International Journal of Mechanical Engineering and Technology (IJMET)

Volume 6, Issue 8, Aug 2015, pp. 126-138, Article ID: IJMET_06_08_012

Available online at
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ISSN Print: 0976-6340 and ISSN Online: 0976-6359
IAEME Publication
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EXPERIMENTAL INVESTIGATION OF
CREEP BEHAVIOUR OF ALUMINIUM
ALLOY (LM25) AND ZIRCONIUM DIOXIDE (ZRO2) PARTICULATE MMC
A. R. Sivaram
Assistant Professor, Department of Mechanical Engineering,
AMET University, Chennai, India.
K. Kris hnakumar
Assistant Professor, EGS Pillay Engineering college,
Nagapattinam, India.
Dr. R. Rajavel
Professor and HOD, Department of Mechanical Engineering,
AMET University, Chennai, India.
R. Sabarish
Assistant Professor, Dept. of Mechanical Engineering,
Bharath University, Chennai, India.
ABSTRACT
Aluminium metal matrix composites are one of the new materials used for
various applications due to their less cost and light weight. Creep is the
tendency of solid material to slowly move or deform permanently under the
influence of stresses when subjected to high temperatures for long duration of
time. So creep is one of the major considerations while analyzing the
materials which are used for high temperature for long durations. Creep
analysis of composite material has a wide scope of research. In this paper, an
Aluminum composite material is produced by mixing high strength low weight
material with zirconium di-oxide for different proportions (0%, 3%, 6%, and
9%) by using stir casting technique. In this paper experimental tests were
carried out to determine the creep strength for different proportions (0%, 3%,
6%,9%) of Zirconium-di-oxide with LM25 by creep testing machine. SEM and
microstructure analysis was also done to see the distribution and presence of
ZrO2 particles in aluminium alloy.

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

Key words: Composite material, Aluminium alloy composite, SEM, Elapsed

strain.
Cite this Article: Sivaram, A. R., Krishnakumar, K., Dr. Rajavel, R. and
Sabarish, R. Experimental Investigation of Creep Behaviour of Aluminium
Alloy (LM25) and Zirconium Di-Oxide (ZrO 2 ) Particulate MMC.
International Journal of Mechanical Engineering and Technology, 6(8), 2015,
pp. 126-138.
http://www.iaeme.com/IJMET/issues.asp?JTypeIJMET&VType=6&IType=8

1. INTRODUCTION:
Composite material is a material composed of two or more distinct phases (matrix
phase and reinforcing phase) and has bulk properties significantly different from those
of any of the constituents. Many of common materials (metals, alloys, doped ceramics
and polymers mixed with additives) also have a small amount of dispersed phase s in
their structures, however they are not considered as composite materials since their
properties are similar to those of their base constituents (physical property of steel are
similar to those of pure iron) . Favorable properties of composites materia ls are high
stiffness and high strength, low density, high temperature stability, high electrical and
thermal conductivity, adjustable coefficient of thermal expansion, corrosion
resistance, improved wear resistance etc. Metal Matrix Composites are composed of a
metallic matrix (Al, Mg, Fe, Cu etc) and a dispersed ceramic (oxide, carbides) or
metallic phase( Pb, Mo, W etc). Ceramic reinforcement may be silicon carbide, boron,
alumina, silicon nitride, boron carbide, boron nitride etc. whereas Metallic
Reinforcement may be tungsten, beryllium etc . MMCs are used for Space Shuttle,
commercial airliners, electronic substrates, bicycles, automobiles, golf clubs and a
variety of other applications. From a material point of view, when compared to
polymer matrix composites, the advantages of MMCs lie in their retention of strength
and stiffness at elevated temperature, good abrasion and creep resistance properties.
Most MMCs are still in the development stage or the early stages of production and
are not so widely established as polymer matrix composites. The biggest
disadvantages of MMCs are their high costs of fabrication, which has placed
limitations on their actual applications. There are also advantages in some of the
physical attributes of MMCs such as no significant moisture absorption properties,
non- inflammability, low electrical and thermal conductivities and resistance to most
radiations. Li Xu-Dong et al [1] have carried out a experimental investigation to
estimate the reliable effect of prior corrosion state on fatigue micro-crack initiation
and early stage propagation behaviour of aluminum alloy based on scanning electron
microscopy (SEM) in situ observation. Results indicated that multi- cracks initiation
occurred almost at the corrosion pits and the early stage of fatigue micro crack
propagation behaviour can be described by KI/KII-mixed mode. Ashley D. Spear et al
[2] have carried out a experimental investigation to study the effect of alkaline
chemical milling used for dimensionally reducing aluminum-alloy structures in terms
of total fatigue life and crack- initiation mechanisms. Chemically milled AlMgSi
specimens exhibited a 50% reduction in average fatigue lives compared to
electropolished AlMgSi specimens at comparable peak-applied loads above
macroscopic yield. D. Q. Peng et al [3] have studied the effect of aluminum ion
implantation on the aqueous corrosion behavior of zirconium, specimens were
implanted with aluminum ions with fluence ranging from 11016 to 11017 ions/cm2 ,
using a metal vapor vacuum arc source (MEVVA) at an extraction voltage of 40 kV.

