Experimental Investigation of Processes and Properties-Thesis

Experimental Investigation of Processes and Properties
of Aluminum Matrix Composites

Thesis
SUBMITTED FOR THE AWARD OF DEGREE OF
Doctor of Philosophy
In
Mechanical Engineering
By
Sajjad Arif
Under the Supervision of
Akhtar Husain Ansari
Department of Mechanical Engineering

ALIGARH MUSLIM UNIVERSITY
ALIGARH-202002 (INDIA)
2018
CANDIDATE’S DECLARATION
I, Sajjad Arif, Department of Mechanical Engineering, certify that the work embodied in this
Ph.D. thesis is my own bonafide work carried out by me under the supervision of Prof. Akhter
Husain Ansari (Supervisor) and M. Arif Siddiqui (Co-Supervisor) at Aligarh Muslim
University, Aligarh. The matter embodied in this Ph.D. thesis has not been submitted for the
award of any other degree.
I declare that I have faithfully acknowledged, given credit to and referred to the research
workers wherever their work have been cited in the text and the body of the thesis. I further
certify that I have not willfully lifted up some other’s work, para, text, data, results, etc.
reported in the journals, books, magazines, reports, dissertations, theses, etc., or available at
websites and included them in this Ph.D. thesis and cited as my own work.
Date: (Signature of the candidate)
Sajjad Arif
CERTIFICATE FROM THE SUPERVISOR
This is to certify that the above mentioned statements made by the candidate is correct to the
best of my knowledge.
Signature of the Supervisor Signature of the Co-Supervisor
Name and Designation: Name and Designation:

Akhter H. Ansari, Professor M Arif Siddiqui, Associate Professor
Department: Mechanical Engineering Department: Mechanical Engineering
(Signature of the Chairman of the Department with seal)
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COURSE/COMPREHENSIVE EXAMINATION/PRE-SUBMISSION
SEMINAR COMPLETION CERTIFICATE
This is to certify that Mr. Sajjad Arif, Department of Mechanical Engineering has satisfactorily
completed the course work/ comprehensive examination and pre-submission seminar
requirement which is part of his Ph.D. program.
Date: (Signature of the Chairman of the Department with seal)
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COPYRIGHT TRANSFER CERTIFICATE
Title of the Thesis: Experimental Investigation of Processes and Properties of Aluminium

Matrix Composites
Candidate’s Name: Sajjad Arif
Copyright Transfer
The undersigned hereby assigns to the Aligarh Muslim University, Aligarh copyright that may
exist in and for the above thesis submitted for the award of the Ph.D. degree.
Signature of the candidate
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ACKNOWLEDGEMENTS
All praises be to The Almighty ALLAH, (S.W.T.) who is the creator of all and who
has given us brain to explore his mysterious and challenging world. And peace be upon His
prophet MUHAMMAD (S.A.W), who has shown us the right path to do so.
First and foremost, I would like to thank my supervisors, Prof. Akhter H. Ansari and
M. Arif Siddique, Mechanical Engineering Department, AMU, for his encouragement, support
and guidance throughout this work, and also in writing this thesis.
I would also like to thank Prof. M. Faisal Sayeed Baig (Chairperson) and Prof. M.
Altamush Siddiqui, (Ex-Chairperson) Department of Mechanical Engineering for providing
me all the facilities required during my research work. I would also like to appreciate and
expressed my thanks to Prof. Mohammad Muzammil, Prof. Mohammed Ali, Prof. Abid Ali
Khan, Dr. Faisal Talib and all the Faculty Members of MED for their valuable suggestions at
many stages during the work.
I am grateful to my senior Dr. Basharat Jamil and Dr. Shahid Husain who helped me
during experimental and Statistical work and made my work easier. I would also like to thank
all my colleagues and friends, especially Mr. Reyaz Arif, Mr. Md. Azhar, Md. Tanwir Alam,
Mohd. Athar Khan, Mohd. Farhaan Zafar and all the Research Scholars for their help whenever
I required.
My special thanks are due, to Mr. Mujahid, Mr. Hussain, Mr. Rehan, Mr. Shoaib, Mr.
Rashid and Mr. Zubair for their help in carrying the experimental work in the Powder
Metallurgy lab and Stress Analysis and tribology lab. I wish to express my sincere gratitude to
everyone who by any means has helped me during my PhD work. I am deeply thankful to my
parents for their love and support at every stage in my life.
Lastly, I would also like to thank University Grants Commission, New Delhi for
providing UGC-Non-NET and Department of Science and Technology for providing funds
under DST-PURSE Programme that were utilized in instrumentation of the experimental set-
up.
Sajjad Arif
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ABSTRACT
Aluminium has been widely used in engineering applications because it is light in weight.
However, use of pure aluminium in many engineering and tribological applications is difficult
because of its low strength and wear properties.
A vast number of experimental studies have been performed on addition of hard ceramic
particles to aluminium matrix to enhance its strength, hardness and wear resistance.
Aluminium Matrix Composites (AMCs) have found potential applications in aerospace,
automobiles and structural sectors because of its low density and high strength. Reduction in
weight of composites by the use of aluminium matrix produces great economic advantage.
AMCs are generally synthesized through Stir Casting and Powder Metallurgy techniques. In
this work, powder metallurgy technique was used to fabricate AMCs because of following
advantages: (a) low processing temperature, (b) homogeneous distribution of reinforcement
and matrix particle, and (c) fabrication of near net shaped products.
The main objective of this research work is to fabricate aluminium matrix composites
reinforced with micro and nanoparticles. Three combinations of aluminium composites were
fabricated through powder metallurgy technique viz. aluminium reinforced with nano zirconia
and micro silicon carbide (Al-SiCmicro-ZrO2nano), aluminium reinforced with micro and nano
silicon carbide particles (Al-SiCmicro-SiCnano) and aluminium reinforced with nano zirconia and
micro graphite particles (Al-ZrO2nano-Grmicro). One combination of composites (Al-SiCmicro-
SiCnano) were also fabricated through electric resistance sintering (Non-Conventional sintering
process) method to compare the differences between conventional and non-conventional
sintering process. For all the fabricated combinations the morphological, physical, and wear
properties of the composites were studied. The wear behaviour of the composites were
performed using pin-on-disc wear tester. Statistical analysis, Artificial Neural Network (ANN)
and Global performance indicator (GPI) have been applied for the quantitative analysis of
experimental data. The detail analysis and their findings have been discussed in the upcoming
paragraphs.
In the first experimental investigation: The mechanical and tribological behaviour of
aluminium (Al)-based silicon carbide (SiC, microparticles) and zirconium oxide (ZrO2,
nanoparticles) particle-reinforced hybrid composites were investigated. The X-Ray
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diffractometer (XRD), Scanning Electron Microscope (SEM), Energy Dispersive Spectrum
(EDS) and Elemental Mapping were used for characterization of composites. Elemental
mapping of the composites exhibited uniform distribution of SiC and ZrO2 in the matrix. The
hardness and wear resistance of the Al+SiC+ZrO2 hybrid composites were found to be
enhanced by increasing ZrO2 content. The worn surface of hybrid composites and pure
aluminium were analyzed through SEM to understand wear mechanism.
Further, tribological performance of aluminium hybrid composites reinforced with micro SiC
and nano zirconia were investigated using statistical and Artificial Neural Network (ANN)
approach. The influence of zirconia reinforcement, sliding distance and applied load were
analyzed with test based on full factorial design of experiments. Analysis of variance
(ANOVA) was used to evaluate the percentage contribution of each process parameters on
wear loss. A very close correlation between experimental and ANN output was achieved by
implementing the model.
In the second experiment work: Aluminium matrix composites reinforced with SiC micro
particles along with SiC nano particles were fabricated through powder metallurgy. The
fabricated hybrid composites were characterized by X-Ray Diffractometer (XRD), Scanning
Electron Microscope (SEM), Energy Dispersive Spectrum (EDS) and elemental mapping. The
relative density, hardness and wear behaviour of all hybrid nanocomposites were studied. The
hardness and wear test results showed that properties of the hybrid composites containing 5
wt. % nano SiC are better than other hybrid composites.
Further, the effect of nano-silicon carbide (SiC), sliding distance and applied load were studied
by full factorial design (5×3×2) of experiments. The influence of SiC, sliding distance and
applied load were found to be 42.4, 42.3 and 11.3 % respectively. The wear resistance of the
nanocomposites reinforced with 5 wt. % SiC nanoparticles is best amongst all synthesized
nanocomposites. Worn surfaces and wear debris were analyzed using both Scanning Electron
Microscopy (SEM) and Electron Dispersive Spectroscopy (EDS) to recognize wear
mechanism. Further, five different regression models were developed to estimate the
tribological behaviour of composites with nano-silicon carbide (SiC) reinforcement, sliding
distance and applied load as inputs. The accuracy of the models was evaluated using five most
commonly used statistical indicators. The models were ranked according to their suitability of
prediction using Global Performance Indicator. The predicted values and experimental data
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showed a high degree of association. It was recognized that the developed models can be used
to predict the wear behavior within the range of investigation.
In the third experimental analysis: Morphological characterization and wear behaviour of
micro graphite (Gr) and nano zirconia (ZrO2) reinforced aluminium hybrid composites were
investigated. The contents of Gr (0, 2, 4, 6 and 8 wt. %) were added to Al+10%ZrO2
nanocomposites through powder metallurgy (PM) technique. The morphological
characterization of all synthesized composites were performed using X-ray diffractometer
(XRD), Scanning Electron Microscope (SEM), Energy Dispersive Spectrum (EDS) and
Elemental Maps. The influence of graphite (0, 2, 4, 6 and 8 wt. %) reinforcement, sliding
distance (400, 600 and 800 m) and applied load (30 and 40 N) were studied using design of
experiments (5×3×2). The contribution of Gr reinforcement, sliding distance and applied were
found to be 80.59, 16.25 and 2.06 % respectively. The wear resistance of the hybrid composites
reinforced with 6 wt. % graphite particles is best amongst all synthesized composites. Worn
surfaces and wear debris were analyzed using both SEM and EDS to recognize wear
mechanism. EDS spectrum of hybrid composites validates the existence of oxides of
aluminium and iron, known as Mechanically Mixed Layer (MML), responsible for enhanced
wear resistance. This investigation revealed that the wear resistance of the hybrid composites
can be enhanced by the combined effect of micro graphite and zirconia nanoparticles. Further,
five different regression models were developed to estimate the wear behaviour of composites
with graphite (Gr) reinforcement, sliding distance and applied load as inputs. The accuracy of
the models was evaluated using five most commonly used statistical indicators. The models
were ranked according to their suitability of prediction using Global Performance Indicator.
The predicted values and experimental data showed a high degree of association (R ranging
from 0.91 to 0.96). It was recognized that the developed models can be used to predict the wear
behavior within the range of investigation.
In the final experimental investigation: Micro and nano-silicon carbide (SiC) reinforced
aluminium matrix composites were fabricated by conventional sintering and electric resistance
sintering processes. The sintering processes were performed at 450°C and 350°C using
conventional and electric resistance process respectively. The fabricated composites were
characterized by X-ray Diffractometer (XRD) and Scanning Electron Microscope (SEM). The
porosity, hardness and wear behaviour of composites were studied with pin-on-disc wear
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apparatus. The composites fabricated through electric resistance sintering showed improved
physical (porosity) and mechanical behaviour (hardness). Further, electric resistance sintering
samples showed improved wear resistance compared to corresponding conventionally
sintering samples.
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Table of contents
CANDIDATE’S DECLARATION ......................................................................................... i

