime s-a fcut prin activare mecanic n
moara cu bile de tipul Pulverisette, raportul dintre bile i material fiind de 10:1, iar lichidul
de umectare a fost alcoolul. Dup activare s-a determinat distribuia dimensiunii particulelor
din cele dou probe i s-a constatat c, aceasta este monomodal, iar valoarea limii
relative de distribuie, este egal cu 3,7 ceea ce arat un grad de mprtiere redus.

Fenomenele chimice care au loc la ardere s-au studiat prin analize termice i s-a constatat
existena unor efecte complexe endoterme, nsoite de pierdere de mas. Acestea sunt
determinate de eliminarea componentelor volatile din La(OH)3, SrCO3 i Co3O4, dar i din
unii compui intermediar formai. Pentru proba cu compoziia La0,5Sr0,5CoO3 s-a observat
la temperatura de 930C, un efect exoterm propriu formrii SrCoO3. Probele menionate au
fost tratate termic, n cuptor electric, la temperaturi cuprinse ntre 1000 i 1250C cu dou
ore palier la temperatura maxim. Compoziia mineralogic a acestora s-a determinat prin
difracie de raze X. Din rezultatele obinute s-a putut constata c, pentru prima dintre
probe, primul compus care se formeaz este LaCO3, iar pentru cea de-a doua prob este
SrCoO3. Prezena celor doi compui se constat chiar de la temperatura de 1000C. Alturi
de acetia se mai observ cantiti reduse de oxid de cobalt pn la temperatura de
1200C. n ambele cazuri, la 1250C se constat formarea unor soluii solide,
La0,6Sr0,4CoO3 avnd structur derivat din LaCoO3, iar La0,5Sr0,5CoO3 din SrCoO3.

Determinrile de densitate au aratt c. la temperatura de 1250C se obine pentru


La0,6Sr0,4CoO3 o densitate relativ de 86%, iar pentru La0,5Sr0,5CoO3 o densitate de 91%.

Rezultatele arat o mai bun tendin la sinterizare pentru cea de-a doua prob. Prin
microscopie electronic, efectuat pe probe tratate termic la 1250C, s-a constatat, n
ambele cazuri, granule de form poligonal de diferite dimensiuni. Prin msurtori de
variaie a proprietilor electrice n funcie de temperatur s-a stabilit c, La0,6Sr0,4CoO3
este un semiconductor cu coeficient de temperatur pozitiv, iar La0,5Sr0,5CoO3 are
comportare metalic.

65
La0,6Sr0,4CoO3- and La0,5Sr0,5CoO3 were synthesized using La2O3, SrCO3 and Co3O4 as
raw materials. The mixture of the raw materials was realized through mechanical activation
in the ball mill type Pulverisette. The ratio of balls and material was 10:1, and the wetting
liquid was alcohol. After the mechanical activation, the particle size distribution for the two
samples was determined, and it has been found that this is unimodal, and the value of the
relative fractional width of differential distribution is equal to 3.7, which looks like a low level
of scattering.

The chemical phenomena that occur at the thermal treatment were studied by the thermal
analyses and it was found the existence of endothermic complex effects accompanied by
mass loss. These are determined by the removal of volatile components from La(OH)3,
SrCO3 and Co3O4, or from the formation of the other intermediate compounds. For the
La0,5Sr0,5CoO3- composition an exothermic effect at 930C was observed. This effect can
be assigned to SrCoO3 formation. The mentioned samples were thermally treated in an
electric furnace at the temperatures between 1000 and 1250C with a plateau of two hours
at maximum temperature. Their phase composition was determined by X-ray diffraction.

The obtained results has presented that in the La0,6Sr0,4CoO3- sample, the first formed
compound is LaCoO3, and for the La0,5Sr0,5CoO3- composition is SrCoO3. The presence of
the two compounds is observed even the temperature of 1000C. Along with them is
observed a small amount of cobalt oxide at temperatures up to 1200C. In both cases at
1250C, it is found the formation of some solid solutions namely La0,6Sr0,4CoO3- based on
LaCoO3 structure and La0,5Sr0,5CoO3- based on SrCoO3 structure.

The density measurements noticed, that at temperature of 1250C for La0,6Sr0,4CoO3- is


obtained a relative density of 86% but for La0,5Sr0,5CoO3- this is 91%.

These results show a greater tendency at sintering for the second sample. By scanning
electron microscopy, carried out on samples treated at 1250C, was found in both cases,
that the grains are polygonal shape of different sizes. By measuring the variation of the
electrical properties depending on temperature, it was determined that La0,6Sr0,4CoO3- is a
semiconductor with a positive temperature coefficient and La0,5Sr0,5CoO3- has a metallic
behavior.

66
CRETEREA STRATURILOR SUBIRI DE TITANAT ZIRCONAT DE
PLUMB (PZT) PENTRU APLICAII N DETECTORII DE INFRAROU
GROWTH OF LEAD ZIRCONIUM TITANATE (PZT) THIN FILMS FOR
INFRA-RED DETECTORS APPLICATIONS
Jenica Neamu1, Alina Iulia Dumitru1, Virgil Marinescu1
1Institutul Naional de Cercetare Dezvoltare pentru Inginerie Electric ICPE CA,
Bucureti, Romnia

Senzorii piroelectrici cu straturi subiri sunt utilizai cu succes pentru multe aplicaii astfel c
monitorizarea polurii, detectori de infrarou pentru securitatea uman i a locuinelor,
Exist o legtur strns ntre piroelectricitate i piezoelectricitate, una din consecinele
acestei legturi fiind faptul c toate materialele piroelectrice sunt n acelai timp i
piezoelectrice.
Scopul lucrrii noastre este creterea straturilor subiri de titanat-zirconat de plumb (PZT)
pentru structurile sensitive ale detectorilor de infrarou, realizai prin microtehnologie.
Straturile subiri de PZT realizate prin depunere n vid inaintat, pulverizare de Radio
Frecven (RF), trebuie s aib proprieti electrice i structurale apropiate de ale
materialului PZT bulk.
Titanat zirconatul de plumb Pb(Zr1-x)TixO3 (PZT) este obinut ca soluie solid din faza
feroelectric PbTiO3 i antiferoelectric PbZrO3. Proprietile ceramicii policristaline pe
baz de soluie solid PZT pot fi adesea modificate prin adiii de donori i acceptori
pentru a obine materiale soft respectiv hard [1,2]. Structura de tipul perovskite este
descris de formula general ABO3 (unde A ion monotrivalent, B ion trihexavalent),
i confer posibilitatea de a se realiza substituii n poziia A respectiv B, obinnd astfel un
material nou PZT.
n prima etap am elaborat, prin tehnologia ceramic, 3 materiale PZT fiind catozii- int
pentru pulverizarea catodic n vid a straturilor subiri. Astfel cele trei compoziii ale
catozilor- int notate cu PZTc, PZTc_PbO,PZTc_MnO sunt prezentate mai jos:
PZTc Pb [( Zr0,52 Ti0,48)]O3
PZTc_PbO Pb [( Zr0,52 Ti0,48)]O3 cu 10%exces PbO
PZTc_MnO Pb [( Zr0,52 Ti0,48)]O3 cu 1% adaos MnO
n elaborarea acestor variante compoziionale am folosit tehnologia proprie pentru
obinerea materialelor ceramice piezoelectrice, urmrind n permanen corelarea dintre
gradul de puritate i finee al materiilor prime utilizate, condiiile specifice fiecrei etape
tehnologice i proprietile fizico-electrice finale. Toate cele 3 variante au prezentat
structura cristalin perovskite i proprieti piezoelectrice.
Pentru creterea straturilor subiri perovskite PZT prin metoda de depunere RF Sputtering
s-au utilizat instalaiile: Magnetron Sputtering (ETPV-SSNT), de la firma BESTEC GmbH,
Germany i UHV System Sputtering& E-Beam ATC-2200V de la firma AJA INT. SUA.
S-au realizat 3 tipuri de straturi subiri PZT utiliznd cei 3 catozi-int PZTc, PZTc_PbO,
PZTc_MnO i n total 12 probe de straturi subiri PZT, prin efectuarea de tratamente
termice la 6000 C/30 min, 6500 C/30 min i 7000 C/30 min in aer.
Grosimea stratului subire PZT crete odat cu temperatura de calcinare i anume s-a
obinut 33 nm pe filmul netratat, 43 nm pe filmul tratat la 6000 C/30 min i 132 nm pe stratul
67
subire tratat la 6500 C/30 min. Se observ formarea structurilor tetragonale caracteristice
pe suprafaa stratului subire odat cu tratamentele la 6500 C/30 min n aer i 7000 C/30
min in aer.

Thin films pyroelectric sensors have been successfully used in many applications, such as
pollution monitoring, infrared detectors for human and home security. It is a tight
connection between pyroelectricity and piezoelectricity, consequently all pyroelectric
materials are at the same time the piezoelectric materials.
The goal of our work it is the growth of lead zirconium titanate (PZT) thin films for sensitive
structures of infra-red detectors fabricated by micro-technology. PZT thin films deposited
by high vacuum RF sputtering must have the electrical and structural properties like these
of PZT bulk materials.
The lead zirconium titanate (PZT) is fabricated as solid solution between ferroelectric
PbTiO3 phase and antiferroelectric PbZrO3. The properties of policrystalline ceramics based
on PZT solid solution can be frequently changed by addition of "donors" and acceptors to
get soft materials respective hard materials [1,2]. The structure of perovskite type with
general formula ABO3 (were A monotrivalent ion, B trihexavalent ion), give the
possibility to achieve the substitutions in A site respective B site getting in this way a new
PZT material.
In first stage we made, by ceramic technology, three PZT materials for the targets used in
PZT thin films sputtering deposition.
So that the compositons of targets noted by PZTc, PZTc_PbO, PZTc_MnO are: PZTc
Pb [( Zr0,52 Ti0,48)]O3
PZTc_PbO Pb [( Zr0,52 Ti0,48)]O3 , 10% PbO excess
PZTc_MnO Pb [( Zr0,52 Ti0,48)]O3 , 1% MnO addition
For materials elaboration we used our piezoelectric materials technology, permanently
corelating the purity and fineness of the used matters, the specific conditions of all stages
technology and the final physico&electrical properties. All the three compositions shows
perovskite structure and piezoelectric properties.
For the growth of lead zirconium titanate (PZT) thin films by RF Sputtering we used the
equipments: Magnetron Sputtering (ETPV-SSNT), BESTEC GmbH, Germany and UHV
System Sputtering& E-Beam ATC-2200V, from AJA INT. SUA.
We achieved 3 types of PZT thin films, from the targets PZTc, PZTc_PbO, PZTc_MnO and
total 12 samples of PZT thin films, by calcinated at 6000 C/30 min, 6500 C/30 min si 7000
C/30 min in air.
The thickness of PZT thin films grow with the temperature from 33 nm on un-calcinated
film to 43 nm for the film calcinated at 6000 C/30 min and 132 nm for film calcinated at 6500
C/30 min. We observe the growth of thetragonal structure of films at the treatments of 6500
C/30 min in air and 7000 C/30 min in air.

References:
1.B. Jaffe, R. W. Cook, and H. Jaffe, Piezoelectric Ceramics. Acad. Press N. Y.( 1971) 234-245
2. G.H.Haertling, J.Am.Ceramic.Soc.82 (1999) pp797

68
EFFECT OF Cu ON THE PHYSICAL PROPERTIES OF ZnO SYNTHESIZED
BY SPRAY PYROLYSIS TECHNIQUE
Abderrahim El Hat, Mustapha Rouchdi, Adil Hadri, Chourouk Nassiri,
Fatima Zahra Chafi, Boubker Fares, Najem Hassanain,
Larbi Laanab, Ahmed Mzerd
Materials physics Laboratory (LPM), University Mohammed V,
Faculty of Sciences, Rabat, Morocco

Zn1-xCuxO thin films with different Cu concentration x= (0; 2; 5; 7 at %) are deposited by


spray pyrolysis technique on heated glass substrate at 350C. The physical properties of
the films are characterized by several techniques in order to study their structural, surface
roughness, optical and electrical properties. It is observed from X-ray diffraction (XRD)
analysis that the Cu doped ZnO films are polycrystalline and exhibit a preferential
orientation along (002) plane. The Atomic force microscopy (AFM) measurements revealed
that the surface roughness of the films is decreased from 0 to 5 at % Cu then increased
strongly for 7 at % Cu. From optical measurements, a significant decrease in average
optical transmission is observed for all doped samples and the band gap value is
decreased from 3.3 to 3.07 eV with increase in Cu concentration. The Hall Effect electrical
measurements show that all samples are n-type and the best value of the electrical
resistivity 1.35x10-1(.cm) is obtained for 5 at % Cu.

69
STRUCTURA, MICROSTRUCTURA I COMPORTAREA ELECTRIC A
UNOR PRODUSE CERAMICE SOL -GEL Ba1-xSrxTiO3
PENTRU APLICAII PIROELECTRICE

STRUCTURE, MICROSTRUCTURE AND ELECTRICAL BEHAVIOUR


OF SOME SOL-GEL Ba1-xSrxTiO3 CERAMICS FOR
PYROELECTRIC APPLICATIONS
Adelina Ianculescu1, Ioana Pintilie2, Lucian Pintilie2*, C. A. Vasilescu1,3, Alina Melinescu1,
Mihaela Botea2, Alin Iuga2, Nicolae Drgan4, Dorel Crian4
1 Universitatea Politehnica din Bucureti, Departamentul de Inginerie i
tiina Materialelor Oxidice, Romnia
2 Institutul Naional de Cercetare-Dezvoltare pentru Fizica Materialelor, Romnia
3 Institutul Naional pentru Fizica Laserilor, Plasmei i Radiaiilor-INFLPR, Romnia
4Institutul de Chimie Fizic Ilie Murgulescu, Academia Romn, Romnia

Nano-pulberile Ba1-x SrxTiO3 (BST) cu x = 0; 0,10; 0,20 i 0,30 au fost preparate prin
metoda sol-gel din izo-propilat de titan i acetai de bariu i stroniu. Datele de difracie cu
raze X au artat formarea fazei perovskit bine cristalizat (Ba,Sr)TiO3, cnd precursorii
gelului au fost tratai termic n aer la 900C timp de 2 ore. Peletele ceramice cu densitate
relativ de 89-95% au fost obinute dup sinterizare la 1400C timp de 4 ore. Creterea
coninutului de Sr induce scderea gradului de tetragonalitate i dimensiunea medie a
granulei. In toate masele ceramice investigate s-au identificat tranziii fazale feroelectrice-
paraelectrice precise, maxima mare de permitivitate dielectric (de 4000 - 5030) i pierdere
dielectric mic la temperatura camerei (tan 3%). Temperatura Curie scade n mod
linear cu creterea adaosului de substan dizolvat, x. La temperatura camerei toate
compoziiile BST sunt n stare feroelectric. Toate compoziiile au dezvoltat proprieti
piroelectrice bune, cele mai bune valori pentru coeficientul piroelectric intrinsec i factorul
de calitate s-au obinut pentru proba cu 30% Sr dopare.