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A. R. Sivaram, K. Krishnakumar, Dr. R. Rajavel and R. Sabarish

The valence states and depth distributions of elements in the surface layer of the
samples were analyzed by X-ray photoelectron spectroscopy (XPS) and auger
electron spectroscopy (AES), respectively. LUO Yun-rong et al [4] have studied the
Effects of Strain Rate on Low Cycle Fatigue Behaviors of High-Strength Structural
Steel. S. Huang et al [5] have carried out a experimental study to investigate Effects
of laser energy on fatigue crack growth (FCG) properties of 6061-T6 aluminum alloy
subjected to multiple laser peening (LP) were investigated. LP experiments and
typical FCG experiments were performed on the compact tension (CT) samples. The
results showed that compressive RS induced by LP can effectively decrease FCG rate
and increase FCG lives of CT samples. The fatigue behavior of aluminium alloy was
investigated under different conditions [69]. K. Mori et al [10] have studied the static
and fatigue strengths of mechanically clinched and self-pierce riveted joints in
aluminium alloy Sheets and compared with those of a resistance spot welded joint. D.
Khireddine et al [11] have carried experimental tests to investigate the Low cycle
fatigue behaviour of an aluminium alloy with small shearable precipitates. V.
Balasubramanian et al [12] have studied Influences of pulsed current welding and post
weld aging treatment on fatigue crack growth behaviour of AA7075 aluminium alloy
joints. The role of microstructural variability on the fatigue behavior aluminum metal
matrix composites were studied by using different techniques [1317]. In this paper,
an Aluminum composite material is produced by mixing high strength low weight
material with zirconium di-oxide for different proportions (0%, 3%, 6%, and 9%) by
using stir casting technique. In this paper experimental tests were carried out to
determine the creep strength for different proportions (0%, 3%, 6%, and 9%) of
Zirconium-di-oxide with LM25 by creep testing machine. SEM and microstructure
analysis was also done to see the distribution and presence of ZrO 2 particles in
aluminium alloy.

2. EXPERIMENTAL WORK
2.1. Stir casting process
Three steps are involved in this casting process are,
1. Heating metal till it becomes molten
2. Pouring the molten metal into a mould
3. Allowing the metal to cool and solidify in the shape of the mould.

Stir Casting is a liquid state method of composite materials fabrication, in which a

dispersed phase (ceramic particles, short fibers) is mixed with a molten matrix metal
by means of mechanical stirring. Stir Casting is the simplest and the most cost
effective method of liquid state fabrication. Liquid state fabrication of Metal Matrix
Composites involves incorporation of dispersed phase into a molten matrix metal,
followed by its Solidification. In order to provide high level of mechanical properties
of the composite, good interfacial bonding (wetting) between the dispersed phase and
the liquid matrix should be obtained. Wetting improvement may be achieved by
coating the dispersed phase particles (fibers). Proper coating not only reduces
interfacial energy, but also prevents chemical interaction between the dispersed phase
and the matrix. The aluminium alloy is casted in a stir casting machine as shown in
Figure 2.1. When setting up the stir caster before an experiment the rotor was first
lowered into the crucible, its height was accurately adjusted to form a partial seal at
the exit such that it was held concentrically during stirring. Only a partial sealing of
the outlet was allowed to ensure that torque pick-up from the rotor-crucible was