CERTIFICATE FROM THE SUPERVISOR ...................................................................... i
COURSE/COMPREHENSIVE EXAMINATION/PRE-SUBMISSION SEMINAR
COMPLETION CERTIFICATE .......................................................................................... ii
COPYRIGHT TRANSFER CERTIFICATE ..................................................................... iii
Acknowledgements ................................................................................................................ iv
Abstract .................................................................................................................................... v
Table of contents .................................................................................................................... ix
List of figures ........................................................................................................................ xiv
List of table ........................................................................................................................... xix
Nomenclature ........................................................................................................................ xx
1. Introduction and Literature Review .............................................................................. 1
1.1 Brief introduction ....................................................................................................... 1
1.2 Composites ................................................................................................................. 2
1.2.1 Aluminium matrix composites (AMCs) ................................................................... 2
1.2.2 Types of AMCs ........................................................................................................ 3
1.3 Fabrication technique of AMCs ................................................................................. 5
1.3.1 Liquid state processing ............................................................................................. 5
1.3.2 Solid state processes ................................................................................................. 6
1.4 Wear ........................................................................................................................... 8
1.4.1 Adhesive wear .......................................................................................................... 9
1.4.2 Abrasive wear ........................................................................................................... 9
1.4.3 Erosive wear ........................................................................................................... 10
1.4.4 Surface-fatigue wear ............................................................................................... 10
1.5 Need of reinforcements ............................................................................................ 11
1.5.1 Silicon carbide (SiC) as a reinforcement ................................................................ 11
1.5.2 Zirconia (ZrO2) as a reinforcement ........................................................................ 12
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1.5.3 Graphite as a reinforcement .................................................................................... 12
1.6 Fabrication of aluminium matrix composites........................................................... 12
1.7 Research gap related to aluminium matrix composites ............................................ 20
1.8 Objectives of the research work ............................................................................... 22
2. Materials and Experimental Procedure ...................................................................... 24
2.1 Materials ................................................................................................................... 24
2.1.1 Aluminium Powder................................................................................................. 24
2.1.2 Silicon Carbide (Micro and Nanoparticles) ............................................................ 24
2.1.3 Zirconia nanoparticles (ZrO2) ................................................................................. 25
2.1.4 Graphite particles .................................................................................................... 25
2.2 Experimental Set-up ................................................................................................. 26
2.2.1 Measurement and mixing of elemental powders .................................................... 26
2.2.2 Compaction of elemental powders ......................................................................... 27
2.2.3 Sintering of green pallets ........................................................................................ 28
2.3 Morphological Characterizations ............................................................................. 28
2.3.1 X-Ray Diffraction ................................................................................................... 28
2.3.2 Metallographic Analysis ......................................................................................... 29
2.4 Density measurement ............................................................................................... 30
2.5 Rockwell Hardness Measurement ............................................................................ 30
2.6 Dry sliding wear test ................................................................................................ 31
3. Study of Mechanical and Tribological Behaviour of Al/SiC/ZrO2 Hybrid
Composites Fabricated Through Powder Metallurgy Technique .................................... 32
3.1 Introduction .............................................................................................................. 32
3.2 Experimental ............................................................................................................ 33
3.2.1 Sample preparation ................................................................................................. 33
3.2.2 Wear test ................................................................................................................. 35
3.3 Results and Discussion ............................................................................................. 36
3.3.1 Morphological study ............................................................................................... 36
3.3.2 Density, Porosity and Relative density measurement ............................................ 39
3.3.3 Hardness measurement ........................................................................................... 41
3.3.4 Sliding wear behaviour ........................................................................................... 44
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3.4 Conclusions .............................................................................................................. 51
4. Analysis of Tribological Behaviour of Zirconia Reinforced Al-SiC Hybrid
Composites Using Statistical and Artificial Neural Network Technique ........................ 53
4.1 Introduction .............................................................................................................. 53
4.2 Experimentation ....................................................................................................... 55
4.2.1 Fabrication of composites ....................................................................................... 55
4.2.2 Wear analysis .......................................................................................................... 56
4.3 Results and discussion.............................................................................................. 56
4.3.1 Experimental design and ANOVA analysis ........................................................... 56
4.3.2 Effect of different process parameters on wear loss ............................................... 58
4.3.3 Linear regression model ......................................................................................... 61
4.3.4 Artificial neural network modelling (ANN) ........................................................... 61
4.3.5 Verification of sliding wear behaviour with ANN ................................................. 63
4.4 Conclusions .............................................................................................................. 64
5. Morphological and Wear Behaviour of New Al-SiCmicro-SiCnano Hybrid
Nanocomposites Fabricated Through Powder Metallurgy ............................................... 66
5.1 Introduction .............................................................................................................. 66
5.2 Experimentation ....................................................................................................... 68
5.2.1 Fabrication of composites ....................................................................................... 68
5.2.2 X-ray diffraction ..................................................................................................... 69
5.2.3 Dry sliding wear test ............................................................................................... 69
5.3 Results and discussion.............................................................................................. 70
5.3.1 Characterization of composites .............................................................................. 70
5.3.2 Relative density ...................................................................................................... 72
5.3.3 Hardness measurement ........................................................................................... 73
5.3.4 Dry sliding wear behaviour .................................................................................... 74
5.4 Conclusions .............................................................................................................. 82
6. Surface Characterization, Wear Investigation and Statistical Modelling of Micro
and Nano-SiC Reinforced Aluminum Hybrid Composites ............................................... 83
6.1 Introduction .............................................................................................................. 83
6.2 Materials and Methods ............................................................................................. 84
6.3 Experimental Plan .................................................................................................... 85
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6.4 Results and Discussion ............................................................................................. 87
6.4.1 Porosity and Hardness measurements .................................................................... 87
6.4.2 Analysis of variance (ANOVA) ............................................................................. 88
6.4.3 Effect of different process parameters on wear loss ............................................... 89
6.4.4 Investigation of wear mechanism by SEM ............................................................. 91
6.4.5 Wear debris analysis ............................................................................................... 94
6.4.6 Mathematical modelling and statistical analysis of models ................................... 96
6.4.7 Statistical analysis of regression models .............................................................. 100
6.4.8 Ranking of models by Global Performance Indicator (GPI) ................................ 101
6.5 Conclusions ............................................................................................................ 102
7. Characterization of Surface Morphology, Wear Performance and Modelling of
Graphite Reinforced Aluminium Hybrid Composites .................................................... 104
7.1 Introduction ............................................................................................................ 104
7.2 Materials and Methods ........................................................................................... 106
7.3 Experimental Plan .................................................................................................. 107
7.4 Results and Discussion ........................................................................................... 109
7.4.1 Morphological characterization of composites..................................................... 109
7.4.2 Hardness measurement ......................................................................................... 112
7.4.3 Sliding wear behaviour ......................................................................................... 113
7.4.4 Analysis of variance (ANOVA) ........................................................................... 117
7.4.5 Effect of different process parameters on wear loss ............................................. 118
7.4.6 Investigation of wear mechanism by SEM ........................................................... 120
7.4.7 Wear debris analysis ............................................................................................. 123
7.4.8 Mathematical modelling and statistical analysis of models ................................. 126
7.4.9 Statistical analysis of regression models .............................................................. 129
7.4.10 Ranking of models by Global Performance Indicator (GPI) .............................. 130
7.5 Conclusions ............................................................................................................ 131
8. Micro and Nano Silicon Carbide Reinforced Aluminium Matrix Composite
Prepared By Conventional and Electric Resistance Sintering Processes ...................... 133
8.1 Introduction ............................................................................................................ 133
8.2 Experimental .......................................................................................................... 135
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8.2.1 Sample preparation ............................................................................................... 135
8.2.2 Conventional sintering .......................................................................................... 135
8.2.3 Electric resistance sintering .................................................................................. 136
8.2.4 Steps involved in fabrication of sample through electric resistance sintering
process ........................................................................................................................... 137
8.3 Results and discussion............................................................................................ 138
8.3.1 Characterization of composites ............................................................................ 138
8.3.2 Scanning Electron Microscopy (SEM) of composites ......................................... 140
8.3.3 Porosity and Hardness measurement .................................................................... 142
8.3.4 Wear behaviour..................................................................................................... 144
8.3.5 Analysis of Worn surface by SEM ....................................................................... 145
8.4 Conclusions ............................................................................................................ 147
9. Recommendations for Future Work .......................................................................... 148
References ............................................................................................................................ 149
List of Publications ............................................................................................................. 162
Reprints of Published Papers ............................................................................................. 163
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List of figures
Figure 1.1 Schematic representation of the abrasive wear mechanism [24]............................. 9