Ba1-x SrxTiO3 (BST) nanopowders with x = 0; 0.10; 0.20 and 0.30 were prepared by sol-gel
method from titanium isopropoxide and barium and strontium acetates. X-ray diffraction
data show the formation of well-crystallized (Ba,Sr)TiO3 perovskite phase, when the gel
precursors were thermally treated in air at 900C for 2 hours. Ceramic pellets with relative
density of 89 95 % were obtained after sintering at 1400C for 4 hours. The increase of
Sr content induces the decrease of tetragonallity degree and average grain size. Sharp
ferroelectric-paraelectric phase transitions, high dielectric permittivity maxima (of 4000 -
5030) and low room temperature dielectric loss (tan 3%) were found for all the
investigated ceramics. The Curie temperature drops linearly with the increase of solute
addition, x. At room temperature all the BST compositions are in the ferroelectric state. All
the compositions exhibited good pyroelectric properties, with the best values for the
intrinsic pyroelectric coefficient and the figure of merit obtained for the sample with 30 % Sr
doping.
70
DEVELOPMENT OF TRANSPARENT CONDUCTIVE TIN DOPED ZnO
THIN FILMS: EFFECT OF TIN CONCENTRATION AND POST ANNEALING
Adil Hadri1,*, Mhamed Taibi2, Ahmed Mzerd1
1 University Mohammed V, Faculty of Sciences, Physics Department, LPM, Rabat,
Morocco
2 University of Mohammed V, Ecole Normale Superieure, LPCMIN, Rabat, Morocco

The present work is devoted to the elaboration and characterization of undoped and tin
doped ZnO deposited onto glass substrates by spray pyrolysis technique, starting from zinc
chloride and tin chloride precursors. The influence of Sn dopant on structural, optical and
electrical properties of ZnO thin films were characterized by X-ray diffraction (XRD),
ultaraviolet-visible spectroscopy and Hall Effect measurements using Van Der Pauws
method. The atomic percentages of dopant in the starting solution were 0%, 1%, 3% and
5%. Structural analysis confirmed the hexagonal wurtzite structure of all deposited films
with a polycrystalline nature. By applying scherrer formula to the preferential orientation,
the grain size decreased from 49.1 nm for undoped ZnO to 30 nm with increasing Sn
content up to 5 at.%. It was also observed that the peak position of the (002) plane shifted
slightly to the high 2 value with increasing Sn doping. The deposited thin films are highly
transparent with an average transmittance above 80% in the visible region. The lowest
electrical resistivity of the as deposited Sn doped ZnO films (71 .cm) combined with the
highest carrier concentration (61016 cm-3) and mobility (1.22 cm2.V-1.s-1) was noted at 3
at.% Sn Doping. In addition, an improvement of the electrical properties was seen after
post annealing under argon atmosphere at 350 C. It was noticed that the electrical
resistivity of the annealed films decreased sharply, by three orders of magnitude, due to
the increase of both carrier concentration and mobility.

71
INVESTIGATION OF STRUCTURAL, OPTICAL AND ELECTRICAL
PROPERTIES OF In DOPED SnO2 THIN FILMS DEPOSITED
BY SPRAY PYROLYSIS

Adil Hadri1, Fares Boubker1, Mohammed Loghmarti1, Chourouk Nassiri1, Ahmed Mzerd1
1University Mohammed V, Faculty of Sciences, Physics Department, LPM, Rabat,
Morocco
Indium doped SnO2- films were deposited on glass substrates by spray pyrolysis
technique and the influence of dopant concentration was investigated using X-ray
diffraction (XRD), Uv-Visible spectroscopy and Hall Effect measurements using van der
Pauws method. X-ray diffraction studies indicated that all films had preferred
orientation along (200) plane and were polycrystalline with tetragonal rutile structure.
The calculated average crystallite sizes increased after doping. Substitution of In into
SnO2- thin films can be confirmed by the shifting of the peaks in the XRD patterns.
Optical transmittance of the films showed high average transparency ~ 80-90% in the
visible region. Hall measurements showed that the conduction type was dependent on
In content. For low doped films (In 3 at.%), the films were n type, while at higher
doping concentration the films were p type.

72
INFLUENA CONDIIILOR DE OBINERE ASUPRA
CARACTERISTICILOR AEROGELURILOR DIN SIO2
THE INFLUENCE OF OBTAINING PARAMETERS UPON
THE CHARACTERISTICS OF SIO2 AEROGELS
Adrian Dnu-ugui, tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

Aerogelurile au fost obinute prin metoda sol-gel. n timpul procesului de obinere s-au
variat mai muli parametri cum ar fi: temperatura, condiiile de maturare, modificarea
caracteristicilor de suprafa, precum i timpul i condiiile de uscare.
Dup uscarea gelurilor a fost efectuat o analiz termic complex pentru a stabili
temperatura de calcinare i pentru determinarea proceselor care apar n timpul nclzirii.
Probele au fost tratate termic la 500, 900 si 1100C, cu un timp de palier de 2 ore.
Identificarea morfologiei nanopulberilor i determinarea compoziiei elementare s-au
efectuat cu ajutorul microscopiei electronice de transmisie (TEM). Pentru identificarea
fazal i a gradului de cristalinitate s-a efectuat analiza de difracie a razelor X.
Densitatea probelor sinterizate a fost determinat cu ajutorul unui densimetru cu heliu.
Conductivitatea termic s-a determinat utiliznd o metod empiric. Determinarea
suprafeei specifice, a dimensiunii porilor i a volumului de pori a fost fcut prin analiza
BET. De asemenea, au fost efectuate i teste de hidrofobicitate.

The aerogels were obtained by sol-gel method. During the obtaining were varied several
parameters such as temperature, aging conditions, alter the surface characteristics as well
as the time and drying conditions.
After gels drying was carried out thermal analysis in order to determine the calcination
temperature and the processes that occur during heating. The samples were thermally
treated at 500, 900 and 1100C, with 2 hours soaking time.
The morphology estimation and the identification of elemental composition of nanopowders
were performed using Transmission electron microscopy (TEM). In order to identify the
phase composition and the degree of crystallinity was carried out X-ray diffraction analysis.
The density of sintered samples was determined with helium densitometer. The thermal
conductivity was determined using an empirical method. The determination of specific
surface area, pore size and pore volume was made by BET method. Also, there were
made hydrophobic tests.

73
SINTEZA I PROPRIETILE UNOR LIANI CU ACTIVARE ALCALIN
DE TIP BOROSILICATIC
SYNTHESIS AND PROPERTIES OF ALKALI ACTIVATED BOROSILICATE
INORGANIC POLYMERS
Adrian Nicoar, Taha H.Abood Al Saadi, Alina Bdnoiu, Georgeta Voicu,
tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

Lucrarea prezint sinteza i proprietile unor polimeri anorganici de tip borosilicatic


(AABSIP) rezultai prin activarea alcalin a unui deeu de sticl, fin mcinat, cu o soluie
alcalin de hidroxid de sodiu i borax. Microstructura materialului obinut s-a apreciat prin
microscopie electronic de baleiaj (SEM) i compoziia prin difracie de raze X (XRD)
respectiv prin analiza EDAX.
Comportarea la tratament termic a produilor de reacie s-a apreciat prin analiza termic
complex - analiza termogravimetric (TG) i analiza termic diferenial (DTA).
Tratamentul termic al AABSIP determin o important cretere a volumului i a porozitii
deschise, comportament specific pentru materialele intumescente.

The paper presents the synthesis and properties of borosilicate inorganic polymers
(AABSIP) obtained by the alkali activation of cullet glass powder with a mixture of sodium
hydroxide solution and borax. The microstructure of resulted materials was assessed by
scanning electron microscopy (SEM) and the composition by X ray diffraction and Energy
Dispersive X ray Analyze (EDAX). The thermal behavior of the reaction products was
assessed by thermogravimetry (TG) coupled with differential thermal analysis (DTA).
Thermal treatment of AABSIP determines an important increase of volume and open
porosity intumescent behavior.

74
FILTRE CERAMICE ALUMINOASE CU SUPRAFA ACTIV
ALUMINA FILTER CERAMICS WITH ACTIVE SURFACE
Adrian Tbcaru, tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

Au fost obinute i caracterizate filtre ceramice aluminoase utiliznd diferite rapoarte de


agent porogen printr-o cale convenional de sintez. Corpurile ceramice crude au fost
obinute prin omogenizarea uscat -Al2O3 cu glucoz i prin presarea uniaxial a
amestecului. Acestea au fost tratate termic la 1400C cu un palier de 2 ore i apoi
caracterizate din punct de vedere ceramic (prin determinarea densitii aparente i a
porozitii deschise) i morfo-structural prin microscopie electronic de baleiaj.
Cu scopul de a mbunti caracteristicile membranare ale filtrelor, acestora li s-a adugat
un strat subire de TiO2 anatas. TiO2 a fost obinut prin metoda gelului galben i
caracterizat prin mai multe tehnici, cum ar fi: microscopia electronic de transmisie,
difracie de electroni pe zona selectat, difracie de raze X.
Proprietile fotocatalitice ale filtrelor s-au determinat prin absorbie UV-Vis, n soluie de
albastru de metilen.
Prin urmrirea vitezei de filtrare i din dimensiunea porilor se poate concluziona c filtrele
ceramice obinute aparin filtrelor specifice microfiltrrii.

Alumina filter ceramics were fabricated by using different ratio of pores generator agent
through a conventionally route of synthesis. Green bodies were obtained by dry mixing -
Al2O3 and D-Glucose and uniaxial pressing the mixture. The green compacts were
thermally treated at 1400C with a soaking time of 2 hours and then characterized from
ceramic view point (determining the apparent density and open porosity), and from
morphological and structural point of view by scanning electron microscopy.

In order to improve their membrane characteristics, a new thin layer of TiO2 anatase was
added on alumina support surfaces. TiO2 anatase was obtained via the yellow-gel method.
The TiO2 anatase was characterized by several techniques such as: transmission electron
microscopy, selected area diffraction, X-ray diffraction.
Also, the photo-catalytic properties were measured by UV-Vis absorption in blue methylene
solution.

The flow rate filtration and the pore size results conclude that the ceramic filters can be
fitted into microfiltration category.

75
ANALIZA DE MONITORIZARE A TEMPERATURII N INDUSTRIA
CIMENTULUI ALTERNATIV CARBUR DE SILICIU
TEMPERATURE MONITORING ANALYSIS IN THE CEMENT INDUSTRY
THE SILICON CARBIDE ALTERNATIVE
Adriana Graiela Pribeanu1, Doru Vladimir Pucau1, Florin Bernea2, Gheorghe Brezeanu3,
Florin Drghici3, Gheorghe Pristavu3, Rzvan Pascu4, Gherghina Ciortan1
1 CEPROCIM SA, Bucureti, Romnia
2 HeidelbergCement (Romnia) SA
3 Universitatea Politehnica din Bucureti, Romnia
4 Institutul Naional pentru Cercetare & Dezvoltare n Microtehnologie, IMT- Bucureti,

Romnia
n mediul industrial este esenial s existe o monitorizare exact a temperaturii n diferite
puncte ale fluxului tehnologic aceasta avnd implicaii n calitatea produsului finit. n
industria cimentului, aparatura de monitorizare a temperaturii este amplasat n diferite
puncte ale fluxului tehnologic.
Pe traseul instalaiei de clincherizare, instalaiei de mcinare combustibil solid, instalaiei
de uscare adaosuri i mcinare ciment monitorizarea temperaturii este necesar deoarece
trebuie determinat gradul de uscare al acestora.
Procesul de desprfuire a gazelor este eficient numai dac gazele introduse n electrofiltru
au o anumit temperatur i umiditate. Monitorizarea temperaturii gazelor, la ieirea din
acesta, determin gradul lor de umezire.
Monitorizarea temperaturii la capul cald i la mantaua cuptorului ne d informaii utile
pentru conducerea procesului de clincherizare. Monitorizarea temperaturii finii care
alimenteaz cuptorul se realizeaz pentru a determina eficiena schimbului de cldur, prin
circulaia n contra curent a gazelor din cuptor i a finii n interiorul schimbtorului de
cldur. Monitorizarea temperaturii clincherului rcit n rcitorul grtar determin gradul de
rcire i informeaz asupra posibilitii de transport a acestuia.
n afar de temperaturile msurate direct n procesul tehnologic, se monitorizeaz i
temperaturile prin care se determin buna funcionare a unor utilaje (lagrele unor utilaje,
nfurrile motoarelor electrice, etc.) pentru sesizarea depirii pragurilor admisibile.
Industria cimentului, datorit mediului de lucru foarte dur, att din punct de vedere
mecanic, ct i chimic, necesit materiale foarte rezistente pentru fabricarea senzorilor
care s monitorizeze procesul de fabricaie a cimentului. Soluiile curente, bazate
predominant pe termocuple i senzori rezistivi, au fiabilitate redus, prezentnd timpi de
via sub 3 luni.
Aceast lucrare i propune studiul unei soluii alternative de msurare a temperaturii n
mediu industrial, bazat pe diode Schottky pe carbur de siliciu, din punct de vedere al
preciziei de msur. Datorit dependenei cvasi-liniare a tensiunii n funcie de
temperatur, la curent constant, aceste dispozitive pot fi folosite cu uurin n detecia
cldurii, prezentnd rezisten mecanic i chimic excelente.