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

negligible. An external plug attached to the batch casting trolley provided a full seal at
the exit. After the caster set- up, metal melted in an induction furnace was tra nsferred
to a resistance holding furnace where it was stabilized at a temperature 20 C above
the liquidus temperature. The melt was then poured into the stir caster furnace which
had been preheated to 570 C for A356 and to 595 C for Al4% Si. Once the
temperature of the semi- solid melt (Tss) was stabilized, giving the desired fs, via the
element controllers, rotation of the stirrer was started. After shearing the alloy at the
specified shear rate and for the specified length of time, the rotor was raised, the plug
on the batch casting trolley. Stir casting setup consists of digital control muffle
furnace and a stirrer made of graphite as shown in Figures 2.2 and 2.3 which is
connected to electric motor with speed range of 22840 rpm. SiC particles were
artificially oxidized in air at 1000 C for 150 min to form a layer of SiO 2 on them and
improve their wet ability with molten aluminium. This treatment helps the
incorporation of the particles while reducing undesired interfacial reactions. Batches
of the matrix alloy were melted in a clay-bonded graphite crucible of 1.5 kg capacity
using a small muffle furnace. The temperature of the alloy was first raised to about
800 C and then stirred at 540 rpm using an impeller fabricated from graphite and
driven by a variable ac motor.
2.1.1. Synthesis of composite
The synthesis of composite is done by stir casting route. The parameters which are
important in this work are stirrer design, preheating temperature for particulate and
stirring speed. These parameters are discussed below.
2.1.2. Stirrer design
It is essentially requires for vortex formation for the uniform dispersion of particles.
There is a no uniform dispersion of particles in case of no vortex formation.
2.1.3. Particle preheating temperature
Preheating of particulate is necessary to avoid moisture from the particulate otherwise
there is chance of agglomeration of particulate due moisture and gases. Along this SiC
particles are heated at 1000 C to form a oxide layer on the SiC particles which make
it chemically more stable and by the oxide layer formation wet ability will increase so
particles will get effectively embedded in aluminium matrix and there will be only
less number of porosities in casting. After oxide layer formation preheating of
particulate is done on temperature of 400 C.
2.1.4. Stirring speed
In this process, stirring speed was 240 rpm which was effectively producing vortex
without any spattering. Stirring speed is decided by fluidity of metal speed, dispersion
of particulates are not proper because of ineffective vortex.

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A. R. Sivaram, K. Krishnakumar, Dr. R. Rajavel and R. Sabarish

Figure 2.1 Aluminium Stir casting Machine

Figure 2.2 Muffle furnace

Figure 2.3 Graphite stirrer

2.2. Materials
The Percentage of composition on each phase and the number of specimens required
are listed below. The specimens are as shown in Figure 2.4. The specimens are,
a) 0.97 weight fraction of LM25 and 0.03 Weight fraction of ZrO 2 ,

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

b) 0.94 weight fraction of LM25 and 0.06 Weight fraction of ZrO 2 ,

c) 0.91 weight fraction of LM25 and 0.09 Weight fraction of ZrO2 ,
d) 100% weight fraction of LM25.
The heat-treated alloy has fairly good machining properties, but tools should
preferably be of high speed steel and must be kept sharp. A moderately high rate of
tool wear may be expected. Liberal cutting lubricant should be employed. As
with LM6, resistance to corrosive attack by sea water and marine atmospheres is high
with this alloy. A protective anodic film can be obtained by either the sulphuric or
chromic acid process, but the grey opaque character of coatings of normal thickness
precludes their colouring in light shades for decorative purposes. There are three
common heat treated conditions for LM25: TE (precipitation treated), TB7 (solution
treated and stabilized, and TF (fully heat treated).

Figure 2.4 LM25 + 0% ZrO2 , LM25 + 3% ZrO2 , LM25 + 6% ZrO2 , LM25 + 9% ZrO2

2.3. Microstructure analysis

The well-polished samples as shown in Figure 2.5 were then observed under an
optical microscope. Micrographs were taken with the help of CCD camera attached to
the optical microscope which is shown in Figure 2.6 and are further viewed on
computer with optical image analyzer software at magnification of 200X.

Figure 2.5 Al +3%ZrO2 , Al +6%ZrO2 , Al +9%ZrO2

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A. R. Sivaram, K. Krishnakumar, Dr. R. Rajavel and R. Sabarish

Figure 2.6 Optical Microscope

2.4. Creep Test

Creep occurs as the result of long term exposures to levels of stress that are below the
yield strength of material. Creep always increases with temperature. The rate of this
deformation is a function of material properties, exposure time, exposure temperature,
and the structural applied load. The creep testing machine and the testing of the
specimen in the creep testing machine is shown in Figure 2.7.

Figure 2.7 Creep Testing Machine

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

3. RESULTS & DISCUSSIONS

3.1. Microstructure Analysis by Optical Microscope
The images of the micro structural characterization carried out by optical microscope
for the 3% , 6%, 9% weight fraction of the particle reinforced composite is shown in
Figures 3.1, 3.2, 3.3.

Figure 3.1 Optical Image of LM25 & 3%ZrO2

Figure 3.2 Optical Image of LM25 & 6%ZrO2

Figure 3.3 Optical Image of LM25 & 9%ZrO2

The grain size estimation for LM25 & 3%, 6%, 9% weight fraction of the particle
reinforced composite is shown in Table 3.1.