Figure 1.2 Schematic representation of the abrasive wear mechanism[24]............................ 10
Figure 1.3 Schematic representation of the erosive wear mechanism[26]. ............................ 10
Figure 1.4 Schematic representation of the surface fatigue wear mechanism [27]. ............... 11
Figure 2.1 SEM micrographs of as-received aluminium powders. ....................................... 24
Figure 2.2 SEM micrographs of as-received (a) SiC micro-particles (b) SiC nano-particles 25
Figure 2.3 SEM micrographs of as-received nano-zirconia (ZrO2) powders ......................... 25
Figure 2.4 SEM micrographs of as-received graphite powders .............................................. 26
Figure 2.5 Digital weighing machine Figure 2.6 Centrifugal ball mill .............................. 27
Figure 2.7 Uniaxial hydraulic pallet press (a), Punch, die (b), and fabricated samples (c). .. 27
Figure 2.8 Electric tubular furnace for conventional sintering (PM Lab., MED) .................. 28
Figure 2.9 X -ray Diffraction machine ................................................................................... 29
Figure 2.10 Scanning Electron Microscope ............................................................................ 30
Figure 2.11 Digital Rockwell Hardness Figure 2.12 Pin-on-disc wear tester .............. 31
Figure 3.1 The size distribution of as-received: (a) Aluminium powder, (b) SiC particles, (c)
ZrO2 particles. ......................................................................................................................... 34
Figure 3.2 XRD pattern of fabricated hybrid composites. ...................................................... 37
Figure 3.3 EDS spectrum of Al+5%SiC+9%ZrO2 reinforced composites. ............................ 37
Figure 3.4 Elemental maps of Al+5%SiC+9%ZrO2 hybrid composites. ............................... 39
Figure 3.5 Influence of micro and nano reinforcements on densities of Al hybrid composites.
................................................................................................................................................. 39
Figure 3.6 Influence of micro and nano reinforcements on porosity of Al hybrid composites.
................................................................................................................................................. 40
Figure 3.7 Variation of relative density of composites with ZrO2 addition. ........................... 41
Figure 3.8 Influence of weight percentage of ZrO2 on hardness of Al hybrid composites .... 42
Figure 3.9 Influence of weight percentage of ZrO2 on wear loss of Al hybrid composites. .. 44
Figure 3.10 Influence of sliding speed on wear loss of Al hybrid composites. ...................... 45
Figure 3.11 Influence of sliding distance on wear loss of Al hybrid composites. .................. 46
Figure 3.12 Influence of load on wear loss of Al hybrid composites. .................................... 46
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Figure 3.13 SEM images of worn surface of aluminium matrix at 30 N load, 2 m/s sliding
speed and 900 m sliding distance: (a) sample at 100× magnification; (b) sample at 200×
magnification; (c) sample at 500× magnification. .................................................................. 49
Figure 3.14 SEM images of worn surface of Al+5%SiC at 30 N load, 2m/s sliding speed and
900 m sliding distance: (a) sample at 100× magnification; (b) sample at 200× magnification;
(c) sample at 500× magnification. .......................................................................................... 49
Figure 3.15 SEM images of worn surface of Al+5%SiC+3%ZrO2 at 30 N load, 2 m/s sliding
Figure 4.1 Main effect plot for process parameters on wear loss of Al-SiC-ZrO2 hybrid
composites............................................................................................................................... 59
Figure 4.2 Interactions of various process parameters on wear loss. ...................................... 59
Figure 4.3 Scatter plot for wear loss ....................................................................................... 60
Figure 4.4 Normal probability plot for residuals of fabricated composites. ........................... 60
Figure 4.5 Neural network with 4-10-1 topology. .................................................................. 61
Figure 4.6 Experimental and predicted results of wear loss form ANN developed model. ... 63
Figure 4.7 ANN model results of various process parameters (a) Effect of ZrO2
concentration. (b) Effect of sliding distance (c) Effect of applied load. ................................. 64
Figure 5.1 XRD pattern Al+10%SiCµm, Al+10%SiCµm+1%SiCnm, Al+10%SiCµm+3%SiCnm,
Al+10%SiCµm+5%SiCnm, Al+10%SiCµm+7%SiCnm. ............................................................. 70
Figure 5.2 EDS spectrum of Al+10% SiCµm+5%SiCnm nanocomposites............................... 71
Figure 5.3 Elemental maps of Al+10%SiCµm+5%SiCnm hybrid composites. ........................ 72
Figure 5.4 Variation of relative density of composites with SiC concentration. .................... 73
Figure 5.5 Variation of hardness of composites with SiC concentration. .............................. 74
Figure 5.6 Variation of wear loss with varying concentration of SiC particles. ..................... 75
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Figure 5.7 Variation of wear loss with varying sliding distance for all fabricated composites.
................................................................................................................................................. 77
Figure 5.8 Variation of wear loss with varying applied load for all fabricated composites. .. 78
Figure 5.9 SEM of worn surface of pure aluminium: (a) Low magnification; (b) High
magnification. ......................................................................................................................... 79
Figure 5.10 SEM morphologies of worn surface of Al+10% SiCµm: (a) Low magnification;
(b) High magnification. ........................................................................................................... 79
Figure 5.11 SEM of worn surface of Al+10% SiCµm+1%SiCnm: (a) Low magnification; (b)
High magnification. ................................................................................................................ 80
Figure 5.12 SEM of worn surface of Al+10% SiCµm+3%SiCnm (a) Low magnification; (b)
Figure 6.1 Porosity and Hardness variation with respect to silicon carbide addition. ............ 87
Figure 6.2 Main effect plot for independent variables on wear loss of Al-SiCmicro-SiCnano
nanocomposites. ...................................................................................................................... 91
Figure 6.3 Interactions of various independent variables on wear loss. ................................. 91
Figure 6.4 SEM morph graphs of worn surface: (a) Pure aluminium, (b) 10 wt. % SiCµm, (c)
1 wt. % SiCnano, (d) 3 wt. % SiCnano, (e) 5 wt. % SiCnano and (f) 7 wt. % SiCnano reinforced Al
composites............................................................................................................................... 94
composites............................................................................................................................... 96
Figure 6.6 EDS of wear debris: (a) 5 wt. % SiCnano and (b) 7 wt. % SiCnano reinforced Al
composites............................................................................................................................... 96
Figure 6.7 Estimated values of wear loss from prediction models and experimental readings.
................................................................................................................................................. 98
Figure 6.8 Scatter plot between experimental wear loss and estimated values from models. 99
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Figure 7.1 XRD of Al+10% ZrO2, Al+10% ZrO2+2% Gr, Al+10% ZrO2+4% Gr, Al+10%
ZrO2+6% Gr and Al+10% ZrO2+8% Gr hybrid nanocomposites. ....................................... 110
Figure 7.2 EDS of Al+10%ZrO2+6%Gr reinforced composites. ......................................... 110
Figure 7.3 Elemental maps of Al+10%ZrO2+6%Gr hybrid composites. ............................. 112
Figure 7.4 Variation of hardness with graphite reinforcement in composites. ..................... 112
Figure 7.5 Variation of wear loss with concentration of graphite reinforcement in composites.
............................................................................................................................................... 113
Figure 7.6 Influence of sliding distance on wear loss of hybrid composites. ....................... 114
Figure 7.7 Influence of applied load on wear loss of hybrid composites. ............................ 115
Figure 7.8 Main effect plot for independent variables on wear loss of Al-ZrO2-Gr hybrid
composites............................................................................................................................. 119
Figure 7.9 Interactions of various independent variables on wear loss. ............................... 120
Figure 7.10 SEM morph graphs of worn surface: (a) Pure aluminium, (b) 10 wt. % ZrO2, (c)
2 wt. % Gr, (d) 4 wt. % Gr, (e) 6 wt. % Gr and (f) 8 wt. % Gr reinforced Al composites. . 123
Figure 7.11 SEM morph graphs of wear debris: (a) Pure aluminium, (b) 10 wt. % ZrO2, (c) 2
wt. % Gr, (d) 4 wt. % Gr, (e) 6 wt. % Gr and (f) 8 wt. % Gr reinforced Al composites. ..... 125
Figure 7.12 EDS spectrum of wear debris: (a) 6 wt. % Gr and (b) 8 wt. % Gr reinforced Al
hybrid composites. ................................................................................................................ 126
Figure 7.13 Estimated values of wear loss from all prediction models and experimental
readings. ................................................................................................................................ 127
Figure 7.14 Scatter plot between experimental wear loss and estimated values from all
models. .................................................................................................................................. 128
Figure 8.1 Electric resistance sintering setup. ...................................................................... 137
Figure 8.2 Typical sequence in an ERS process ................................................................... 138
Figure 8.3 XRD pattern of fabricated composites: (a) Conventional sintered samples and (b)
Electric resistance sintered samples. ..................................................................................... 139
Figure 8.4 SEM micrographs of conventional (a, c, e and g) and electric resistance sintered
samples (b, d, f, and h). ......................................................................................................... 141
Figure 8.5 Porosity (percentage) of samples fabricated through conventional and electric
resistance sintering. ............................................................................................................... 143
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Figure 8.6 Rockwell hardness of samples fabricated through conventional and electric
resistance sintering. ............................................................................................................... 144
Figure 8.7 Wear behaviour of samples fabricated through conventional and electric resistance
sintering................................................................................................................................. 145
Figure 8.8 SEM micrographs of worn surface of conventional (a, c and e) and electric
resistance (b, d and f) sintered samples. ............................................................................... 146
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List of table
Table 3.1 Details of reinforcement particles. .......................................................................... 33