Pentru amplificarea i conversia semnalului dat de diod-senzor se folosete un circuit


dedicat.

76
Banda acestuia de amplificare este determinat prin simulri i comparat cu spectrul de
variaie a temperaturii incintei-int, n acest caz instalaia de mcinare materii prime, n
vederea confirmrii unei amplificri constante pe ntreaga plaj de variaie. Punctele
selectate pentru monitorizarea termic sunt intrare/ieire gaze moar de fin.
Nivelul de temperatur al gazelor nregistrat n camera de comand este cuprins ntre
250C i 400C, respectiv 80C i 120 C.

In an industrial environment, it is essential to monitor the exact temperature having


implications for the quality of the finished product. In cement industry the equipment for
monitoring temperature is located in various points of the process flow.
The path on the clinkering installation, the grinding installation of the solid fuel, the drying
and grinding plant cement admixtures, temperature monitoring have to be determined
because we have determined their wheat drying.
Process dedusting of the gas is effective only if the gases placed in electrofilter have a
certain temperature and humidity. Gas temperature monitoring at the exit from it, determine
their degree of wetness.
Monitoring temperature at the hot end and the furnace shell of the kiln give us useful
information to management process. Monitoring temperature of the flour what feeds the
kiln is performed to determine the efficiency of the heat exchange, by countercurrent flow
of gas from kiln and the flour in the inside heat exchange. Monitoring temperature of the
clinker cooled in the cooler grill determines the degree of cooling and informs on the
possibility of the its transport.
Outside the temperature measured directly in the process, is monitoring and the
temperatures that determines the proper functioning of equipment (bearings of machinery,
the windings of electric motors, etc.) for the exceeding the allowable threshold.
The cement industry, due to tough working environment, both in terms of mechanically and
chemically requires highly resistant materials for the manufacture of sensors to monitor the
cement production process.
Current solutions based predominantly on thermocouples and resistive sensors have poor
reliability, presenting life time under 3 months.
This work aims to study an alternative solution for temperature measurement in an
industrial environment, based on silicon carbide Schottky diodes, in terms of measurement
accuracy.
Due to the quasi - linear voltage-temperature dependence at constant current, these
devices can be used easily for temperature monitoring, while also exhibiting excellent
mechanical and chemical resistance.
For amplification and signal conversion, the diode sensor uses a dedicated circuit. Its
bandwidth is determined by simulations and compared to the spectrum of temperature
variation in the target enclosure, in this case the raw material grinding plant, in order to
confirm a constant gain on the entire range of variation. Thermal monitoring is established
at the gas entry and exit points of the flour mill. Gas temperature levels recorded in the
control room are 250C - 400C and 80C - 120C, respectively.
77
Acknowledgments. The work has been funded by the national Program PN2, contract no. 21/2012.

MATERIALE COMPOZITE DESTINATE PROTECIEI IMPOTRIVA


RADIAIILOR GAMMA
COMPOSITE MATERIALS USED FOR GAMMA RADIATION SHIELDING

Adriana Moan1, Viorel Fugaru2, Maria Gheorghe3, Ionela Petre1, Mariana Coarn1,
Lidia Radu3, Nastasia Saca3, Eugeniu Vasile4, Roxana Truc4
1 CEPROCIM SA, Bucureti, Romnia
2 Institutul Naional de Cercetare - Dezvoltare pentru Fizic i Inginerie Nuclear
"Horia Hulubei ", Romnia
3 Universitatea Tehnic de Construcii Bucureti, Romnia
4 METAV C&D, Romnia

Utilizarea materialelor radioactive pentru producerea energiei electrice, n industrie,


medicin sau pentru cercetare, conduce inevitabil la formarea de deeuri radioactive,
pentru gospodrirea crora este necesar dezvoltarea unui program integrat, care s
includ depozitarea definitiv. Acest program trebuie s indeplineasc obiectivul
fundamental de securitate, anume protejarea sntii oamenilor i a mediului nconjurtor,
acum i in viitor, de efectele nedorite ale radiaiilor ionizante.
Depozitarea deeurilor radioactive rezultate, conform condiiilor impuse de UE, se poate
face numai n spaii distincte, special amenajate pentru protejarea mediului nconjurtor.
n Romania, cea mai utilizat metod de protecie mpotriva radiaiilor o reprezint
utilizarea ecranelor protectoare din plumb, fier sau beton. Utilizarea acestor materiale
prezint dezavantajul necesitii realizrii unor ecrane de protecie cu grosimi
considerabile.
Astfel, la nivel naional, se are n vedere cercetarea posibilitii realizrii unor materiale
liante speciale (ciment, mortar i beton) destinate proteciei radioactive.
Folosirea acestor materiale, cu o compoziie corespunztoare, ca ecran de protecie
mpotriva radiaiilor reprezint o soluie eficient, datorit faptului c acestea pot prezenta
att proprieti de absorbie a radiaiilor ct i bune caracteristici mecanice i de
durabilitate.
Articolul prezint rezultatele experimentrilor de laborator privind posibilitatea utilizrii unor
materii prime naturale i deeuri, cu greutate specific mare, la realizarea unor materiale
cu capacitate sporit de ecranare a radiaiilor gamma, cu utilizri n domeniul nuclear.
Au fost preparate i caracterizate o serie de materiale de construcii (cimenturi, mortare i
betoane). Acestea au fost caracterizate din punct de vedere fizico-mecanic, structural i a
capacitii de atenuare a radiaiilor.
Rezultatele cercetrilor arat c utilizarea materiilor prime naturale i a deeurilor cu
greutate specific mare reprezint o soluie optim pentru obinerea materialelor compozite
cu capacitate sporit de ecranare a radiaiilor gamma.

78
Using of radioactive materials for electrical energy producing, in industry, medicine or for
research, direct inevitably at forming of radioactive wastes, for which administration is
necessary an integrated program, implying a definitive storage. This program must fulfill
the fundamental objective of security, such as protection of people health and environment,
as well as the protection against undesirable effects of ionizing radiations.

The storage of radioactive wastes, according to the UE imposed conditions, can be done
only in distinct spaces, especially designed for environment protection.
In Romania, the most used method of protection against radiations is the usage of
protection screen made of lead, iron or concrete. The main disadvantage of these
mentioned materials is the screens considerable thicknesses.

Thus, at national level, there are research regarding the possibility to obtain some special
building materials (cement, mortar and concrete) for radioactive protection.
Using of these materials, with a corresponding composition, as protection shield against
radiations represents an efficient solution, because these materials can have properties for
radiation absorption, as well as good strength and durability characteristics.

This paper presents laboratory experimental results regarding the possibility of using some
natural raw materials and wastes, with high specific weight, for obtaining some building
materials with increased shielding capacity for gamma radiations, with application in
nuclear range.

A series of building materials (cements, mortars and concrete) were prepared and
characterized. These materials were characterized from physical-mechanical, structural
point of view and of capacity for attenuation of the radiations.

The results of this research pointed out that the usage of the natural raw materials and
wastes with high specific weight could be good candidates for obtaining composite
materials with increased capacity of shielding gamma radiations.

79
VITROCERAMICI N SISTEMUL NA2O-CAO-P2O5-SIO2
PENTRU INGINERIA TISULAR
GLASS-CERAMICS IN NA2O-CAO-P2O5-SIO2 SYSTEM
FOR TISSUE ENGINEERING
Andreea Cristina Vjan, tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

n secolul XX o revoluie n domeniul sntii a generat o nou provocare pentru


societate: meninerea calitii vieii pentru populaia n curs de mbtrnire.

Biosticlele au fost mult timp studiate cu intenia de a dezvolta materiale adecvate pentru a
fi utilizate ca implanturi n corpul uman pentru restabilirea sau nlocuirea osului deteriorat.
Pentru c nu au rezisten mecanic, tendina tuturor este s transforme aceste biosticle n
vitroceramici.

Studii recente au artat c dintre toate potenialele faze care s-ar putea forma la o
cristalizare controlat a unei sticle Hench rezistena cea mai bun o d unul dintre
metasilicaii dubli de calciu i sodiu i anume NC2S3.

Astfel obiectivul acestei lucrri a fost obinerea i caracterizarea unui material vitrocristalin
care s conin NC2S3, obinut prin cristalizarea unei biosticle clasice (45S5) care conine
Na2O.

Pentru obinerea biosticlei Hench clasice s-a utilizat metoda sol-gel. Dup obinerea i
caracterizarea biosticlei, a fost obinut un material vitroceramic bioactiv prin cristalizarea
controlat a biosticlei. Pe materialul cristalizat s-au fcut studii asupra compoziiei fazale i
elementare cu ajutorul difraciei de raze X i cu ajutorul analizei EDX. De asemenea s-au
determinat proprietile ceramice (densitatea aparent i porozitatea deschis) i
proprietile mecanice. Analizele structural morfologice s-au realizat cu ajutorul
microscopiei electronice de baleiaj. Biocompatibilitatea materialului a fost demonstrat fie
prin imersarea probei n SBF urmrindu-se depunerea unui strat de fosfai de calciu pe
suprafaa probei, fie prin urmrirea viabilitii celulare timp de 72 de ore.

80
A 20th century revolution in health policies generated a new challenge to society:
maintaining the quality of life for the aging population.

Bioglasses have long been studied with the intent to develop suitable materials for implants
in the human body to restore or replace the damaged bone. Because they have low
mechanical resistance, the trend is to transform all these bioglass in glass-ceramics.

Recent studies have shown that of all the potential phase which may be formed by a
controlled crystallization of a Hench glass, the best mechanical strength is given by one of
the double calcium and sodium metasilicates namely NC2S3.
Thus the objective of this study was to obtain and characterize a glass-ceramic containing
NC2S3, obtained by crystallization of classical bioglass (45S5) with Na2O.

To obtain bioglass, the sol-gel method was used. After obtaining and characterization
bioglass, the bioactive glass-ceramic was obtained by controlled crystallization of bioglass.

The crystallized materials have been characterized from phase and elemental composition
view point using X-ray diffraction and EDX analyses. The ceramic properties (apparent
density and open porosity) were determined and the mechanical properties were assessed.
The morphological and structural analyzes were performed using scanning electron
microscopy. The biocompatibility of the obtained material has been demonstrated either by
immersing the sample in SBF aiming to calcium phosphates layer deposition on the
samples surface, either by tracking the cell viability (MTT assay) for 72 hours.

81
MODIFICATION OF GFRC TO INCREASE THE PERSISTENCE
OF THE FIBERS
Aleksey Kharitonov1, Nina Shangina2, Antonina Ryabova1
1 Saint Petersburg State University of Architecture and Civil Engineering, Russian
Federation
2 Petersburg State Transport University, Moscow, Russian Federation

The article presents the investigated results of physical and mechanical properties of glass
fiber reinforcement concrete (GFRC) in dependence on the reinforcement degree and of
the cement amount.
Its have been obtained the data on tensile and compression strength of the GFRC. The
dependence of the long-term deformation of concrete (creep and shrinkage) on the degree
of reinforcement has been discovered. It is shown that the use of glass fiber significantly
increases tensile strength but the compressive strength is being reduced slightly. It is
determined that fiber reinforcement leads to lower creep and shrinkage by almost twice. It
is experimentally proved that the introduction of the high active metakaolin increases the
tensile and compressive strength to a greater extent comparing to silica fume and the
fulleroid modifier. This trend is also correct to non alkali-resistant glass fiber.
Overall, the obtained data allow to estimate the influence of different additives on the
properties of GFRC.

82
COMPORTAMENTUL MATERIALELOR DE LEGTUR DINTR-UN
SISTEM DE BARIERE TERMICE LA TEMPERATURI INALTE

HIGH TEMPERATURE OXIDATION BEHAVIOUR OF ALTERNATIVE


BOND COAT MATERIALS AS PART OF A TBC SYSTEM
Amalia Soare1, Ioana Cski2, Cristina Oprea3, Sorin Soare1, Cristian Predescu2
1 Institutul Naional de Cercetare-Dezvoltare pentru Tehnologii Criogenice Izotopice-
INCDTCI- Rmnicu Vlcea, Romnia
2 Universitatea Politehnica din Bucureti, Romnia
3 TENSOR SRL, Romnia

Obiectivul principal al acestui proiect este cercetarea fundamental n ceea ce privete


proiectarea, performana i durabilitatea sistemelor de bariere termice (TBC). Acest sistem
complex este format din mai multe straturi: bariera termic (reprezint partea superioar),
oxidul crescut in urma expunerii la temperatura (TGO - Thermally Grown Oxide), stratul de
legtur (BC Bond Coat) i superaliajul pe baz de Ni care reprezint componenta
principal a sistemului. Se poate argumenta c BC este cel mai important component al
sistemului care, n principal, este alctuit din -NiAl i aliaje de (Ni, Co) CrAlY.
n cadrul acestui proiect propunem o alternativ la materialele traditionale care compun
stratul de legatur, pe baz de Ru, care, dac se va dovedi eficient va avea un important
impact economic.

The main objective of this project is the fundamental research into the design, performance
and durability of thermal barrier systems (TBC). This complex system is made of several
layers: the thermal barrier coating on top, the thermally grown oxide TGO which grows on
the bond coat BC during high temperature exposures and the Ni base superalloy which is
the main component of the system. Arguably, the BC is the most important layer of the
system and traditionally are based on single phase -NiAl (typically Pt-modified) and on
(Ni, Co)CrAlY alloys. We propose within this project an alternative to the traditional BCs,
based on Ru which if proved efficient will have an important economical impact.

83
EFFECT OF Nd AND Tm CO-DOPING ON STRUCTURAL, OPTICAL
AND ELECTRICAL PROPERTIES OF ZnO THIN FILMS
Amina El Fakir
University of Mohammed V-Materials Physics Laboratory, Faculty of Sciences, Morocco

Rare earth (Nd, Tm) co-doped ZnO thin films were deposited on glass substrates by
chemical spray pyrolysis method. The influence of both doping concentration on structural,
optical and electrical properties were studied by various techniques. X-ray diffraction (XRD)
patterns revealed that all the films have a polycrystalline nature fitting with a hexagonal
wurtzite structure. Transmittance measurements showed that the addition of Tm reduced
the optical transmittance from 80 % to about 50 % in the visible region while the optical
band gap increased slightly with Tm doping concentration. Photoluminescence spectra
were dominated by an emission band due to the radiative recombination of excitons and a
large band attributed to the defects, which decreased and shifted toward lower wavelength
region after Tm doping. Electrical resistivity value around 4 10-2 .cm was achieved for
(Nd,Tm) co-doped films.