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A. R. Sivaram, K. Krishnakumar, Dr. R. Rajavel and R. Sabarish

Table 3.1 Grain Size Estimation
Parameter
Field measured
Total area
Standard
ASTM GRAIN
SIZE#
INTERCEPTS
MEAN Int.
LENGTH
STANDARD
DEVIATION
95%CI
RA%

LM25 & 3%
ZrO2

LM25 & 6%
ZrO2

LM25 & 9%
ZrO2

2
0.88474 sqmm
ASTM E1382

1
0.44237 sqmm
ASTM E1382

1
ASTM E1382

1.5

0.6

3.3

286

85

190.2425

256.6118

13969.6

0.117

5018.157

0.229
120.248

8042.722
57.573

3.1.1. MICROSTRUCTURE ANALYSIS BY SCANNING ELECTRON

MICROSCOPE
The micro structural characterization carried out by scanning electron microscope for
the 3%, 6%, 9% weight fraction of the particle reinforced composites are shown in
Figures 3.43.10.

Figure 3.4 SEM Image of LM25 & 3%ZrO2 for 250 k

Figure 3.5 SEM Image of LM25 & 3%ZrO2 for 250 SE

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

Figure 3.6 SEM Image of LM25 & 6%ZrO2 for 250 k

Figure 3.7 SEM Image of LM25 & 6%ZrO2 for 250 SE

Figure 3.8 SEM Image of LM25 & 6%ZrO2 for 500 SE

Figure 3.8 SEM Image of LM25 & 9%ZrO2 for 250 SE

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A. R. Sivaram, K. Krishnakumar, Dr. R. Rajavel and R. Sabarish

Figure 3.9 SEM Image of LM25 & 9%ZrO2 for 250 k

Figure 3.10 SEM Image of LM25 & 9%ZrO 2 for 500 SE

From the micro structural analysis, it is found that the Zirconium di-oxide
particles are of non-uniform size, irregularly shaped and randomly dispersed in the
alloy matrix. Agglomeration or clustering of the particles is also observed, resulting in
particle-rich and particle depleted regions. This material in homogeneity is generally
higher in these types of composites than the unreinforced matrix alloy. This was
probably formed during composite fabrication, by reaction between the Zirconium dioxide particles and LM25 matrix aluminum alloy. Moreover the particle clusters are
found to be more when compared with others. These results, also often reported for
particle reinforced composites, are generally related to the intrinsic micro structural in
homogeneity of these materials, as regards to distribution.

3.2. Creep Test Analysis

200
195

Displacement(mm)

Pure LM25

190
LM25 & 3%
ZrO2

185

180
175
170
165
160
0

10

Load(kg)

Figure 3.11 Comparison on variation of displacement with respect to load for different
proportions of particle reinforced composite.

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Experimental Investigation of Creep Behaviour of Aluminium Alloy (LM25) and Zirconium

Di-Oxide (ZrO2 ) Particulate MMC

From the Figure 3.11, it can be observed that, the creep strength is low for LM25
& 3% of ZrO 2. LM25 & 6% ZrO 2 have same creep strength as that of pure LM25.
LM25 & 9% ZrO 2 have the highest creep strength of all the samples. It is seen that
with the increase in addition of ZrO 2 with LM25 the creep strength of the composite
material increases. It is also seen that with the increase in load displacement increases.

4. CONCLUSION:
Based on the experimental investigations of the role of ZrO 2 particulates with LM25
aluminum alloy metal matrix composites, the following conclusions can be made.
1. The Creep strength of the Aluminium alloy (LM25) reinforced with Zirconium dioxide (ZrO2 ) particulate composites is generally higher than that of unreinforced
Aluminium alloy and consistent with other studies on particle reinforced metal matrix
composites.
2. The beneficial effect of particle addition on Creep strength is more evident at lower
stress levels and there is no appreciable change in creep strength with increasing
weight fraction of particulates at higher stress level.
3. The Creep strength of the Aluminium alloy (LM25) - Zirconium di-oxide (ZrO2 )
particulate composite, which may be attributed to its coarser grain size and in
homogeneity of particle distribution and this also consistent with micrographs of the
composites.
4. It is seen that with the increase in addition of ZrO 2 with LM25 the creep strength of
the composite material increases. It is also seen that with the increase in load
displacement increases. Moreover, the weight fraction of above 3% particle
reinforcement has no appreciable effect on creep properties.

In future, the results of this study can be compared with other combination of
matrix and reinforcement to develop cost effective material with respect to
applications.

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