Table 3.2 Various wear test conditions and parameters. ........................................................ 35
Table 3.3 List of elements present in the Al+5%SiC+9%ZrO2 reinforced composites. ........ 37
Table 3.4 Comprehensive look of previous works regarding ceramic reinforced aluminium
matrix composites. .................................................................................................................. 43
matrix composites. .................................................................................................................. 48
Table 4.1 Information of reinforced particles. ........................................................................ 55
Table 4.2 Test variables and process parameters. ................................................................... 56
Table 4.3 Process parameters with their different levels. ....................................................... 56
Table 4.4 General full factorial design ................................................................................... 57
Table 4.5 Results for ANOVA for wear loss (mg) ................................................................. 57
Table 5.1 Information of experimental particles..................................................................... 68
Table 5.2 XRD experimental description. .............................................................................. 69
Table 5.3 Test variables and process parameters. ................................................................... 69
Table 5.4 Details of elements present in Al+10%SiCµm+5%SiCnm nanocomposites. ............ 71
Table 6.1 Full factorial design (5×3×2) of experiments and their respective. ........................ 85
Table 6.2 Multilevel factorial design of experiments. ............................................................ 86
Table 6.3 Analysis of variance for the wear loss. ................................................................... 88
Table 6.4 Statistical indicators of developed regression models. ......................................... 101
Table 6.5 Statistical indicator (Scaled), GPI and Ranking of the models............................. 102
Table 7.1 Feature of reinforced particles. ............................................................................. 106
Table 7.2 X-ray diffractometer description. ......................................................................... 107
Table 7.3 Sliding wear test variables. ................................................................................... 107
Table 7.4 Full factorial design (5×3×2) of experiments and their respective. ...................... 108
Table 7.5 Multilevel factorial design of experiments. .......................................................... 108
Table 7.6 Elements present in Al+10%ZrO2+6%Gr hybrid nanocomposites. ..................... 110
matrix composites. ................................................................................................................ 116
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Table 7.8 Analysis of variance for the wear loss. ................................................................. 117
Table 7.9 Statistical indicators of developed regression models. ......................................... 130
Table 7.10 Statistical indicator (Scaled), GPI and Ranking of the models........................... 131
Table 8.1 Details of samples prepared. ................................................................................. 135
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Nomenclatures
Abbreviations
AMCs Aluminium Matrix Composites
ANN Artificial Neural Network
ANOVA Analysis of Variance
APS Average particle size
BPR Ball to Powder ratio
SEM Scanning Electron Microscopy
MMC Metal Matrix Composites
EDS Electron Dispersive Spectroscopy
PM Powder Metallurgy
ERS Electric Resistance Sintering
GPI Global Performance Indicator
MML Mechanically Mixed Layer
MAE Mean Absolute Error
MAPE Mean Absolute Percentage Error
MBE Mean Bias Error
RMSE Root Mean Square Error
XRD X-Ray Diffraction
Latin Symbols
R Correlation Coefficient
WLoss (i, exp) Experimental wear loss (g)
WLoss (i, model) Predicted wear loss (g)
WLoss (i, avg.) Average wear loss (g)
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1. Introduction and Literature Review
1.1 Brief introduction
Recently, the material scientists are heavily indulged in developing new and advanced material
matrix composites all around the globe. Due to exposure of harsh engineering environment a
single metal/alloys are failing to achieve the requirements. This initiates the need of fabrication
of metal matrix composites with certain specific properties to meet future engineering
challenges.
In the last few decades, metal matrix composites have found potential application in aerospace,
automobiles, space, defense and structural sectors because of higher specific strength, good
wear resistance, higher thermal conductivity than ceramic materials and lower coefficient of
thermal expansion etc.[1,2]
The target properties of composites depend upon combined effect of reinforced particle and
fabrication technique. As far as fabrication technique is concerned several techniques are
available such as spray deposition, squeeze casting, compo-casting, stir casting and powder
metallurgy [3]. The conventional stir casting process involves some major drawbacks like
inadequate wettability between reinforcement and matrix, nonhomogeneous distribution and
formation of brittle intermetallic compound at the reinforcement and matrix interface[1]. In
order to overcome these serious drawbacks, powder metallurgy can be used because of the
following advantages: (a) low processing temperature (b) homogeneous distribution of
reinforcement and matrix particle (c) fabrication of near net shaped product[4].
At present, aluminium matrix hybrid composites reinforced with micro and nanoparticles have
gained increased application because of enhanced mechanical and tribological properties [5].
The reason of enhancement in properties could be attributed due to the following reasons:
(a) Incorporation of uniformly dispersed nanoparticles improves the performance of
matrix due to Orowan strengthening mechanism.
(b) Better microstructure and mechanical properties can be achieved by changing particle
size from micro to nano level [6].
(c) Nano particle also retains the ductility of composites and improves fracture toughness
[7].
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(d) Micro particle works as a skeleton for aluminium matrix and enhances the hardness
and wear properties[8,9].
However, aluminium reinforced with single ceramic micro particles deteriorates the ductility
of composite because of their tendency to crack during loading condition, when their
concentration is high in the matrix. Further, incorporating nanoparticles enhances the
mechanical properties of composites by obstructing dislocation movement and promoting fine
grain structure. Therefore, overall enhancement in the performance of composites can be
achieved by reducing the concentration of micro particles and increasing the amount of
nanoparticles to get synergistic improvement in mechanical and tribological properties [10].
Thus, the main objective of this research work is to fabricate aluminium matrix composite
through conventional and nonconventional sintering process, when they are reinforced with
combinations of micro/nano silicon carbide, micro silicon carbide and nano zirconia, and
zirconia and micro graphite particles. For all the fabricated combinations the morphological,
physical, and wear properties of the composites were studied. The wear behaviour of the
composites were performed using pin-on-disc wear tester.
1.2 Composites
The term “composite” broadly refers to a material system which is composed of a discrete
constituent (the reinforcement) distributed in a continuous phase (the matrix), and which
derives its distinguishing characteristics from the properties of its constituents, from the
geometry and architecture of the constituents, and from the properties of the boundaries
(interfaces) between different constituents. The composite materials are composed of two
major constituents: (a) matrix, and (b) reinforcements. The reinforcements are hard, stiff, wear
resistant, forming a sort of backbone, while the soft matrix retains the reinforcement in a set
place. The classification of composite materials are done on the basis of physical or chemical
nature of the matrix phase, e.g., polymer matrix, metal-matrix and ceramic composites [1].
1.2.1 Aluminium matrix composites (AMCs)
In AMCs pure aluminium or its alloys serves as a matrix phase which creates a percolating
network. The reinforcements, non-metallic and commonly ceramic such as carbide, nitride and
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oxide, are embedded into the soft matrix to enhance its properties. The end properties of AMCs
depends on the nature and volume fraction of reinforcements [2].
Some potential advantages of AMCs are listed below:
 Superior strength
 Enhanced abrasion and wear resistance
 Enhanced stiffness
 Reduction in density(weight)
 Improved high temperature properties
 Controlled thermal expansion coefficient
 Thermal/heat management
 Improved and tailored electrical performance.
AMCs materials are replacing monolithic materials because it offer superior combination of
properties. Various engineering field like structural, non-structural and functional sectors have
raised the demand of AMCs because of their performance, economic and environmental
benefits. Transportation sectors are greatly benefitted by AMCs due to lower fuel consumption,
less noise and lower airborne emissions. Further, strict environmental guidelines and
importance on upgraded fuel economy, use of AMCs in transport sector will be unavoidable
and necessary in near future [11].
1.2.2 Types of AMCs
Depending upon the type of reinforcements AMCs are classified in four different categories.
 Particle-reinforced AMCs (PAMCs)

 Whisker or short fibre-reinforced AMCs (SFAMCs)
 Continuous fibre-reinforced AMCs (CFAMCs)
 Mono filament-reinforced AMCs (MFAMCs)
The brief explanation of all four types of AMCs are discussed below.
1.2.2.1 Particle-reinforced AMCs (PAMCs)

They are isotropic in nature and equiaxed ceramics particles having aspect ratio less than 5 are
usually reinforced. Carbide, nitride, boride and oxide phases of ceramics with volume fraction
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less than 30% are reinforced for tribological and structural applications. However, volume
fraction could be as high as 70% in electronic packaging applications. Both solid (powder
metallurgy) and liquid state (stir casting, infiltration and in-situ) processes could be used to
fabricate PAMCs and they are usually cheaper in comparison to other available AMCs. After
synthesis, variety of secondary operations like forging, rolling and extrusion can be performed
on PAMCs [11].
1.2.2.2 Whisker-or short fibre-reinforced AMCs (SFAMCs)