84
INFLUENA GRANULOMETRIEI ARGILEI ASUPRA RECICLRII
NMOLURILOR DE EPURARE NTR-O MATRICE CERAMIC

THE INFLUENCE OF CLAY FINENESS UPON SLUDGE RECYCLING


IN A CERAMIC MATRIX
Anna-Mria Szke1, Marcela Muntean2
1 Universitatea Babe-Bolyai,Facultatea de tiina Mediului, Extensia Sf.-Gheorghe,,
Romnia
2Universitatea Politehnica din Bucureti, Facultatea de Chimie Aplicat i

tiina Materialelor, Romnia

Fezabilitatea reciclrii nmolului n procesul de fabricaie a ceramicii a fost evaluat prin


testare in condiii de laborator. Asemenea reziduuri au compoziie chimic i mineralogic
similar cu amestecul brut pentru ceramica bruta ecologica utilizat n construcii.
Au fost preparate cteva mase ceramice cu argil i diferite proporii de nmol care au fost
caracterizate din punct de vedere al proprietilor fizico-mecanice. Pentru fiecare amestec
brut a fost considerat fineea argilei, componenta principal a ceramicii brute ecologice.
Proporia de nmol de epurare adugat depinde de fineea argilei i de asemenea de
capacitatea de sinterizare, care crete cu fineea argilei.
n prezena unei proporii mici de nmol (7-20%) proprietile ceramice, n mod particular
porozitatea deschis i proprietile mecanice, prezint mici modificri. Introducerea unui
asemenea deeu n matricea ceramic de construcii (crmizi, igle i plci) are o foarte
bun perspectiv.

Cuvinte cheie: materii prime, fineea argilei, matricea ceramic

The feasibility of sludge recycling in the ceramic manufacture was evaluated through
laboratory testing. Such residues have similar chemical and mineralogical composition with
the raw mixture of the green ceramic body used in construction.
Several ceramic masses with clay and various proportion of sludge have been synthesized
and then characterized by their physical-mechanical properties. The fineness of the clay,
the main component of the green ceramic body, has been considered for every raw
mixture. The proportion of the sludge waste addition depends on the clay fineness and the
sintering capacity also, increases with the clay fineness.
The ceramic properties, particularly, the open porosity, and mechanical properties, in
presence of small sludge proportion (7-20 %) shows small modification. The introduction of
such waste into building ceramic matrix (bricks, tiles, and plates) has a very good
perspective.

Keyword. Raw materials, clay fineness, ceramic matrix.

85
COMPORTAREA CRMIZILOR REFRACTARE BAZICE N TIMPUL
FUNCIONRII CUPTORULUI DE CLINCHER
THE BEHAVIOR OF THE REFRACTORY BASIC BRICKS
DURING OPERATION OF A CLINKER KILN
Bogdan Ctlin Marin, Georgeta Voicu, tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

Calitatea refractarelor utilizate n cuptoarele rotative de clincherizare este un factor


important n operarea eficient i sigur. Refractarele bazice sunt un subiect sensibil cu un
impact major asupra costurilor de producie, care sunt intens cercetate pentru a se
dezvolta noi produse inovatoare cu o durat de via ct mai mare. De asemenea, n
prezent coroziunea refractarelor este mult mai intens datorat tendinelor actuale de a
substitui ntr-o proporie ct mai mare combustibilul primar (crbunele), cu o serie de
combustibili alternativi.
Crmizile refractare pe baz de MgO sunt utilizate cu succes att n industria cimentului
ct i in industria de var, avnd o stabilitate termic ridicat i o stabilitate chimic bun.
Prezentul studiu are ca scop investigarea crmizilor refractare din zona central de
ardere dup o funcionare de 1700 de ore ntr-un cuptor de clincherizare cu o capacitate de
3000 t / zi.
Crmida puternic corodat dup o perioada scurt de utilizare a fost analizat folosind
tehnicile de microscopie electronic de baleiaj asociat cu sonda EDX i analiza de
difracie a razelor X comparativ cu eantioane noi de crmid, urmrind n acelai timp
compoziia lipiturii formate pe suprafa.
De asemenea, lipitura format n zona central de ardere este caracterizat att
compoziional ct i morfologic, pentru a determina eventuale variaii sau gradieni de
concentraie elaborndu-se astfel mecanismul de formare al lipiturii.

The quality of refractories used in rotary clinker kilns is an important factor in the efficient
and safe operation. Basic refractories are a sensitive subject with major impact on
production costs; they are extensively researched in order to develop new innovative
products with long lifetime. Also, in present the corrosion is more intense due to current
trend to replace a higher rate of primary fuel (i.e. coal) with different alternative fuels.
MgO based refractory bricks are used successfully in both the cement and lime industry,
having an upstanding thermal stability and good chemical stability.
This paper investigates the refractory bricks from the central burning zone after the running
1,700 hours in a clinker kiln with a capacity of 3000 tons per day.
Heavily corroded brick after a short period of use was analyzed using scanning electron
microscopy techniques, associated with energy dispersive X-ray analysis (EDX) and X-ray
diffraction analysis and compared to new brick samples. In the same time was analyzed
the composition of melted coating formed on the refractory surface.
The kiln melted coating formed in the central burning zone is characterized both from
compositional and morphological view point to determine any changes or concentration
gradients for identifying its formation mechanism.
86
EVALUAREA NANO-PULBERILOR DE HIDROXIAPATIT OBINUTE IN
CONDIII DE LABORATOR, PENTRU NDEPRTAREA IONILOR DE
PLUMB DIN SOLUIILE LOR APOASE
EVALUATION OF LAB SCALE NANO-HYDROXYAPATITES FOR
LEAD IONS REMOVAL FROM AQUEOUS SOLUTIONS
Christu rdei1, Claudia Maria Simonescu2, Cristian Onose2, Bogdan Alexandru Sava3*,
Lucica Boroica3, Dorinel Tlpeanu1, Gabriela Sbrcea1

1 Institutul Naional de Cercetare-Dezvoltare pentru Inginerie Electric, ICPE-CA,


Bucureti, Romnia
2 Universitatea Politehnica din Bucureti, Facultatea de Chimie Aplicat i tiina

Materialelor, Bucureti, Romnia


3 Institutul Naional pentru Fizica Laserilor, Plasmei i Radiaiei, Mgurele, Romnia

Scopul acestui studiu a constat in stabilirea influenei condiiilor de preparare asupra


nanopulberilor de hidroxiapatit (n-HAP) elaborate in condiii de laborator prin reacii de
precipitare i metode sol-gel si de asemenea, a corelaiilor principalelor caracteristici
precum cristalinitatea si suprafaa specific cu capacitatea lor de a retine ioni de metale
grele (Pb2+). S-a testat mbuntirea capacitii de reinere a Pb2+ din soluiile sintetice
apoase prin adaosul de dispersant (0.11.5%) si respectiv, prin substituii izomorfe (Six-
HAP, x=0.5; 1). Experimentele au fost realizate in regim discontinuu utiliznd diferite
pulberi n-HAP, si au fost testate comparativ pentru ndeprtarea ionilor Pb2+ din soluiile lor
apoase, in condiii diferite precum concentraia iniial a ionilor metalici si pH-ul soluiilor.

Rezultatele au demonstrat ca pulberile n-HAP obinute prin precipitare au ca unic faz


compusul HAP in schimb, nanopulberile obinute prin procese sol-gel prezint i cantiti
minore de -TCP; testele au demonstrat ca ndeprtare a ionilor metalici se coreleaz cu
natura adsorbantului (morfologie i suprafa specific) i concentraia iniial in ioni
metalici din soluiile lor apoase.

Mulumiri: Studiul a fost finanat de Ministerul Educaiei Naionale (MENUEFISCDI), Program Parteneriate
n Domenii Prioritare, prin proiectele PN-II-PT-PCCA, Contract Nr. 92/2014, i M-ERA.NET, Contract Nr. 7-
081/2013, MAGPHOGLAS.

This study aimed to investigate the effect of preparation conditions on different


hydroxyapatite nanopowders (n-HAP), obtained on the laboratory scale, by the solution
precipitation and sol-gel methods, and to correlate the main characteristics like crystallinity
and specific surface area with the ion Pb2+ immobilization capacity. It is tested the
increasing performance of nano-HAP so obtained, to remove heavy metals from aqueous
solutions through dispersant addition (0.11.5%) and isomorphic substitution (Six-HAP,
x=0.5; 1). Batch experiments were carried out using different synthetic nano-
hydroxyapatites; powders were comparatively tested for lead removal process from
aqueous solutions, under different conditions, i.e. initial metal ion concentration, and pH of
the solutions.
87
Results showed that all HAP powders obtained by precipitation contain hydroxyapatite as
the only crystalline phase instead, the sol-gel HAP powders contains minor quantities of -
TCP. Experimental results shown that, the amount of metal ions (Pb2+) removed correlates
to the nature of the adsorbents (morphology and specific surface area), and to the
concentration of the synthetic solution in metallic ions.

Keywords: nano crystalline hydroxyapatite, heavy metals, lead removal, adsorption

Acknowledgements: The research was financed by the Ministry of National EducationExecutive Unit for
Financing Higher Education, Research and Development and Innovation (MENUEFISCDI) in the
PARTNERSHIP, through projects PN-II-PT-PCCA, Contract No. 92/2014 and M-ERA.NET, Contract No. 7-
081/2013 MAGPHOGLAS.

88
HIDROXIAPATIT SUBSTITUIT CU MAGNEZIU I SILICE
PENTRU APLICAII MEDICALE
MAGNESIUM AND SILICON SUBSTITUTION OF HYDROXYAPATITE
FOR MEDICAL APPLICATION
Costel Cristian Ion, tefania Stoleriu
Universitatea Politehnica din Bucureti

Biocompatibilitatea hidroxiapatitei poate fi mbuntit prin dopare cu magneziu i silice.


Astfel, a fost studiat hidroxiapatita dopat cu magneziu i silice, obinut prin precipitare.
Nanopulberile au fost obinute prin precipitarea precursorilor Ca(NO3)4H2O, orto-H3PO4
(85%), TEOS, Mg(NO3)6H2O i H2O. Nanopulberile au fost caracterizate prin tehnici
specifice, precum: difracia de raze X, microscopie electronic de transmisie, analize
termice i spectroscopie FT-IR. Pentru ca probele sinterizate s conin o anumit
porozitate deschis, nanopulberile au fost amestecate cu glucoz. Corpurile ceramice
crude, obinute prin presare uniaxial, au fost tratate termic la 650, 900 i 1100C, timp
de 2 ore.

Microstructura i compoziia fazal a probelor sinterizate au fost evaluate prin microscopie


electronic de baleiaj i prin difracie de raze X. Vibraiile legturilor chimice au fost
studiate prin spectroscopie FT-IR. Biocompatibilitatea ceramicilor obinute a fost estimat
prin teste de proliferare celular (teste MTT).

The biocompatibility of hydroxyapatite ceramics can be improved by substitution of


constituent atoms with magnesium and silicon. Thus, the magnesium and silicon
substituted hydroxyapatite, obtained by co-precipitation route, were studied.

The nanopowders were obtained through precipitation route from Ca(NO3)4H2O, ortho-
H3PO4 (85%), TEOS, Mg(NO3)6H2O and H2O. The nanopowders were characterized by
specific techniques such as: X-ray diffraction analysis, transmission electronic microscopy,
thermal analysis and FT-IR. To induce porosity to the sintered samples, the nanopowders
were mixed with glucose. The green bodies, obtained by uniaxial pressing, were thermally
treated at 650, 900 and 1100C, for 2 hours.

The microstructure and phase composition of the sintered ceramics were evaluated
through scanning electron microscopy and X-ray diffraction analysis. The chemical bonding
vibrations were study with FT-IR analysis. Also, the biocompatibility of obtained ceramics
was analyzed by cell proliferation (MTT assay).

89
INFLUENA SULFOALUMINATULUI DE CALCIU ASUPRA
PROPRIETILOR LIANTE ALE COMPUILOR NALT REFRACTARI
DIN CIMENTURILE SUPERALUMINOASE
THE INFLUENCE OF CALCIUM SULPHOALUMINATE ON BINDER
PROPERTIES OF THE HIGH REFRACTORY MINERALOGICAL
COMPOUNDS FROM HIGH ALUMINA CEMENTS
Cristina Stancu
Ceprocim S.A.,Bucureti, Romnia

n utilizarea practic a cimenturilor superaluminoase este foarte important ca acestea s


prezinte proprieti fizico-mecanice bune att la temperatur normal (dupa hidratare) ct i
la temperatura de lucru (temperatur ridicat).

Compoziia mineralogic a cimentului superaluminos este factorul principal care


guverneaz proprietile fizico-mecanice la temperaturi ridicate i, prin urmare este benefic
ca cimentul superaluminos s conin faze mineralogice cu refractaritate ridicat.

Scopul acestei lucrri este acela de a proiecta i caracteriza diferite cimenturi


superaluminoase ce conin compuii mineralogici cu refractaritatea cea mai ridicat din
sistemul binar CaO-Al2O3, ca de exemplu dialuminatul monocalcic CA2 si hexa aluminatul
monocalcic - CA6; i de a prezenta influena pe care utilizarea unui aditiv accelerator, n
cazul de fa a sulfoaluminatului de calciu, o poate avea asupra mbuntirii hidratrii
fazelor mineralogice din cimenturile superaluminoase proiectate, fr a diminua ns
performana lor refractar.

Pentru realizarea acestui deziderat, cimenturile superaluminoase proiectate trebuie s


prezinte proprieti fizico-mecanice mai bune dect cele ale unui ciment superaluminos
uzual, utilizat n prezent pentru aplicaile industriale pe scar larg, cu o compoziie
mineralogic bazat pe monoaluminat monocalcic - CA i dialuminatul monocalcic CA2.

Cuvinte cheie: Ciment superaluminos, compui mineralogici nalt refractari, monoaluminat


monocalcic, dialuminat monocalcic, hexa aluminat monocalcic.

In practice is very important that the high alumina cement used to present both good
physical and mechanical properties at normal temperature (after hydration) and at work
temperature (high temperature).

The mineralogical composition of the high alumina cement is an important factor that
governing the physical and mechanical properties at high temperatures and hence is
beneficial for the high alumina cement to contain high refractory mineralogical compounds.

The purpose of this paper is to design and characterize different high alumina cements
containing the highest refractory mineralogical compounds from the binary system Al2O3-
90
CaO, such like monocalcium dialuminate - CA2 and monocalcium hexa aluminate - CA6;
and to present the influence of using an additive accelerator, in this case the calcium
sulphoaluminate, that can improve the mineralogical phases hydration of high alumina
cements designed, but without diminishing their refractory performance.

To achieve this, the high alumina cements designed must present improve physical and
mechanical properties than those of a high alumina cement commonly used today for
industrial applications, with a mineralogical composition based on monocalcium
monoaluminate - CA and monocalcium dialuminate - CA2.

Keywords: high alumina cement, high refractory mineralogical compounds, monocalcium


monoaluminate, monocalcium dialuminate, monocalcium hexa aluminate.

91
POLIMORFISMUL PRINCIPALELOR FAZE ALE CLINCHERULUI DE
CIMENT PORTLAND RAPORTATE LA IONII STRINI
MAIN PORTLAND CEMENT CLINKER PHASES POLYMORPHISM
RELATED TO FOREIGN IONS
Daniela Nstac1, Luminia Predoan2, Cornel Munteanu2 , Victor Fruth2
1CEPROCIM S.A., Bucureti, Romnia
2 Institutul de Chimie Fizic Ilie Murgulescu al Academiei Romne, Bucureti, Romnia

Structura cristalin a principalelor faze ale clincherului, alit, belit, aluminat tricalcic i
aluminoferit de calciu, este practic influenat i de ncorporarea elementelor minore i n
urme. ncorporarea acestor elemente, de asemenea, depinde de viteza de ardere i
regimul de rcire, avnd n total un efect combinat asupra modificrilor reactivitii
clincherului. Diverse clinchere de laborator i principalele faze individuale ale clincherului
dopat cu Zn, Cd, Sn si P au fost obinute pentru acest studiu. S-au observat diferite forme
polimorfe ale alitului i belitului n funcie de cantitatea de ioni strini introdui n structura
cristalin. De asemenea, s-a observat formarea de noi faze. Difracia cu raze X (XRD) a
fost util n determinarea polimorfismului i identificarea de noi faze. Microscopia
electronic de baleiaj cuplat cu analiza spectroscopic cu dispersie a energiei razelor X
(SEM-EDS) a fost utilizat pentru caracterizarea chimic a principalelor faze ale
clincherului. Microscopia optic (OM) a fost utilizat pentru a evalua microstructura
clincherului. De asemenea, OM a fost util pentru a distinge diferitele tipuri de aluminat
tricalcic pe baza caracteristicilor cristaline. O metod grafic bazat pe sistemul de
coordonate polare este prezentat pentru a facilita vizualizarea coninutului n elemente
minore.
Mulumiri: Aceast lucrare a fost realizata prin programul Parteneriate in domenii prioritare
- PN II, derulat cu sprijinul MEN-UEFISCDI, proiect nr. 223/2014.

The crystalline structure of the main clinker phases, alite, belite, tricalcium aluminate and
calcium aluminoferrite, are basically influenced by the incorporation of minor and trace
elements. Incorporation of these elements is also a function of the burning regime and
cooling rate, altogether having a combined effect on the changes in the reactivity of clinker.
Various laboratory clinkers and individual main clinker phases doped with Zn, Cd, Sn and P
were obtained for this study. It was found different polymorphic forms of alite and belite
depending on the amount of foreign ions introduced in the crystalline structure. Also, new
phases formed were observed based on the previous consideration. X-ray diffraction
(XRD) was useful in polymorphism determination and new phases identification. The
scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-
EDS) analysis was used on the chemical characterization of the main clinker phases. The
optical microscopy (OM) was used to assess the clinker microstructure. Also, OM was
useful to distinguish the different kinds of tricalcium aluminate based on their crystal
features. A graphical method based on the polar coordinate system is presented to
facilitate the visualization of the trace element content.

92
SENZORI DE GAZE TOXICE I INFLAMABILE BAZAI PE
CAPACITOARE MOS PE SiC
TOXIC AND INFLAMMABLE GAS SENSORS BASED ON SiC
MOS CAPACITORS
Doru Vladimir Pucau1, Adriana Graiela Pribeanu1, Rzvan Pascu2, Florea Crciunoiu2
Gheorghe Brezeanu3, Florin Drghici3, Gheorghe Pristavu3, Gherghina Ciortan1
1 CEPROCIM S.A, Bucureti, Romnia
2 Institutul Naional pentru C&D n Microtechnologie, IMT- Bucureti, Romnia
3 Universitatea Politehnica din Bucureti, Romnia

Dezvoltarea dispozitivelor realizate pe semiconductori de band larg poate fi cheia ctre o


tehnologie eficient n realizarea unor aplicaii pentru medii ostile, cum ar fi: temperatura
ridicat, vibraii i medii corozive. nlocuirea sistemelor convenionale cu unele care au la
baz un semiconductor de band larg, aa cum este carbura de siliciu (SiC), poate duce
la ctiguri substaniale n ceea ce privete att fiabilitatea dispozitivelor, ct i costul de
fabricaie al acestora. Mai mult, un senzor de gaz fabricat pe SiC poate asigura un rspuns
mult mai rapid atunci cnd temperatura mediului n care se afl crete.

n aceast lucrare vom discuta despre realizarea i testarea unor capacitoare MOS pe SiC
ca senzori pentru diferite gaze inflamabile, cum ar fi H2 i CH4. Aadar, senzorii MOS au
fost fabricai pe plachete de politipul 4H-SiC, achiziionate de la Cree, avnd un strat
epitaxial cu o grosime de 8 m i o concentraie a purttorilor donori de 2.07 x 1016 cm-3.

Oxidul MOS a fost obinut prin oxidare uscat de O2 la o temperatur de 1100C, timp de 3
ore, obinndu-se o grosime a oxidului de aproximativ 30 nm. Electrozii de poarta ai
capacitoarelor MOS au fost obinui n urma depunerii unui film subire de Pd (50 nm) i au
o configuraie circular cu diametre de 200, 300 i 400 m. Pentru a realiza att padurile
structurilor MOS, ct i contactul ohmic, a fost depus un sandwich metalic format din Ti/Au
pe ambele fee ale plachetei. Dispozitivele test au fost trasate i ncapsulate n capsule de
tip TO39, utiliznd tehnologia lipirii cu fir de aur. Senzorii de gaz au fost caracterizai
electric prin obinerea de caracteristici C-V ncepnd cu temperatura camerei i pn la o
temperatur de 200C. Toate aceste msurtori electrice s-au realizat ntr-o incint n care
se poate controla precis concentraia gazului. Performanele capacitoarelor MOS pe SiC
au fost testate la o concentraie fix de H2, respectiv CH4 la temperaturi diferite de
msur, observndu-se o tendin de cretere a rspunsului senzorului cu temperatura de
msur.

The development of devices based on wide band gap semiconductors could be the key to
an efficient technology for applications in hostile environments such as high temperature,
vibration and corrosive environments. Replacing conventional systems with some which
are based on a wide band gap semiconductor, such as silicon carbide (SiC), can leads to
substantial gains regarding the both reliability and fabrication costs. Moreover, a gas
sensor fabricated on SiC can provide a more rapid response with temperature increasing.
93
In this paper MOS capacitors based on SiC have been fabricated and tested for hydrogen
and CH4 sensing applications.
Therefore, the MOS sensors have been fabricated on n type 4H-SiC wafers from Cree,
with an 8 m epitaxial layer having a nominal doping of 2.07 x 1016 cm-3. The samples
were oxidized at 1100C in dry oxygen for 3h, being obtained a thickness of 30 nm,
determined by capacitance voltage (C-V) characteristics.

Circular dots of palladium, nominally 50 nm thick, were defined using photolithographic


mask with diameter of 200, 300 and 400 m. In order to obtain the both pads contact and
ohmic contact, a Ti/Au stack has been deposited on both wafer sides. The test samples
have been packaged in TO 39 case, using wire bonding technology. The gas sensors
based on SiC MOS capacitors have been electrical characterized via C-V measurements,
starting from room temperature up to 200C in a chamber with a controlled gas
atmosphere. The H2 detection performance of the Pd gate MOS sensor was determined by
analyzing the C-V characteristics measured on the encapsulated samples. The sensor
responsivity substantially increases with temperature up to 200C.

Acknowledgments. The work has been funded by the national Program PN2, contract no.
204/2012.

94
MORFOLOGIA I COMPOZIIA MICROSFERELOR ANORGANICE
UTILIZATE N MORTARE
MORPHOLOGY AND COMPOSITION OF INORGANIC
MICROSPHERES USED IN THERMO INSULATING MORTARS
Georgeta Velciu1, Virgil Marinescu1,4, Christu rdei1, Gabriela Sbrcea1,
Adriana Moan2, Mirela Menicu2, Constantin Dorinel Voinichi3, Gheorghe Ghe.Ioni4

1Institutul Naional de Cercetare-Dezvoltare pentru Inginerie Electric ICPE-CA,


Bucureti, Romnia
2 CEPROCIM SA, Bucureti, Romnia
3 Universitatea Tehnic de Construcii Bucureti, Romnia
4Universitatea Valahia din Trgovite, Romnia

n aceast lucrare sunt prezentate caracteristicile structurale i microstructurale ale


microsferelor ceramice de sintez i a mcirosferelor anorganice cu caviate utilizate ca
filer n mortarele de construcii.

Microsferele au fost caracterizate microstructural prin SEM i EDX pentru determinarea


dimensiunilor i a compoziiei elementale. Microsferele ceramice au o compoziie
majoritar de Al2O3 iar dimensiunea microsferelor variaz ntre 18-30 m, iar grosimea
peretelui este mai mic de 10% din diametrul microsferelor. Microsferele din cenua de
termocentral cu cavitate au o compoziie majoritar alumino-silicatic, iar diametrul
microsferelor variaz ntre 1 i 5 m. Caracterizarea structural i microstructural a
microsferelor ne permite evaluarea utilizrii lor n scopul obinerii unor mortare cu
proprieti termoizolatoare.

In this paper are presented micro-structural characteristics of synthesized ceramic


microspheres and cavity inorganic microspheres used in thermo-insulation plasters and
mortars, construction materials.

Microspheres were micro and structural investigated by Scanning Electron Microscopy


(SEM) and Energy Dispersive Spectra (EDS) to determine dimensions and elemental
composition of them. Ceramic microspheres have a majority composition of -Al2O3
compound and their dimensions vary between 18-30 m the wall thick is 10% lower than
all diameter of obtained microspheres. Coal plant cavity microspheres have a general
composition made by aluminums- silicates compounds and their diameters vary in the
range of 1 and 5 m. Micro and structural investigations of these microspheres will permit
us to evaluate these materials like potential candidates for obtaining thermo-insulation
plasters and mortars used in the construction domains.

95
METODOLOGII DE OPTIMIZARE A PROCESELOR ANALITICE
MODELUL MATEMATIC AL SISTEMULUI OPTIMIZAT
METHODOLOGIES OF OPTIMIZATION FOR ANALYTICAL PROCESSES
MATHEMATIC MODEL OF OPTIMIZED SYSTEM
Gherghina Ciortan
CEPROCIM S.A, Bucureti, Romnia

Desfurarea proceselor analitice in laborator poate avea anumite performane tehnice i


economice, funcie de alegerea parametrilor sistemului, condiiile si modul de lucru.
Alegerea cea mai bun a parametrilor de reacie se face cu ajutorul unei metode de
optimizare adecvat. Orice metod de optimizare presupune gsirea funciei obiectiv i
a funciei restrictive.
Funcia obiectiv este exprimarea matematic a influenei cantitative a celor mai
semnificativi parametri asupra caracteristicii de calitate a sistemului de reacie.
Funcia restrictiv este funcia ce delimiteaz domeniul de variaie admis pentru funcia
obiectiv si parametrii sistemului de reacie.
In concluzie, gsirea condiiilor optime de desfurare a unei reacii chimice este aadar,
gsirea condiiilor corespunztoare maximului sau minimului funciei obiectiv, care trebuie
bine studiat cu ajutorul metodelor de optimizare analitic sau alfanumerice.

n practic, problemele de optimizare pot fi rezolvate cu ajutorul metodelor statistice ale


experimentului factorial i analiza de dispersie. Un sistem analitic cu funcie de detecie,
identificare sau determinare este un lan informaional la intrarea cruia se gsete
materialul de analizat (proba), iar la ieire rezultatul de analiz. Sistemul analitic poate fi
uor descompus in urmtoarele subsisteme: eantionarea probei, tratamentul fizico-chimic
al eantionului, msurarea semnalului analitic, prelucrarea semnalelor i in final calculul
rezultatelor. n general, in analiza chimic se optimizeaz individual aceste subsisteme sau
elemente ale lor.
Lucrarea prezent urmrete s evidenieze si s prezinte o prima etap n procesul de
optimizare, de alegere a caracteristicilor de performan tehnice (precizia,
corectitudinea, selectivitatea i rezoluia, limita de detecie, limita de cuantificare).

The development of analytical processes in laboratory may have certain technical and
economical performances, depending on choosing of system parameters, the conditions
and the way of working. Choosing of the best parameters of reaction is made with aid of an
adequate method of optimization. Any method of optimization supposes the finding of
objective and of restrictive function.

Objective function is mathematical expressing of quantitative influence of the most


significant parameters on the characteristic of quality of the system of reaction.

96
Restrictive function is the function that delimitate the range of variation admitted for
objective function and the parameters of reaction system.

In conclusion, founding of optimum conditions of development of a chemical reaction is


therefore, founding of corresponding conditions of the maximum and minimum of objective
function, which must be well studied with aid of the methods of analytical optimization or
alpha-numerical.