In this class of AMCs, the aspect ratio should be greater than 5, but fibre should not be
continuous. Both powder metallurgy and infiltration process are used to fabricate SFAMCs.
Short fibre-reinforced AMCs are first used to fabricate most popular piston. Further, due to
health hazard their usage are limited despite of having improved mechanical properties. Their
characteristics lies between continuous fibre and particle reinforced AMCs [11].
1.2.2.3 Continuous fibre-reinforced (CFAMCs)

The fibre diameter should be less than 20µm in continuous fibre-reinforced AMCs but the
orientation of the fibre should be continuous. Parallel, pre woven and braided fibres are used
prior to fabrication of composites. Pressure infiltration route and squeeze infiltration technique
are used for fabricating AMCs in which fibre volume fraction can be raised upto 40% [11].
1.2.2.4 Mono filament reinforced AMCs (MFAMCs)

Chemical vapour deposition of either SiC or B into a core of carbon fibre or W wire is used to
fabricate monofilaments fibres. They are having large diameters usually ranges from 100 to
150 µm. Bending flexibility multifilaments is high compared to monofilaments. Diffusion
bonding techniques are used to fabricate mono filament reinforced AMCs. Mono filament
works as a load bearing constituents in this class of AMCs. However, aluminium makes strong
bond to the reinforcements to transfer and distribute the load. They exhibits low strength in
perpendicular direction of fibre orientation because they possess directionality. In particle and
whisker reinforced AMCs, aluminum bears the load and reinforcement strengthen the
composite by restricting the deformation of matric under loading condition[1–3,11].
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1.3 Fabrication technique of AMCs
There are two most important technique to fabricate aluminium matrix composites.
 Liquid state processes.
 Solid state processes.
1.3.1 Liquid state processing
1.3.1.1 Stir casting

Stir casting is most widely used technique to develop metal matrix composites. In this method,
after melting the metal hard ceramic particles are added and then allowed the mixture to
solidify. However, the most challenging stage is to get the proper wettability between
reinforcement and matrix material. Vortex technique or stir-casting technique is adopted to
overcome the wettability problem. In this approach ceramic reinforcements are added to the
molten metal which is under mixing by mechanical stirrer. In stir casting process distribution
of reinforcement is difficult due to following reasons: (a) due to continuous movement of solid-
liquid interface, and (b) density difference between ceramic and matrix materials[11].
1.3.1.2 Infiltration process

Molten metal is injected into the porous network of particle/short fibre/continuous to fabricate
aluminium matrix composite in infiltration process. In some cases pressure is applied to inject
the molten metal. In infiltration process, the reinforcement amount can be varied from 10 to
70%. Composites fabricated through infiltration process exhibits presence of porosity and local
inhomogeneous distribution of reinforcement [11].
1.3.1.3 Spray deposition

In spray deposition process, molten spray of aluminium metal receives forced injection of
ceramic (particle/whisker/short fibre) reinforcement to fabricated AMCs. Osprey process or
by thermal spray process can be used to create the spray. Similar to infiltration process,
porosity and inhomogeneous distribution of reinforcements is found in spray deposition
process within range 5 to 10% filler content. The cost of the product fabricated through spray
deposition process is relatively cheap and generally lies between cost of the product fabricated
through stir cast and PM processes [11].
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1.3.2 Solid state processes
1.3.2.1 Diffusion bonding

In this process, both similar and dissimilar metal can be joined together by the combined action
of pressure and high temperature. The interdiffusion of atoms takes place from the clean
metallic surface and provides the strength to the composites. Major advantage of the process
includes that large variety of metal with control of orientation and volume reinforcement is
possible. High temperature and pressure, long processing time, inhomogeneous distribution
and difficult to achieve complex shapes are the major disadvantages.
1.3.2.2 Physical vapour deposition

The process involves continuous passage of fibre through a region of high partial pressure of
the metal to be deposited, where condensation takes place so as to produce a relatively thick
coating on the fibre. The vapour is produced by directing a high power electron beam onto the
end of a solid bar feed stock. Typical deposition rates are 5–10 µm per minute[2,8,12].
1.3.2.3 Powder metallurgy (PM)

In powder metallurgy process, thoroughly mixed elemental powders are compacted in a
suitable die to get the initial shape of final product. This simply compacted product do not have
any mechanical strength, known as green samples. To impart the strength, green samples are
heated in a furnace at a temperature below its melting point. This heating process is known as
sintering process and usually performed in controlled atmosphere to prevent the samples from
oxidation. Therefore, PM process mainly involves three basic steps: (a) mixing of powders (b)
compaction of mixed powders (c) sintering. When more than one type of powders are used
mixing is performed to get homogeneous mixture. Depending upon the requirements the
compaction can be performed in single and double acting dies. The compaction is usually
performed at room temperature. Sintering promotes the fast diffusion of atoms of consolidated
samples to impart the required the strength. The powder metallurgy is equally competitive than
other fabrication technique like casting, forging and machining. High strength and wear
resistance materials can be easily fabricated through PM technique. The main benefits of PM
process are as follows: (a) homogeneous distribution of mixed powders, (b) complex shapes
and near net shaped products can be fabricated, and (c) processing temperature is low hence
unwanted interfacial reactions are prevented. Further, elimination of casting defect such as
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blow holes, shrinkage and inclusions. However, PM is economical only in mass production
because of high tooling cost of dies and cost associated to development of elemental powders.
The biggest consumers of P/M parts at present are automotive industries. Hardware, tools,
cameras, farm and garden equipment industries, business machines, sporting goods and
military products are just a few more areas where usage is on the upswing [3,13,14].
Some fast sintering techniques are developed in recent years like electric resistance sintering,
micro wave sintering and spark plasma sintering. Inclusion of new sintering techniques have
imparted superior mechanical strength and wear resistance to developed materials. Further,
production rate have also be escalated by using recent sintering techniques. The detail
explanation of each sintering processes are discussed below:
Electric resistance sintering: The major drawback of hot pressing is the availability of high
temperature resistant material. This problem is eliminated by using electric resistance sintering
because in this approach material is heated not the die. A low voltage (around 10 V) high
current (typically> 5 kA/cm2) transformer is used to generate the high amperage of current that
flows to the samples which is subjected to pressure. The temperature of samples rises due to
flow of current, Joule’s heating, which promotes the bonding of particles. Electrical resistance
sintering (ERS), was already described in 1933 by Taylor [15] and later modified by Cremer
[16] in 1944. Highly conductive materials of small size can easily consolidated at laboratory
scale through ERS process [17–19]. However, its usage can be further extended for materials
with lower electrical conductivity like composites and cermets by incorporating medium
voltage machines. The difference between conventional hot pressing and ERS process are as
follows: (a) ERS takes very short processing time that eliminates protective environment (b)
die is not heated only powder is heated due to flow of current (c) difference in pressure and (d)
cooling of samples are very fast in ERS process.
Micro-wave sintering: In microwave sintering body is heated by radiant/resistance heating
followed by transfer of thermal energy via conduction to the inside of the body. Complete
volume of body being heated by the conversion of electromagnetic energy into thermal energy.
This phenomena is instantaneous, rapid and highly efficient. The microwave part of the
electromagnetic spectrum corresponds to frequencies between 300 MHz and 300 GHz.
However, most research and industrial activities involve microwaves only at 2.45 GHz and
915 MHz frequencies. The heating rates is more than 100°C min-1 for powdered metals because
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they are very good absorbers of microwaves. The degree of microwave absorption, and
consequently of heating, changes dramatically with temperature[20].
Spark plasma sintering (SPS): In this approach, low voltage, pulsed d.c. current and pressure
are used to perform sintering. New compounds and dense materials can be fabricated by SPS
technique in one step [21]. It differs from hot pressing due to different phenomena of heat
production and transmission to materials. The set up consists of dies (graphite die), punch
(conducting material), compaction unit coupled with low voltage (typically below 10V) high
d.c. (typically from 1 to 10 kA) transformer. The process operated under controlled
atmosphere. Pulsed direct current along with load (50 and 250 kN) is applied for few
milliseconds to get dense network. Maximal temperature achieved by using standard graphite
tools lies up to 2400 °C.
1.4 Wear
The progressive loss or damage of material from one or both surface under relative motion
(sliding, rolling, or impact motion) is known as wear. The wear phenomena generally occurs
due to surface interactions at asperities. The physico-mechanical characteristics and physical
condition of surface are considered by the researcher to develop various wear theories.
In 1938 Holm developed wear theory based on atomic mechanism and calculated volume wear
loss of substrate over unit sliding path. Burwell and Strang (1952), Archard (1953) and Archard
and Hirst (1956) developed the adhesion theory of wear and proposed a theoretical equation
identical in structure with Holm’s equation. In sliding, a fixed volume of material is subjected
to many times repeated action, which weakens the material and finally leads to rupture.
The amount, size, shape, and distribution of fibers or hard/soft particles embedded into the
matrix have some effects on the wear and friction performance of the composites. In addition,
the interfacial bonding between the reinforcements and the matrices is another important factor
which affects the mechanical and tribological properties of the MMCs. Generally, it is an
admissible opinion that the hard particles as reinforcements in the matrix increase the strength
and wear resistance of MMCs; however, it decreases the ductility of the composites. On the
other hand, soft particles usually act as a solid lubricant and hence decrease the friction
coefficient of the MMCs [22]
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In the last two decades numerous studies of wear properties of aluminium based metal matrix
composites with different type of reinforcements has been studied. Their results show that the
wear behaviour of particulate reinforced aluminum composite is significantly affected by
volume fraction of reinforcement and particle size [23]. The four basic types of wear
mechanisms are given below and it is shown in Figs 1.1-1.4.
 Adhesive wear.
 Abrasive wear.
 Erosive wear.
 Surface-fatigue wear.
1.4.1 Adhesive wear
The material loss due to failure of localized bond during sliding environment from one or both
of the surface is known as adhesive wear. The continuous contact of surfaces are necessary for
the initiation of adhesive wear. It can be controlled by the application of lubricating film, which
inhibits direct contact. The phenomena of adhesive wear can be clearly understand by the Fig.
1.1 as shown below.
Figure 1.1 Schematic representation of the abrasive wear mechanism [24].
1.4.2 Abrasive wear
Abrasive wear is the most common which is responsible for wear loss encountered in actual
practice. It occurs when a hard surface cuts a groove on the other mating surface during sliding
environment. Abrasive wear depends upon various factors such as size, shape of abrasive,
content, hardness of the sliding surface, loading conditions and environment. Latest industrial
survey revealed, largest amount of material is lost due to abrasive wear [25]. A typical abrasive
wear is shown in the Fig. 1.2.
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Figure 1.2 Schematic representation of the abrasive wear mechanism[24].
1.4.3 Erosive wear
The loss of material due to impingement of solid particles on the metal surface is known as
erosive wear. The liquid or gas, which may or may not carry foreign particles, impinges on the
surface caused erosive wear. It is similar to abrasion when the angle of impingement is small.
However, large impingement angle dislodged the material due to plastic flow. An example for
erosive wear is shown in the Fig. 1.3.
Figure 1.3 Schematic representation of the erosive wear mechanism[26].
1.4.4 Surface-fatigue wear
When a metal wheels on tracks or a ball bearing rolling in a machine runs initiates surface
fatigue wear due to repeated high stress. This repeated stress promotes subsurface cracks in
either the moving or the stationary component. As a result material fails in the form of large
particles, leaving pits on surface, due to propagation of initiated cracks. Surface-fatigue wear
is the most common form of wear affecting rolling elements such as bearings or gears. For
sliding surfaces, adhesive wear usually proceeds sufficiently rapidly that there is no time for
surface-fatigue wear to occur. An example for erosive wear is shown in the Fig.1.4.
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Figure 1.4 Schematic representation of the surface fatigue wear mechanism [27].
1.5 Need of reinforcements
Recently, material scientists and engineers are continuously working to develop new and
advanced method to enhance the friction and tribological behaviour of aluminium matrix
composites. Coating is one of the method to reduce the friction. The coefficient of friction of
aluminium could be reduced to 0.1 by using diamond-like carbon (DLC) coating [28]. The
other and most widely used method to improve tribological behaviour is to embed hard ceramic
particles. Wide variety of ceramic particles are reinforced in metal matrix. However, most
commonly used ceramics which are being used are Al2O3, SiC, and B4C. Their addition
remarkably improves the mechanical properties of MMCs. Further, their addition also
enhances the wear resistance and frictional co-efficient of composites [29,30]. The following
are the main factors related to reinforcement which affect the tribological performance of
aluminium matrix composites are: (a) volume/weight fraction (b) reinforcement size (c)
reinforcement shape. Apart from improving the tribological properties of aluminium matrix
composites appropriate selection of reinforcement and their amount improves other physical,
thermal and mechanical properties.
1.5.1 Silicon carbide (SiC) as a reinforcement
Most widely used ceramic particles which falls under the category carbide nature is silicon
carbide. It exhibits remarkable wear and thermal shock resistance. It shows good mechanical
behaviour at high temperatures. Silicon carbide is used extensively for mechanical seals
because of its chemical and wear resistance. SiC is an artificial (man-made) mineral known for
its very high hardness and abrasion resistance. Common applications include pump seals, valve
components, and wear-intensive applications such as rollers and paper industry retainers [31].
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1.5.2 Zirconia (ZrO2) as a reinforcement
Zirconia ceramics have special ability to absorb great amounts of stress relative to other
ceramic materials. It exhibits the highest mechanical strength and toughness at room
temperature. Zirconia has excellent wear, chemical and corrosion resistance, and low thermal
conductivity. Due to its excellent fracture toughness zirconia is now accepted by the researcher
to reinforce in aluminium matrix to prevent the failure during service. Common applications
include extrusion dies, wire and pipe extension, guide and other wear rollers, pressure valves,
and bearing materials.
1.5.3 Graphite as a reinforcement
The addition of hard ceramic particle enhances the physical, mechanical and wear behaviour
of the matrix material. This increase in properties are achieved at the cost of ductility and
fracture toughness. Further, addition of hard ceramic reinforcement enhances the hardness and
causing the machining difficult and uneconomical. So, it is a challenge for the researcher to
create a balance between hardness, fracture toughness, wear resistance and machining of the
ceramic reinforced composites. Aluminium metal matrix reinforced with graphite is one of the
most preferred combination because graphite enhances both the wear resistance and
machinability of the composites. During sliding condition graphite forms a thin layer which
prevents direct metal to metal contact and thus reducing wear loss.
In general, addition of graphite particles as reinforcement to an aluminum matrix enhances