In practice, the problems of optimization may be solved with aid of statistical methods of
factorial experiment and analyze of dispersion. An analytical system with function of
detection, identification or determination is an informational chain at its inlet is found the
material of analyzing (sample), ant at outlet the result of analyze. Analytical system may be
easy decomposed in the following sub-systems: sampling of the assay, physical-chemical
treatment of the sample, measuring of analytical signal, processing of the signals and
finally the calculation of the results. Generally, in chemical analyze these sub-systems or
elements of them are individually optimized.

Present paper, follows to accentuate and to present a first stage of optimization, of


choosing the characteristics of technical performance (accuracy, correctitude,
selectivity and resolution, limit of detection, limit of quantification).

97
IMPACT OF THE RIVER AGGREGATE PARTICLE SIZE DISTRIBUTION
ON THE QUANTITY OF CEMENT AND ADMIXTURES REQUIRED FOR
MAKING OF CONCRETE MIXES OF THE SAME PROPERTIES
Gordana Toplii-uri, Duan Grdi, Nenad Risti, Zoran Grdi
University of Nis, The Faculty of Civil Engineering and Architecture Nis, Serbia

The share of aggregate in concrete composition, in terms of volume is 70%-80%. The


properties of fresh and hardened concrete depend on the aggregate properties, primarily
on particle size distribution. The paper considered impact of particle size distribution of
aggregates from two screening plants from the South Morava river on the properties of
concrete. The intention was to make concrete mixtures with the aggregate which would
have as identical particle size distribution, as similar consistency of fresh concrete as
possible and same compressive strengths. For making of afore mentioned concrete mixes,
the same sort of cement and same admixtures were used.

It was concluded that the difference in the particle size distribution of aggregate fractions
had an impact on the composition of concrete mixes of the identical properties. Specifically,
the quantities of cement, admixtures and water were different in the afore mentioned
mixtures.

The technical specifications of the cement manufacturers include a recommended quantity


of cement for specified concrete classes. It is concluded that these values are only rough
guidelines. The same holds for the recommended quantities of admixtures. For that
reason, every required concrete mixture must be verified in laboratory, i.e., previously
tested.
Key words: river aggregate, particle size distribution, cement, admixture, concrete

98
ASPECTE DE MEDIU LA STABILIZAREA ZGURILOR METALURGICE (LF)
UTILIZATE N AGRICULTURA SUSTENABIL
ENVIRONMENTAL ASPECTS IF THE USE OF STABILISED
METALURGICAL LADDL FURNACE (LF) SLAGS IN SUSTAINABLE
AGRICULTURE
Lavinia Gabriela Popescu1, Eniko Volceanov1,2, Florian Zaman1
Valerica Slavescu1, Ildiko Anger 3, Ecaterina Matei2
1 Institutul de Cercetri Metalurgice- ICEM, Bucureti, Romnia
2 Universitatea Politehnica din Bucureti, Romnia
3 Institutul Naional de Cercetare-Dezvoltare pentru Metale Neferoase i Rare, Romnia

Cuvinte cheie: pelete, zgur LF, levigabilitate, granulometrie


Lucrarea prezint o evaluare a factorilor de mediu la utilizarea zgurilor albe LF sub forma
de pelete. Au fost efectuate teste de levigabilitate i analiz chimic a acestora prin diverse
metode, comparativ cu zgurile sub form de pulbere de la 2 surse din industria
metalurgic.

Compoziia chimic a levigatului rezultat pentru diferite fracii granulometrice ale deeului
de zgur LF a fost determinat cu ajutorul spectrometriei de absorbie atomic, n special
pentru determinarea concentraiei de metale grele, antrenate din zgur. De asemenea, a
fost investigat evoluia pH-ului i conductibilitii electrice pe probele de levigat, preparate
la raportul solid/lichid de 1:2 i 1:10.

Avantajul folosirii zgurilor LF sub forma de pelete const n reducerea instabilitii zgurii LF
(zgura cu caracter prfos - fapt ce duce la dispersia prafului in mediul nconjurtor). Acest
lucru este posibil prin prelucrarea la o granulaie optim, care conduce la obinerea unui
produs mai omogen i din punct de vedere al caracteristicilor fizico-chimice pentru a putea
fi utilizat ca amendament al solurilor acide in agricultur.

Keywords: pellets, LF slag, leachability, grain size distribution


This paper presents a comparative assessment of environmental factors by using an
industrial waste from secondary metallurgy, such as white slag. It were investigated LF
slags generated at two sources as powder and subsequently as pelletized form. The
chemical composition of the investigated slags were analysed by x-Ray Flurorescence
(XRF).

Leachability tests were carried out and the chemical analysis thereof by various methods.
Consequently, the chemical composition of the leachate for various particle size fractions
of the waste LF slag was determined by using atomic absorption spectrometry, in particular
for determining the concentration of heavy metals brought by slag.

99
Also, it was investigated the evolution of pH and electrical conductivity on leachate
samples, prepared to solid / liquid ratio of 1: 2 and 1:10.

The advantage of using LF slag as pellets consist on decreasing the LF slag instability,
comparatively with the initial powdered slags, which leads to dispersion of dust in the
environment. This is possible by processing the slags to an optimal grain size distribution
and also physical and chemical characteristics of a more homogeneous product. Their use
as acid soil amendment in agriculture is effective.

100
EVOLUIA EMISIILOR DE METALE GRELE DIN FABRICILE DE CIMENT
IN ANII 2014 I 2015 N RAPORT CU LIMITRILE LEGII
THE EVOLUTION OF HEAVY METALS EMISSIONS FROM
CEMENT PLANTS IN THE YEARS 2014 AND 2015
IN RELATION TO LIMITATION OF LAW
Marina Martin
CEPROCIM S.A., Bucureti, Romnia

Legea nr. 278 din 24.10.2011, stabilete cadrul general pentru prevenirea i controlul
polurii, pentru toate fabricile care incinereaz deeuri, printre care se afl i industria
cimentului i care trebuie s limiteze emisiile de poluani din fabricile de incinerare.

Aceast lucrare evideniaz evoluia emisiilor de metale grele din trei fabrici de ciment din
Romnia n perioada 2014-2015.
n lucrare se prezint parametrii tehnici de metode, reactivii, aparatura i modul de lucru
care s-au utilizat n determinarea metalelor grele din emisii.

Cuvinte cheie: metale grele, emisii, deeuri, industria cimentului

Law no. 278 from 24.10. 2011 establishes the general framework for pollution prevention
and control for all plants incinerating waste, including cement industry, and which must limit
emissions of pollutants from incineration plants.

This paper highlights the evolution of heavy metals emissions in three deferent plants of
cement from Romania in the period 2014-2015.
Also the paper presents the technical parameters of methods, reagents, equipment and the
procedure which have been used in determination of heavy metals emissions.

Key words: heavz metals, emissions, waste, cement industry

101
INERTIZAREA UNUI DEEU INDUSTRIAL CU CONINUT DE CROM
NTR-O MATRICE LIANT ANORGANIC
INERTIZATION OF AN INDUSTRIAL WASTE CONTAINING CHROMIUM IN
A INORGANIC BINDER MATRIX
Marius Prvan, Carmen Oproiu, Georgeta Voicu, Alina Bdnoiu, Roxana Truc,
Simina tefan
Universitatea Politehnic din Bucureti, Romnia

n prezenta lucrare s-a cercetat posibilitatea inertizrii unui deeu industrial rezultat n
industria de obinere a bicromatului de potasiu, avnd coninut de crom.

Deeul a fost dozat astfel nct concentraia cromului n masa liant s fie de 0,5 i 1%,
fiind utilizate dou tipuri de cimenturi CEM II/A-L (LL) i CEM II/A-M (S-LL) 42.5R.
Rezistenele mecanice la compresiune a cimenturilor compozite cu i fr coninut de
deeu au fost realizate pe mortare plastice (raport ap:liant=1:2 i raport liant:agregat =
1:3), turnate n matrie prismatice (15x15x60 mm3), ntrite 7-90 zile.

Pentru punerea n eviden a proceselor de interacie care au loc n astfel de mase, au fost
preparate paste liante cu raport ap: liant = 0,5, ntrite 3-90 zile. Procesele de interacie
au fost studiate prin utilizarea difraciei de raze X (DRX), spectroscopiei FT-IR (FT-IR) i
analizei termice complexe (ATD-TG). Caracteristicile microstructurale au fost puse n
eviden prin microscopie electronic de baleiaj (MEB).

De asemenea au fost realizate teste de levigare pe pastele ntrite 28 zile, utilizndu-se


pentru determinarea concentraia de crom n levigat (SR EN 12457-4:2003) prin
spectroscopie de emisie optic n plasm cuplat inductiv (ICP OES).

Din cercetrile realizate a rezultat c un astfel de deeu nu afecteaz important


rezistenele mecanice la compresiune. n plus, inertizarea cromului n pastele liante se
realizeaz prin formarea unor sruri greu solubile, prin substituia de cationi din
hidrocompui, n special din hidrosulfat aluminai de calciu (AFm, AFt).

Mulumiri:
Aceast cercetare a fost parial susinut financiar de Programul Operaional Sectorial Dezvoltarea
Resurselor Umane 2007-2013, finanat de Fondul Social European i de Guvernul Romniei, sub
numrul de contract POSDRU / 156 / 1.2 / G / 135764 " mbuntirea i implementarea de programe
universitare de master n domeniul Chimiei Aplicate i tiinei Materialelor ChimMaster.
Analizele de difracie cu raze X au fost posibile datorit Programului Operaional Sectorial de Dezvoltare
a Resurselor Umane, finanat din Fondul Social European i de Guvernul Romniei, sub numrul de
contract POSDRU / 86 / 1.2 / S / 58146 (MASTERMAT). De asemenea, analizele de microscopie
electronic de baleiaj au fost posibile datorit proiectului cu finanare i de la UE- POSCCE-A2-O2.2.1-
2013-1 / Prioritar Axa 2, Proiectul Nr 638 / 12.03.2014, ID-ul 1970, SMIS- cod 48652 CSNR.

102
The inertization of an industrial waste, with high chromium content, from the manufacture
of potassium dichromate, was investigated in this study.

The waste dosage in the cementitios mixture corresponds to of 0.5% and 1% Cr with
reference to binder. Two types of cement - CEM I 42.5 and CEM II/A-M (S-LL) 42.5R were
used as binding agents.

The compressive strengths of cementitious composites with/without waste content, were


assessed on plastic mortars (water:binder = 1:2 ratio and binder:aggregate = 1:3 ratio),
cast in prismatic molds (15x15x60 mm3), hardened different periods of time comprised
between 7 to 90 days.

The interaction processes which occur in the cementitious systems with/without waste
content were assessed on pastes with water to binder ratio equal to 0.5, hardened for 3 up
to 90 days. X-ray diffraction (XRD), infrared spectroscopy (FT-IR) and complex thermal
analysis (DTA-TG) were used for the pastes characterization. The microstructure of mortar
specimens was assessed by scanning electron microscopy (SEM).

In order to assess the leachability of chromium from these cementitious composites,


leaching tests (SR EN 12457-4:2003) were performed on the paste specimens hardened
for 28 days. The concentration of chromium in leachates, was determined by inductively
coupled plasma optical emission spectrometry (ICP-OES).

The obtained experimental data showed a reduced influence of this waste on the
compressive strengths values of cementitious composites. Moreover, in the cementitious
paste the inertization of chromium occurred due to the formation of insoluble salts or by the
substitution of cations from hydrates, in particular calcium aluminates sulphate hydrates
(AFm, AFt).

Acknowledgements:
This research was partially financially supported by Sectoral Operational Programme Human Resources
Development 2007-2013, financed by the European Social Fund and by the Romanian Government
under the contract number POSDRU/156/1.2/G/135764 Improvement and Implementation of
Universitary Master Programs in the Field of Applied Chemistry and Materials Science ChimMaster.
The X-ray diffraction analyses were possible due Sectoral Operational Programme Human Resources
Development, financed from the European Social Fund and by the Romanian Government under the
contract number POSDRU/86/1.2/S/58146 (MASTERMAT). Also, the electron microscopy
analyzes/images obtained on the samples were possible due to EU-funding project POSCCE-A2-
O2.2.1-2013-1/Prioritary Axe 2, Project No. 638/12.03.2014, ID 1970, SMIS-CSNR code 48652.

103
CARACTERIZAREA FIZICO-MORFOLOGIC A UNOR VITROCERAMICI
DIN DEEURI DE STICL CRT
PHYSICAL AND MORPHOLOGICAL CHARACTERISATION OF SOME
GLASS-CERAMICS FROM CRT GLASS WASTES
Mihai Eftimie, Alina Melinescu, Eduard Marinescu
Universitatea Politehnica din Bucureti, Romnia

Experimentele noastre privind recuperarea deeurilor de sticl rezultate din tuburile


catodice - CRT s-au concentrat asupra proiectrii compoziiilor de vitroceramic din
deeuri de sticl, cu posibile aplicaii n materiale compozite. Reetele au fost calculate
folosind ct mai mult deeu posibil, utiliznd diveri ageni de nucleaie i procente
variabile. Raportul sticla CRT folosit pentru componentele gt:plnie:panou au fost
5:30:65%, identice cu cele din CRT. S-au determinat urmtoarele proprieti fizice i
morfologice: densitate, porozitate, dilatare termic, stabilitate hidrolitic. Pentru a
caracteriza din punct de vedere compoziional i microstructural, analizele au fost efectuate
prin msurtori de difracie de raze X i microscopie electronic de baleiaj, care arat
influena agentului de nucleaie i temperaturii de tratament termic asupra proprietilor
vitroceramicii.

Our experiments on the recovery of the glass waste resulted from cathode ray tubes - CRT
were focused to designing compositions of glass-ceramic from glass waste with possible
applications in composite materials. The recipes were calculated using as much waste as
possible, using various nucleating agents and varying percentage. The report of CRT glass
used for the neck:funnel:panel components were 5:30:65%, identical to the ones in CRT.
We determined the following physical and morphological properties: density, porosity,
thermal expansion, hydrolytic stability. In order to characterize in terms of compositional
and microstructural, the analyses were carried out by X-ray diffraction and scanning
electron microscopy measurements, showing the influence of the nucleating agent and
thermal treatment temperature on the properties of the glass ceramics.