tribological properties compared to aluminum composite reinforced with other ceramic
particles such as Al2O3 and SiC [32]. There is a significant reduction in friction and wear rate
in self-lubricating composites in comparison with unreinforced matrix alloys as a result of
incorporation of graphite particles [33]. Furthermore, the addition of graphite particles
decreases the frictional heat generated at the interface by its intrinsic lubrication behavior. This
will consequently increase wear resistance due to the reduction in friction force [34].
1.6 Fabrication of aluminium matrix composites
Alpas and Zhang [35] studied dry sliding wear behaviour of cast aluminium alloys (A356)
reinforced with SiC particles. The effect of SiC (10-20 vol. %) reinforcement, applied load (1-
150N) and sliding speed (0.16 and 0.8 ms-1) were investigated. Scanning electron microscopy
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and X-ray diffraction analysis were used to identify the effect of SiC particles on wear
mechanism. It was found that SiC particles acts as a load bearing agent and their abrading
action creates an iron-rich layer between the rubbing surfaces which is responsible for the
enhanced wear resistance of composite over unreinforced alloy.
Iwai et al. [36] investigated wear properties of aluminium alloy (Al2024) composite reinforced
with silicon carbide (whisker, 0-16 vol. %) fabricated through powder metallurgy technique.
The test materials of a disk were rubbed against a 0.45% carbon steel counterface pin at 40 N
and 0.1 m s-l. Initially the wear rate is severe but it become mild at large sliding distances for
both unreinforced matrix and composites. The wear rate decreases by the increase in volume
fraction of SiC in severe zone, because whiskers prevent propagation of wear cracks. While in
mild wear, the wear rate decreased with SiC addition because the wear particles became
smaller due to surface hardening. Therefore it was concluded that the SiC reinforcement can
improve the wear resistance of aluminum alloy for both severe and mild wear.
Ma et al. [37] fabricated SiC particles reinforced Al2024 composites by powder metallurgy
and the effect of size, concentration and load on tribological behaviour have been studied. He
concluded that reinforcement size is more significant than concentration for improving wear
resistance.
Al-Rubaie et al. [38] studied two-body abrasive wear behaviour of aluminium matrix
composites reinforced with silicon carbide particles fabricated through powder metallurgy
followed by hot extrusion process. The size (10, 27 and 43 µm) and concentration of SiC (5,
10 and 20 vol. %.) particles have been varied and wear test have been carried on pin-on-disc
wear tester against two different abrasive (silicon carbide and alumina) grits. They have
concluded three major findings which are as follows: (a) the improvement imparted by the SiC
reinforcement generally was higher against alumina than against silicon carbide for all grits
tested (b) at constant volume fraction of SiC reinforcement, the abrasion resistance increased
with an increase in the reinforcement size within the range studied (c) plastic deformation
(micro cutting and micro ploughing) was identified as the main wear mechanism operating on
the worn surfaces of the composites studied.
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Acilar and Gul [39] et al fabricated aluminium silicon carbide composite by vacuum infiltration
technique and its wear behaviour have been explored at applied load (12, 24 and 36 N) and
sliding distance (2.2, 3.6 and 5.0 km) with fixed sliding speed 1.0 m/s. The volumetric wear
rate have been increased with sliding distance and applied load. Worn surfaces were also
examined using SEM morph graphs.
Gul and Acilar [40] studied the effect of volume fractions of SiC (0–40 vol. %) particles on
wear behaviour of Al–10Si/SiCp composites produced by vacuum infiltration technique. Tests
were carried out on pin-on-disc wear tester with applied loads of 12, 24 and 36 N with a fixed
sliding speed of 1.0 m/s. Worn test specimens were examined by a scanning electron
microscope (SEM) and energy dispersive X-ray analysis (EDAX) to understand mechanisms.
The volumetric wear rate increased with increasing applied load while it decreased with
increasing volume fraction of the SiCp. The results showed that the wear mechanism was
oxidation at low load levels and adhesion and delamination at high load levels in the composite
having low volume fraction of reinforcement.
Hassan et al. [41] studied the wear behaviour of Al–Mg–Cu alloys with different weight
percentage of Cu (0, 1, 2, 3, 4, and 5 wt%) and corresponding metal matrix composites
reinforced with 5 or 10 vol% silicon carbide particles (SiC) fabricated via powder metallurgy
technique. He concluded that both hardness and wear resistance were enhanced by the addition
of Cu and/or SiC to the Al-4 wt% Mg alloy. The formations of mechanically mixed layer
(MML) as a result of material transfer from counter face disk to the samples and vice versa
were observed in all tested specimens.
Hassan et al. [42] explored the wear behavior of Al–Mg–Cu alloys and Al–Mg–Cu–based
composites containing SiC particles fabricated through slurry casting method. He found that
the silicon carbide particles play a significant role in improving wear resistance of the Al–Mg–
Cu alloying system. The formation of mechanically mixed layer (MML) due to the transfer of
Fe from counterface disk to the pin was observed in both Al–Mg–Cu alloys and Al–Mg–
Cu/SiC composites.
Kumar et al. [43] studied the mechanical and tribological properties of Al6061–SiC (2–6 wt.
%) composites prepared using liquid metallurgy route. The experimental results showed that
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the density of the composites increase with increased SiC content and agrees with the values
obtained through the rule of mixtures. The hardness and ultimate tensile strength of Al6061–
SiC composites were found to increase with increased SiC content in the matrix at the cost of
reduced ductility. The wear properties of the composites containing SiC were superior to that
of the matrix material.
Mazahery and Shabani [44] explored the effect of size of SiC (1, 5, 20 and 50 μm) particles
and volume fraction (5%, 10% and 15%) on the microstructure and tribological properties of
Al-based composite. Composites were produced by applying compo casting process.
Tribological properties of the unreinforced alloy and composites were studied using pin-on-
disc wear tester, under dry sliding conditions at different specific loads. It has been found that
the hardness of tested materials increases with the increase of SiC particles amount. The matrix
hardness exerts a strong influence on the dry sliding wear behaviour of the SiC particles
reinforced composite and the composite with the lowest matrix hardness displays the lowest
wear rate.
Shirazi et al. [45] studied the corrosion, corrosive wear and dry sliding wear of Al/SiC
nanocomposites synthesized by mechanical milling, cold pressing and hot extrusion. The
microstructures of the samples and their worn surfaces were examined using scanning electron
microscopy. It was shown that the dry sliding wear and corrosion resistance of these
nanocomposites were improved with the increase of SiC content. The prominent wear
mechanism in the unreinforced alloy was adhesive wear. However, for Al/SiC nanocomposites
the wear mechanism changed to abrasive.
Goudarzi and Akhlaghi [46] investigated the dry sliding wear behaviour of Al 5252 alloy and
its composites reinforced with nanometric or micrometric SiC particles. The wear tests were
conducted on hot extruded samples using a pin on the disc configuration under normal stresses:
0.3, 0.6 and 0.9 MPa at a sliding speed of 0.5 m/s and distance of 1000 m. The composite
reinforced with micrometric SiC particles showed the lowest wear rate at the applied stresses
of 0.3 and 0.6 MPa, while the nano-composites exhibited the best wear resistance at the normal
stress of 0.9 MPa.
15 | P a g e
Manivannan et al. [47] studied the wear characteristics of aluminum alloy Al6061, and its
nanocomposites, Al6061/nano-SiC processed by Liquid metallurgy method. The experiments
were conducted in pin-on-disk setup by varying the parameters load at 10N, 20N, 30N, 40N,
and sliding speed at 0.5m/s with a distance of 1000m. The worn samples and wear debris were
analyzed under a Field Emission Scanning Electron Microscope (FESEM) equipped with an
Energy Dispersive Spectrometer (EDS) to understand the wear mechanisms. The wear test
result shows that Al6061- SiC nanocomposites exhibited improved wear resistance than the
Al6061 alloy. Worn surface analysis shows different dominant mechanisms, like abrasion,
delamination, oxidation and adhesive at different applied loads.
Jiménez et al. [48] fabricated aluminium matrix-zirconia nanoparticles reinforced composites