104
SYNTHESIS AND MAGNETIC PROPERTIES OF Mg DOPED ZnO THIN
FILMS: EXPERIMENTAL AND AB-INITIO STUDY
Mustapha Rouchdi1, El mehdi Salmani2, Abderrahim El hat1, Chourouk Nassiri1,
Adil Hadri1, Boubker Fares1 and Ahmed Mzerd1
1 Materials Physics Laboratory, Mohammed V University, Faculty of Sciences,

Rabat, Morocco
2 LMPHE, Mohammed V University, Faculty of Sciences, Rabat, Morocco

Structural and magnetic properties of Mg doped ZnO thin films and diluted magnetic
semiconductors have been investigated. This sample has been synthesized using a simple
spray pyrolysis. The hexagonal Wurtzite structured ZnO thin films were confirmed by X-ray
diffraction (XRD). The morphology of the thin films were characterized by atomic force
microscopy (AFM). The optical properties were studied in details by using UVvis and Hall
Effect measurements for electrical characteristic. The results obtained by AFM indicate
qualitative and quantitative way how the surface properties (topography, roughness) varies
with concentration. The optical characterization showed that the transmittance of MZO thin
films increased from 78 to about 90 % and optical band gap energy from 3.22 eV to 3.40
eV. The electrical study showed the lowest resistivity value was 3.45102 .cm, which
was obtained for the film doped with 2 .at% Mg.
In order to confirm our results the band structure of Wurtzite Zn1xMgxO is calculated by
abinitio calculations using the KorringaKohnRostoker method combined with the
coherent potential approximation (KKR), as well as coherent potential approximation CPA.
Keywords: ZnO, thin films, spray pyrolysis, optical properties, abinitio calculations.

105
CORELAII STRUCTUR BAZICITATE PROPRIETI PENTRU
STICLE DIN SISTEMUL Al2O3 NaPO3
STRUCTURE BASICITY PROPERTIES CORRELATIONS FOR
GLASSES FROM Al2O3 NaPO3 SYSTEM
Ovidiu Dumitrescu, Dorel Radu
Universitatea Politehnica din Bucureti, Facultatea de Chimie Aplicat i tiina
Materialelor, Dep. tiina i Ingineria Materialelor Oxidice i Nanomateriale, Bucureti,
Romnia

Sticlele alumino-fosfatice sunt ce n ce mai studiate mai ales datorit proprietilor lor
optice interesante. n consecin a crescut i volumul de informaii legat de structura
acestora.
Sticlele din sistemele alumino-fosfatice alcaline prezint o structur complex, datorit
posibilelor modificri ale numrului de coordinare aluminiu, n funcie de compoziia
efectiv. Acest lucru conduce la o evoluie interesant a proprietilor.
Au fost elaborate o serie de sticle definite de formula molar xAl2O3.(1-x)NaPO3 unde x=0;
2,5; 5; 7,5; 10; 12,5; 15; 20 i 25%. Pentru aceste sticle sintetizate a fost determinat
experimental curba de dilatare din care s-au extras temperatura tranziiei vitroase, Tg i
coeficientul de dilatare termic liniar, . De asemenea, s-a determinat experimental
bazicitatea definit prin ponderea bazicitii, pB.
Pe baza datelor de literatur MAS-RMN, s-a calculat ponderea aluminiului tetra, penta i
hexa coordinat. S-au obinut o serie de corelaii structur bazicitate proprieti care au
artat o bun concordan, ceea ce pare a valida modelul structural propus pe baza
msurtorilor de MAS-RMN.

Alumino-phosphate glasses are increasingly studied because of their particularly


interesting optical properties. As a result of these studies the volume of information related
to their structure has increased.
The glasses from the alkali alumino-phosphate systems present a complex structure, due
to the possible changes of the aluminium coordination number, as function of the actual
composition, resulting in an interesting evolution of the properties.
There were obtained a series of glasses having the molecular formula xAl2O3.(1-x)NaPO3
were x = 0; 2.5; 5; 7.5; 10; 12.5; 15; 20 and 25%. For these synthesized glasses were
determined experimentally the thermal expansion curves from which were extracted: the
vitreous transition temperature Tg and the coefficient of linear thermal expansion, . Also,
the basicity defined by the basicity index, pB has been experimentally determined.
On the basis of literature data MAS-NMR was calculated the concentration of tetra, penta
and hexa coordinated aluminum. There were obtained a series of correlations between the
(structure and basicity) oxide composition and the glass properties which seems to validate
the structural model proposed by the MAS-NMR measurements.

106
PROPRIETI MAGNETICE I MAGNETO-OPTICE ALE STICLEI
ALUMINOFOSFATICE DOPATE CU Bi I Pb
MAGNETIC AND MAGNETO-OPTICAL PROPERTIES OF Bi AND Pb-
DOPED ALUMINOPHOSPHATE GLASS
Raluca Iordnescu1, Mihail Elisa1, Cristina Vasiliu1, Bogdan Alexandru Sava2,
Lucica Boroica2, Mihaela Vleanu3, Victor Kuncser3, Adrian Volceanov4, Mihai Eftimie4,
Alina Melinescu4, Anca Beldiceanu5
1 Institutul Naional pentru Optoelectronic INOE 2000, Romnia
2Institutul Naional pentru Fizica Laserilor, Plasmei i Radiaiei, Romnia
3 Institutul Naional de Fizica Materialelor, Romnia
4 Universitatea Politehnic din Bucureti, Facultatea de Chimie Aplicat i tiina

Materialelor, Romnia
5 ProOptica S.A., Romnia

Sticla aluminofosfatic dopat cu Bi3+ si Pb3+ a fost obinut printr-o metod


neconvenional pe cale umed, plecnd de la formula molar 6LiPO3 3Al(PO3)3
1Ba(PO3)2 10Bi(PO3)3 80Pb(PO3)2.
Proba din sticl a fost investigat pentru a-i determina omogenitatea, densitatea,
coeficienii de dilatare termic, vscozitatea i stabilitatea hidrolitic.
Msurtorile magnetice pentru sticla fosfatic dopat cu Bi i Pb au pus in eviden un
comportament diamagnetic suprapus de un comportament paramagnetic ce ar putea fi
atribuit impuritilor prezente n matricea vitroas.
In ceea ce privete proprietile magneto-optice, constanta Verdet a sticlei dopat cu Bi i
Pb are valori pozitive, dovedind comportamentul diamagnetic al materialului studiat (Fig.
1), iar valorile relativ sczute ale acesteia pot fi explicate prin extragerea contribuiei
paramagnetice din valoarea final a constantei Verdet.
Autorii acestei lucrri sunt recunoscatori Unitii Executive pentru Finanarea Educaiei
Superioare, Cercetrii si Inovrii (UEFISCDI) pentru suportul financiar acordat in cadrul
proiectelor: nr. 186/2012 - Program Parteneriate, nr. 7-081/2013 - M-ERA.Net i nr. PN
16.40.01.02 OPTRONICA IV, din Programului Nucleu, sub suportul ANCS.
300 400 500 600 700 800

0,30
Sticla dopata cu Bi-Pb
0,10
0,25
Transmitanta (%) 100

0,20
V [min/(Oe cm)]

0,15
0,05

0,10

0,05

0,00
0,00

-0,05
300 400 500 600 700 800
Lungimea de unda [nm]

Fig.1. Constanta Verdet (V) i transmisia optic n funcie de lungimea de und a radiaiei
pentru sticla aluminofosfatic dopat cu Bi i Pb
107
Referine:
1. M. Valeanu, M. Sofronie, A. C. Galca, F. Tolea, M. Elisa, B. Sava, L. Boroica and V.
Kuncser, Relationship between magnetism and magneto-optical effects in new
aluminophosphate glasses, in press, J. Phys. D, 2015
2. M. Sofronie, M. Elisa, B. A. Sava, L. Boroica, M. Valeanu, and V. Kuncser, Rapid
determination of Faraday rotation in optical glasses by means of secondary Faraday
modulator, Rev. Sci. Instrum., 86, pag. 053905-1, 053095-7, 2015

Bi3+ and Pb3+-doped aluminophosphate glass was obtained by unconventional wet method,
the molar formula of the glass being 6LiPO3 3Al(PO3)3 1Ba(PO3)2 10Bi(PO3)3 80Pb(PO3)2.
The glass samples were investigated to determine the homogeneity, the density, the
thermal expansion coefficients, the viscosity and the hydrolytic stability.
The magnetic measurements for Bi and Pb-doped phosphate glass revealed a diamagnetic
behavior overlaid by a paramagnetic behavior that can be attributed to the impurities
presented in the matrix.
Regarding the magneto-optical properties, the Verdet constant for the Bi and Pb-doped
glass appeared to have positive values proving a diamagnetic behavior of the investigated
material (Fig. 1), but its relatively low value may be explained by the subtraction of the
paramagnetic contribution to the Vedet constant.
300 400 500 600 700 800

0.30
Bi-Pb Glass
0.10
0.25

Transmittance (%)x100
V [min/(Oe cm)]

0.20

0.15
0.05

0.10

0.05

0.00
0.00

-0.05
300 400 500 600 700 800
Wavelength [nm]

Fig.1. Verdet constant (V) and transmittance versus radiation wavelength for Bi and
Pb-doped aluminophosphate glass
References:
1. M. Valeanu, M. Sofronie, A. C. Galca, F. Tolea, M. Elisa, B. Sava, L. Boroica and V.
Kuncser, Relationship between magnetism and magneto-optical effects in new
aluminophosphate glasses, in press, J. Phys. D, 2015
2. M. Sofronie, M. Elisa, B. A. Sava, L. Boroica, M. Valeanu, and V. Kuncser, Rapid
determination of Faraday rotation in optical glasses by means of secondary Faraday
modulator, Rev. Sci. Instrum., 86, pag. 053905-1, 053095-7, 2015

108
MINERALOGICAL COMPOSITION OF THE SEN INTERNAL BUILD-UP
Sneana Devi1, Mira Coci2
1 IMS Institute Belgrade, Belgrade, Serbia
2 University of Belgrade, Technical Faculty Bor, Serbia

The mineralogical composition of the internal build-up of the SEN (submerge entry nozzle)
is presented in this paper, which is formed in the continuous steel casting process. Two
methods were used for determining the mineralogical composition of build-up: optical
microscopy and X-ray diffraction method. Optical testing was carried out on the polarization
microscope for transmitted light - Jena pole (immersion preparations), and XRD was
performed on the X-ray diffractometer Kristaloslex 810. The spectrometer ARL 9800 IX-P
was used for determining the changes in chemical composition of the SEN wall, by zones,
namely, by the X-ray fluorescent spectrometry method. SEN is a part of the nozzle set that
is used for continuous steel casting. It is manufactured from the refractory material based
on the alumino-graphite, by the isostatic pressing method. The basic role of the SEN, in
continuous steel casting, is providing a uniform steel flow from the tundish into the
crystallizer and protecting steel from oxidation. During the casting process, the internal side
of the SEN wall is in contact with steel. Build-up is often formed on the internal side,
reducing the SEN orifice, steel flow and lifetime of the nozzles. The formation of build-up
on the internal side of the SEN is caused by the accumulation of Al2O3 and reactions of
Al2O3, that can occur as the steel deoxidation product, as the product of the secondary
steel oxidation by means of the air (reoxidation), through the formation of the crystallization
core, induced by temperature decrease near the SEN surface, but also as the product of
reaction between Al in molten steel and SiO2 from the SEN refractory material. The
processes occurring at the steel casting temperature (1550-1556C) enable the formation
of gas sub-oxides Al2O and SiO in the refractory material itself, diffunding through the
nozzle wall toward the channel surface, and then to the steel melt. On the surface of phase
limits and directly with it goes on the oxidation reaction of gas sub-oxides with oxygen from
the steel and the formation of Al2O3 .The formation of internal build-up is often the result of
combination of the stated processes. The internal build-up, presented in this paper, has
been formed not only by the effect of steel deoxidation and reoxidation process, but also
due to the appearance of internal erosion and diffusion that was going on in the SEN
refractory material. For the presentation of mineralogical composition of the internal build-
up of SEN, five build-ups were selected, formed at continuous casting of two steel grades.
Three build-ups were formed at carbon steel casting (A series) and two build-ups formed at
casting of the aluminum killed steel (B series).
The paper contributes to better understanding of the phenomenon of build-up formation,
because it shows the results of five tested internal build-ups of the SEN, changes in the
contact zone of the SEN wall with steel, but also the conditions and some technological
parameters that dominated in the process during the formation of the same.

Key words: SEN (submerge entry nozzle), refractory material, steel, build-up

109
DETERMINAREA GROSIMII STRATULUI DEZALCALINIZAT DE STICL I
A GRADULUI DE DEZALCALINIZARE PRIN METODA HF-SECIONRII
DETERMINATION OF THE THICKNESS OF DEALKALIZED LAYER OF
GLASS AND THE DEGREE OF DEALKALIZATION USING THE METHOD
OF THE SECTION ETCHING BY HF SOLUTION
Vasile aragov, Svetlana Raifura, Galina Curicheru
Universitatea de Stat Alecu Russo din Bli, Republica Moldova

Scopul lucrrii const n determinarea caracteristicii stratului dezalcalinizat de sticl prin


metoda HF-secionrii.
Obiectele investigaiilor au fost produsele industriale: ambalaj din sticl incolor
transparent (butelii, borcane, flacoane), butelii din sticl verde nchis i probe din sticl
de geam.

Esena metodei const n dizolvarea secionat a sticlei i analiza extractelor obinute dup
decapare. Metodica HF-secionrii a sticlelor industriale n literatur nu este descris.
Dezalcalinizarea produselor industriale din sticl a fost efectuat, utiliznd tratarea
termochimic cu reageni gazoi. n condiii de laborator i de producere pentru tratarea
probelor din sticl au fost folosite reagenii gazoi: difluordiclormetan, difluorclormetan,
dioxid de sulf i amestecuri de gaze. Regimurile de tratare a probelor n experimentele de
laborator sunt: temperatura de la 20 la 600 0, volumul reagentului gazos la tratare 15
l, durata 15 min. Regimurile principale ale tratrii produselor din sticl cu medii gazoase
n condiii de producere sunt: temperatura sticlei de la 500 la 700 0C, durata nu mai
mult de 1 s, partea de volum a gazului la produs (raportul volumului de gaz ctre
capacitatea buteliei sau borcanului) de la 0,1 la 10,0 %.

Pentru prima dat, cu ajutorul metodei secionrii cu HF, s-a efectuat analiza straturilor
superficiale ale sticlelor cu destinaie industrial pn la adncimea de 30 m i mai mult.
Rezultatele obinute demonstreaz c sticla industrial are o structur stratificat. Datele
privind HF-secionarea ne permit s apreciem orientativ caracterul i grosimea unor straturi
separate a sticlei.

Dezalcalinizarea sticlei de geam cu difluordiclormetanul i difluorclormetanul duce la o


schimbare n compoziia i structura stratului superficial la adncimea de 20-30 m.
Totodat se formeaz dou straturi cu proprieti diferite. Stratul de sus cu grosimea 1 m
se mbogete cu dioxid de siliciu, n rezultat, sporete microduritatea lui. Structura
stratului de jos cu grosimea de la 10 la 30 m este mai puin compact, dect cea a masei
de baz a sticlei. Rezultate asemntoare au fost obinute pentru ambalajul din sticl,
tratat cu reagenti gazoi.

110
This paper aims at determining the characteristics of dealkalized layer of glass using the
method of section etching with HF solution.
The objects of investigations were industrial glassware: containers of colorless glass
(bottles, jars and flasks), bottles of green glass and sheet glass samples.

The method consists in section dissolution of glass and analysis of extracts obtained after
etching. The method of section etching with HF solution of the industrial glasses is not
described in specialized literature. Dealkalization of industrial glassware has been carried
out, using thermochemical treatment with acid gases. Gaseous reagents:
difluorodichloromethane, difluorochloromethane, sulfur dioxide and mixtures of these gases
have been used for the treatment of glass samples in laboratory and manufacturing
conditions. Regimes of treatment of samples in laboratory experiments are the following:
temperature from 20 to 600 0, volume of gaseous reagent to the treatment 15 l,
duration 15 min. The main regimes of treatment of glassware with gaseous media in the
manufacturing conditions are: glass temperature from 500 to 700 0C, duration no more
than 1 s, volume fraction of gas on glassware (ratio of the volume of gas vs. capacity of the
bottle or jar) from 0,1 to 10,0 %.

For the first time, the surface layers of bottles for industrial purposes were analyzed to the
depth of 30 m, and more with the help of section etching of HF solution. The obtained
results demonstrate that industrial glass has a stratified structure. The data on the section
etching with HF solution allow us to estimate the preliminary nature and thickness of
separate glass layers.

Dealkalization of sheet glass with difluorodichloromethane and difluorochloromethane


changes the composition and structure of surface layer at the depth of 20-30 m. At the
same time, two layers are formed with different properties. The top layer with thickness of 1
m is enriched with silicon dioxide, as a result, its microhardness increases. The structure
of the bottom layer with the thickness from 10 to 30 m is less compact than that of the
bulk glass. Similar results were obtained for glass containers, treated with gaseous
reagents.

111
INTENSIFICAREA PROCESULUI DE DEZALCALINIZARE A
STICLELOR INDUSTRIALE CU GAZE ACIDE
INTENSIFICATION OF THE DEALKALIZATION PROCESS OF
INDUSTRIAL GLASSES WITH ACID GASES
Vasile aragov1, Gheorghe Duca2, Ion Burcovschi1
1 Universitatea de Stat Alecu Russo din Bli, Republica Moldova
2 Academia de tiine a Moldovei, Chiinu, Republica Moldova

O metod simpl i eficient de sporire a stabilitii chimice a suprafeei sticlelor


industriale este tratarea termochimic cu gaze acide. Esena acestei metode const n
extragerea cationilor de metale alcaline din stratul superficial al sticlei [1, 2].
Ca obiecte de cercetare au fost utilizate produse industriale din sticl cu destinaie diferit.

Experimentele s-au efectuat cu probe de sticl de geam, de ambalaj (butelii, borcane,


flacoane) din sticl incolor, verde i brun, disperstori de lumin din sticl incolor i
opac, vesel chimic de laborator i menaj, fiole din sticl medicinal. Pentru tratarea
sticlei pot fi utilizai oxizi de sulf, clorur de hidrogen, derivai halogenai ai hidrocarburilor i
ali reageni gazoi.

n rezultatul dezalcalinizrii crete stabilitatea chimic a sticlei de zeci de ori i are loc
mbuntirea proprietilor mecanice i a rezistenei termice. Dezavantajul principal al
tratrii termochimice cu reageni gazoi este grosimea mic a stratului dezalcalinizat al
sticlei. n dependen de regimul i condiiile de tratare termochimic grosimea stratului
dezalcalinizat la sticlele industriale este de la pri de m pn la 1 m.

Intensitatea dezalcalinizrii sticlelor industriale cu gaze acide a fost apreciat cu ajutorul


vitezei de extracie a cationilor de metale alcaline din stratul superficial al probei. Pentru
intensificarea procesului de dezalcalinizare a sticlelor industriale cu gaze acide au fost
utilizate urmtoarele ci: optimizarea regimurilor de tratare termochimic, determinarea
reagenilor gazoi mai eficieni n procesul de dezalcalinizare a sticlei din poziie
termodinamic, tratarea termochimic a sticlei cu reageni gazoi sub influena cmpurilor
electrice i magnetice. n baza experimentelor efectuate am obinut creterea de cteva ori
a vitezei de extracie a cationilor de metale alcaline din probele de sticl.

Referine
1. Verita M., Geotti-Bianchini F., De Riu. Surface analysis of internally treated dealkalized containers.
Fundamentals of Glass Science and Technology, 1997. P. 174-181.
2. Sharagov, V., Duca, G. Increasing physical and chemical properties of annealed hollow glassware as
well as of those stored and used. Romanian Journal of Materials. 2013, nr. 43 (2). P. 218-222.

112
Thermochemical treatment with acid gases is a simple and efficient method to increase the
chemical stability of the surface of industrial glasses. The essence of this method consists
in the extraction of alkali metal cations from the surface layer of glass [1, 2].

Industrial glass of different purposes served as objects of investigation. The experiments


were carried out on samples of sheet glass, containers (bottles, jars and flasks) of
colorless, green and brown glasses, illuminating glassware made from transparent
colorless and milk glasses, laboratory and assorted glassware, ampoules made from
medical glass. Sulfur oxides, hydrogen chloride, halogenated derivatives of hydrocarbons
and other gaseous reagents may be used for thermochemical treatment of glass.

As a result of dealkalization chemical resistance of glass increases by dozens of times,


mechanical properties and thermal resistance are improved. The main disadvantage of
thermochemical treatment with gaseous reagents is small thickness of the dealkalized
layer of glass. Depending on the regime and conditions of thermochemical treatment, the
thickness of dealkalized layer of industrial glasses varies from parts of m to 1 m.

The intensity of dealkalization of industrial glasses with acid gases was estimated with the
help of extraction rate of cations of alkaline metals from the surface layer of sample. To
intensify the process of dealkalization of industrial glasses with acid gases the following
ways have been used: optimization of regimes of thermochemical treatment, determination
of the most efficient gaseous reagents in the process of dealkalization of glass from the
thermodynamic position, the thermochemical treatment of glass with gaseous reagents
under the influence of electric and magnetic fields. Based on the performed experiments,
we obtained an increased rate of extraction of alkali metal cations from the samples of
glass.

References
1. Verita M., Geotti-Bianchini F., De Riu. Surface analysis of internally treated dealkalized containers.
Fundamentals of Glass Science and Technology, 1997. P. 174-181.
2. Sharagov, V., Duca, G. Increasing physical and chemical properties of annealed hollow glassware as well
as of those stored and used. Romanian Journal of Materials. 2013, nr. 43 (2). P. 218-222.

113
SINTEZA I CARACTERIZAREA COMPOZITELOR DE TIP
HIDROXIAPATIT - TITANAT DE BARIU PENTRU INGINERIA
TISULAR OSOAS
SYNTHESIS AND CHARACTERIZATION OF
HYDROXYAPATITE - BARIUM TITANATE COMPOSITES FOR
BONE TISSUE ENGINEERING
Victor Badea, Anamaria Puia, tefania Stoleriu
Universitatea Politehnica din Bucureti, Romnia

n domeniul biotehnologiei, este extrem de studiat obinerea de noi tipuri de implanturi


care accelereaz formarea i creterea esutului osos. Prezentul studiu este axat pe
sinteza i caracterizarea compozitelor de tip hidroxiapatit - titanat de bariu.

Compozite hidroxiapatit titanat de bariu, cu un raport masic de 9: 1, s-au obinut prin


mai multe rute, care au avut drept scop de a mbunti contactul dintre cele
dou componente. Intr-una din rute, prin metoda sol-gel s-a obinut nanopulberea de
titanat de bariu. Ulterior, hidroxiapatita a fost precipitat n suspensii stabilizate de titanat
de bariu calcinat sau doar uscat. n cealalt rut de obinere, ambele componente au fost
obinute prin metoda sol-gel i au fost amestecate mpreun nainte de gelificare. Gelul a
fost apoi uscat i calcinat.

Compoziia fazal i microstructura materialelor obinute au fost analizate folosind difracia


de raze X, microscopie electronic de baleiaj, microscopie electronic de transmisie i
difracia de electroni zona selectat.
Studiile in vitro au fost efectuate cu scopul de a studia biocompatibilitatea compozitelor.

Manufacturing new implants that accelerate the bone formation and growth is highly
studied in the field of biotechnology. This study is focused on the synthesis and
characterization of hydroxyapatite - barium titanate composites.

Hydroxyapatite - barium titanate composites, with a 9:1 mass ratio, were obtained through
several synthesis methods that were aimed to improve the contact between the
components. In one of the methods barium titanate nanoparticles were obtained through
sol-gel route. Afterwards hydroxyapatite was precipitated in stabilized suspensions of
calcined as well as dried gel of barium titanate particles. The precipitate was then washed,
dried and calcined. In other method, both components were obtained through sol-gel
methods and were mixed together prior to gelation. The gel was then dried and calcined in
order to obtain the composites.

The microstructure and phase composition of the studied materials were analyzed, using
X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and
selected area electron diffraction.
In vitro studies were carried out in order to study the biocompatibility of the composites.
114
CORELAII NTRE COMPOZIIE, CONDIIILE DE PROCESARE I
MICROSTRUCTURA CLINCHERULUI PORTLAND PRIN UTILIZAREA
ANALIZEI MULTIVARIATE

CORRELATIONS BETWEEN COMPOSITION, PROCESSING CONDITIONS


AND MICROSTRUCTURE OF PORTLAND CLINKER USING
MULTIVARIATE ANALYSIS
Zeno Ghizdve1, Daniela Nstac2, Mihai Eftimie1, Adrian Volceanov1
1Universitatea Politehnica din Bucureti, Romnia
2CEPROCIM S.A., Bucureti, Romnia

Analiza multivariat (MVA), pe o baz de date complex a fost realizat, cu scopul de a


observa corelaii ntre compoziie, condiiile de prelucrare i microstructur. Baza de date a
constat din analiza chimic a clincherului de ciment, informaii extrase din analiza de
imagine a microfotografiilor clincherului i parametri de proces nregistrai n timpul
procesului de clincherizare. Clincherul a fost sintetizat n diferite condiii n mediu industrial
(19 clinchere) sau n laborator (14 clinchere diferite n dou grupe). Analiza de imagine a
fiecrui clincher a fost realizat prin calcularea parametrilor de form, dimensiunii fractale
i a unui parametru derivat din entropia Shannon, denumit grad de uniformitate. Analiza a
fost fcut cu o abordare euristic. De asemenea, faza interstiial a clincherelor a fost
izolat i analizat prin valorile dimensiunii fractale.

Rezultatele MVA au identificat n mod clar parametrii de influen. n special, s-a constatat
c coninutul de CaO liber din clincher a influenat att compoziia i microstructura ct i
parametrii de proces ai lanului compoziie-condiii de procesare-microstructur. Prin
urmare, s-a concluzionat c CaO liber poate fi privit ca o legtur ntre condiiile de
laborator i parametrii industriali pentru nelegerea acestor corelaii. Este de ateptat ca
procedura utilizat aici s ajute la poziionarea unui clincher necunoscut, avnd n vedere
un set minim de rezultate de laborator, de exemplu, analiza fazelor principale. Procedura
dat n aceast lucrare poate fi folosit pe orice material, pe imagini de microscopie optic
sau SEM, cu ajustri foarte mici.

Aceasta lucrare a fost realizat prin programul Parteneriate n domenii prioritare - PN II,
derulat cu sprijinul MEN-UEFISCDI, proiect nr. 223/2014.

Multivariate Analysis (MVA) on a complex database has been performed, aiming to reveal
correlations between composition, processing conditions and microstructure. Database
consisted of cement clinker chemical analysis, information extracted from image analysis of
clinker micrographs and process parameters recorded on the clinkering plant were the
clinkers were obtained. Clinkers have been burned in various conditions in industrial
environments (19 clinkers) or in laboratory (14 different clinkers in two groups). Image

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analysis of each clinker has been made by computing Shape Parameters, Fractal
Dimension and a parameter derived from Shannon Entropy, called the Uniformity Degree.

Analysis has been made with a heuristic approach in mind. Also, interstitial phase of the
clinkers has been isolated and analyzed here by their Fractal Dimension values.
MVA results clearly identified the influential parameters on the database. Particularly, it
was found that the free CaO content in clinker was influential on both composition-
microstructure and process parameters blocks of the composition-processing conditions-
microstructure chain. Therefore, we concluded that the free CaO can be seen as a link
between laboratory and industrial parameters in understanding these correlations. It is
expected that the procedure used here can help to position an unknown clinker, given a
minimal set of laboratory results, on, for example, Principal Component Analysis plots, if a
relevant database was used in the analysis.

The procedure given in this paper can be used on any material, on optical microscopy or
SEM images, with very little adjustments.

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