by the infiltration technique. The wear resistance of zirconia-modified aluminium was
significantly improved due to the presence of the ceramic nanoparticles embedded into the
matrix.
Fuentes et al. [49] synthesized a novel aluminium–zirconia composite, with improved wear
resistance. The method consists of compacting aluminium powder mixed with cellulose fibres,
which are then eliminated by a heat treatment. The compacted piece was immersed several
times in a colloidal (i.e. nanosized) zirconia solution until a constant weight was reached. The
solution penetrated and infiltrated the preform. Then, the aluminium matrix presented zirconia
tetragonal and monoclinic phases. Wear test was carried out in a pin-on-disc machine. By
measuring the weight loss it was shown that the composite had significant improvement in
wear resistance, as compared to pure aluminium.
Uthayakumar et al. [50] studied the dry sliding wear behavior of aluminum reinforced with 5%
SiC and 5% B4C hybrid composite fabricated through stir casting process using a pin on disc
tribometer. Wear performance of the hybrid composites were evaluated over a load ranges of
20–100 N, at the sliding velocities from 1 to 5 m/s. Detailed metallurgical examination and
energy dispersive analysis were carried out to assess the effect of SiC and B4C particles on the
wear mechanisms. The experimental results show that the hybrid composites retain the wear
resistance properties up to 60 N load and sliding speed ranges 1–4 m/s. The enhancement of
wear resistance with small amount of SiC and B4C is achieved by the cooperating effect of
reinforcement particles.
16 | P a g e
Rajmohan et al. [51] studied the mechanical and wear properties of hybrid aluminium matrix
composites. Mica and SiC ceramic particles were incorporated into Al 356 alloy by stir-casting
route. Microstructures of the samples were studied using scanning electron microscope (SEM).
The chemical composition was investigated through energy dispersive X-ray (EDX) detector.
The results indicate that the better strength and hardness are achieved with Al/10SiC−3mica
composites. The increase in mass fraction of mica improves the wear loss of the composites.
Basavarajappa et al. [52] studied the dry sliding wear behavior of Al 2219 alloy and Al
2219/SiCp/Gr hybrid composites. The composites are fabricated using the liquid metallurgy
technique. The dry sliding wear test is carried out for sliding speeds up to 6 m/s and for normal
loads up to 60 N using a pin on disc apparatus. It is found that the addition of SiCp and graphite
reinforcements increases the wear resistance of the composites. The wear rate decreases with
the increase in SiCp reinforcement content. As speed increases, the wear rate decreases initially
and then increases. The wear rate increases with the increase in load. Scanning electron
microscopy micrographs of the worn surface are used to predict the nature of the wear
mechanism. Abrasion is the principle wear mechanism for the composites at low sliding speeds
and loads. At higher loads, the wear mechanism changes to delamination.
Radhika and Subramanian [53] fabricated AlSi10Mg alloy reinforced with 3, 6 and 9 wt-%
alumina with constant 3 wt.% graphite particles composite stir casting technique.
Microstructural investigations as well as evaluation of mechanical properties such as hardness,
tensile strength and double shear strength were conducted on composites and unreinforced
alloy specimens. Tribological behaviour of hybrid composites was studied using pin on disc
test machine. Worn out surfaces were analyzed using scanning electron microscopy, and wear
debris were analyzed using X-ray diffraction. Results revealed that the mechanical properties
of hybrid composites were higher than unreinforced alloy. Dry sliding wear test results
indicated that the aluminium alloy reinforced with 9 wt-% alumina and 3 wt-% graphite has
highest wear resistance compared to unreinforced alloy.
Ravindran et al. [54] fabricated and studied the tribological behaviour of aluminium (Al)-based
graphite (Gr) and silicon carbide (SiC) particle reinforced hybrid composite materials by
powder metallurgy. It was found that with an increase in the SiC content, the wear resistance
increased monotonically with hardness. The hybridization of the two reinforcements also
17 | P a g e
improved the wear resistance of the composites, especially under high sliding speeds. The
composite with 5 wt. % Gr and 20 wt. % SiC showed the greatest improvement in tribological
performance. The wear mechanism was studied through worn surface and wear debris analysis
as well as microscopic examination of the wear tracks.
Baradeswaran and Perumail [55] investigated the influence of graphite on the wear behavior
of Al 7075/Al2O3/5 wt. % graphite hybrid composite fabricated using liquid metallurgy route.
Ceramic particles along with solid lubricating materials were incorporated into aluminium
alloy matrix to accomplish reduction in both wear resistance and coefficient of friction. The
Al 7075/Al2O3/graphite hybrid composite was prepared with 5 wt. % graphite particles
addition and 2, 4, 6 and 8 wt. % of Al2O3. The hardness, tensile strength, flexural strength and
compression strength of the Al 7075–Al2O3–graphite hybrid composites are found to be
increased by increased weight percentage of ceramic phase. The wear properties of the hybrid
composites containing graphite exhibited the superior wear-resistance properties.
Hayajneh et al. [56] used neural network in prediction of wear loss quantities of aluminum–
copper– silicon carbide composite materials. Effects of addition of copper as alloying element
and silicon carbide as reinforcement particles to Al–4 wt.%Mg metal matrix have been
investigated. Different Al–Cu alloys and composites were subjected to dry sliding wear test
using pin-on-disk apparatus under 40N normal load with rotational speed of counter face disk
of 150rpm at room conditions (∼20 ◦C and∼50% relative humidity). The experimental results
were firstly coded prior to training in a feed forward back propagation artificial neural network
(ANN) and the results were compared with experimental results. The average value of absolute
relative error of un-coded values reaches 2.40%.
Shabani and Mazahery [57] applied a combination of artificial neural network and finite
element technique in order to predict the wear properties of A356 unreinforced alloy and
composites with different vol. % of boron carbide particles. It is observed that predictions of
ANN are consistent with experimental measurements for A356 composite and considerable
savings in terms of cost and time could be obtained by using neural network model.
Ravindran et al. [58] studied the wear and sliding friction response of a hybrid aluminium
metal matrix composite reinforced with hard ceramic (5 wt.% of SiC) and soft solid lubricant
18 | P a g e
(0, 5, and 10 wt.% of graphite) fabricated by powder metallurgy. Analysis of variance
(ANOVA) was used to investigate the influence of the parameters on both the wear rate and
the coefficient of friction. The hardness of the composites decreases as the % of graphite (Gr)
increases. The wear and friction coefficient were mainly influenced by both the sliding distance
and the load applied. The morphology of the worn out surfaces and the wear debris was
analysed to understand the wear mechanisms. The wear resistance of the hybrid composite
containing 5 wt.% SiC and 5 wt.% graphite is superior to that of the graphite free composites
and the other hybrid composites. Further, ANOVA shows that the most significant variables
affecting the sliding wear of composites (in terms of their individual percentage contributions)
are the sliding distance (56.74%), sliding speed (13.40%), applied load (13.49%), and graphite
content in the composite (11.67%), as well as the interaction effect of the load with the sliding
speed (2.01%), within the selected range of investigations.
Ravindran et al. [59]employed an orthogonal array, the signal-to-noise ratio and analysis of
variance to study the optimal testing parameters using Taguchi design of experiments.
ANOVA showed that the most significant variables affecting the sliding wear of the
composites (in terms of their individual percentage contributions) were the sliding distance
(57.12%), sliding speed (12.43%), applied load (13.78%) and graphite content in the composite
(11.23%) within the selected range of investigations.
Özyürek et al. [60] studied the wear properties of SiC particle reinforced aluminium (A356)
composite materials (MMCs), produced with thixomoulding method, by experimental and
Artificial Neural Network (ANN) model. Two different temperatures (590ºC and 600ºC) were
used in production of the MMCs containing 5%, 10%, 15 % and 20% SiC (vol%). The samples
of MMC were tested at 2 ms-1 constant sliding speed under 30N and 60N loads against four
different sliding distances (500, 1000, 1500, and 2000m). In the theoretical prediction model
of the MMCs, weight loss, SiC per cent, production temperature, applied weight and sliding
distance were used as input values. After comparing the experimental results and the ANNs
predicted data it was observed that R2 was 0.9855. This shows that the developed prediction
model has a high level of reliability.
Baradeswaran et al. [61] fabricated aluminium alloy (AA) 6061 and 7075 composites
reinforced with 10 wt. % of boron carbide (B4C) and 5 wt. % of graphite through liquid casting
19 | P a g e
technique. The wear experiment was carried out by using a pin-on-disc apparatus with various
input parameters like applied load (10, 20, and 30 N), sliding speed (0.6, 0.8, and 1.0 m/s) and
sliding distance (1000, 1500, and 2000 m). Response Surface Methodology (RSM) using
MINITAB 14 software was used to analyse the wear rate of hybrid composites and aluminium
alloys. The graphical and analytical results of RSM show the optimum combination of applied
load (10 N), sliding speed (0.8 m/s) and sliding distance (2000 m) for the minimum wear rate.
Stojanovic et al. [62] analyzed the influence of graphite reinforcement, load, sliding speed, and
sliding distance on tribological behavior of A356 aluminum matrix composites reinforced with
silicon carbide and graphite using the full-factorial design. The wear rates of A356/10SiC
composite material and A356/10SiC/1Gr and A356/10SiC/3Gr hybrid composites have been
analyzed. The composites were obtained by a modified compocasting procedure. Tribological
tests were performed on a block-on-disc tribometer without lubrication. The testing included
sliding speeds of 0.25 and 1.0 m/s, normal loads of 10 and 20 N, and sliding distances of 300
and 900 m. The analysis of the obtained results was performed using the full factorial method
based on the signal-to-noise (S/N) ratio. The effects of load, sliding speed, weight percentage
of graphite reinforcement, and sliding distance on the wear rate are 38.99, 17.87, 13.95, and
11.25%, respectively. The best tribological characteristics were exhibited by the
A356/10SiC/1Gr hybrid aluminum composite.
1.7 Research gap related to aluminium matrix composites
After going through the exhaustive literature regarding the fabrication and properties of
aluminium matrix composites, it has been found that powder metallurgy offers remarkable
advantages over other fabrication techniques like stir casting, squeeze casting and compo-
casting etc. because of its low manufacturing temperature, which avoids strong interfacial
reactions, and minimizes undesired reactions between the matrix and the reinforcement. An
additional advantage of powder metallurgy is the uniformity in the reinforcement distribution.
This uniformity improves not only the structural properties but also the mechanical strength as
well as imparts high wear resistance.
Further, special attention is given to literature which emphasizes the enhancement of

morphological and tribological properties. From the literature it has been found that
20 | P a g e
incorporation of hard ceramic reinforcements improves the wear resistance of composites
because hard particles acts as a load bearing agent for the soft aluminium matrix. Some authors
also reported that particle size is more significant in comparison to amount of reinforcement
for controlling the wear loss. The addition of hard micro-sized ceramic reinforcement
deteriorates the ductility of composites which can be controlled by the addition of nano-sized
reinforcement. Therefore, a combination of micro and nano particles reinforcement could be a
better option for the development new and advanced metal matrix composites. Hence, the
combination possesses great potential, scope and opportunities for the researchers. Further,
statistical and soft computing techniques are required to predict and optimize the process
parameters in order to reduce the cost and time required for the exhaustive experimentation.
Although some studies have been reported on the aluminium matrix composites reinforced
with single micro and nano ceramic reinforcements but very little attention is given to the
composites reinforced with both micro and nano-sized particles.
Some of the limitations identified based on the literature survey of the topics are listed below:
i. From the past literature, it is observed that a vast number of investigations are
performed on aluminium composite reinforced with micro and nano silicon carbide
fabricated through powder metallurgy technique. However, no detailed findings are
available for the simultaneous addition of both micro and nano-sized silicon carbide in
aluminium matrix.
ii. Limited study is present on non-conventional sintering process of aluminium matrix
composites.
iii. Amongst various available ceramic, zirconia is least used as a reinforcement in
aluminium matrix. However, fracture toughness and wear properties of zirconia are
very high.
iv. Limited study have been made on aluminium composites involving both micro silicon
carbide and nano zirconia reinforcements even though it is very interesting and
provides scope to overcome harsh tribological challenges.
v. According to the best of author’s knowledge limited study have been made on
aluminium composites reinforced with both nano-zirconia and soft graphite. However,
21 | P a g e
it is very interesting combination and can be utilized at a location where application of
lubrication externally is difficult.
vi. Factorial technique, statistical analysis and Artificial Neural Network (ANN) methods
have not been implemented so far to estimate mechanical and tribological behaviour of
the aluminium matrix composites.
1.8 Objectives of the research work
The objective of this research is to fabricate the aluminium matrix composite reinforced with
micro and nano particles. The composites are fabricated by powder metallurgy technique using
conventional and non-conventional sintering technique. The morphological and tribological
behaviour of various composites have been investigated with the following specific objectives:
i. Fabrication of aluminium composites reinforced with micro silicon carbide and nano
zirconia by powder metallurgy technique.
ii. Analysis of wear performance of Al-SiC-ZrO2 composites on pin-on-disc wear tester.
iii. Analysis of tribological behaviour of Al-SiC-ZrO2 composites using statistical and
artificial neural network techniques. Analysis of variance (ANOVA) is also performed
to find out the percentage contribution of each process parameter on wear loss of
composites.
iv. To fabricate aluminium matrix composites reinforced with micro and nano silicon
carbide particles by powder metallurgy technique.
v. The tribological behaviour of fabricated composites have been explored at different
process parameters using pin-on-disc wear tester.
vi. Fabrication of aluminium composites reinforced with zirconia nanoparticles and soft
graphite particles by powder metallurgy technique.
vii. Analysis of wear behaviour of Al-ZrO2-Gr hybrid composites using pin-on-disc wear
tester.
viii. Full factorial design of experiment, Analysis of variance (ANOVA) and Artificial
Neural Network (ANN) were used for the quantitative analysis of each process
parameter on wear behaviour of developed composites. Further, regression models
were developed to estimate the wear loss of composites within the selected range of
22 | P a g e
investigation. The statistical analysis were performed using MINITAB-17 software
package.
ix. Fabrication of aluminium composites reinforced with micro and nano-silicon carbide
using non-conventional sintering process (Electric resistance sintering). Analysis of
wear behaviour is also performed.
x. The morphological study of all the fabricated composites is done using X-ray
diffractometer (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive
Spectroscopy (EDS) and elemental mappings.
xi. The worn surfaces and wear debris are also analyzed using SEM to understand the wear
mechanisms.
23 | P a g e
2. Materials and Experimental Procedure
This chapter deals regarding particles used, experimental procedures and equipment used for
investigation of fabricated composites. In this work, different aluminium matrix composites
have been fabricated through powder metallurgy technique. Ceramic particles such as silicon
carbide (micro and nanoparticles) and zirconia (nanoparticles) were reinforced in aluminium
matrix. Further, in one such combination graphite particles were also reinforced along with
ceramic particles.
2.1 Materials
2.1.1 Aluminium Powder
Aluminium powder (99.9% pure) was procured from Otto Chemicals ltd. Mumbai (India). The
average particles size (APS) range was 10 μm. The SEM of as-received powder is shown in
Fig.2.1.
Figure 2.1 SEM micrographs of as-received aluminium powders.
2.1.2 Silicon Carbide (Micro and Nanoparticles)
Silicon carbide micro and nanoparticles (SiCn) were purchased from Otto Chemicals ltd.
Mumbai (India). The APS are 37 μm And 50 nm respectively. The SEM of as-received
particles are shown in Fig. 2.2(a-b).
24 | P a g e
(a) (b)
Figure 2.2 SEM micrographs of as-received (a) SiC micro-particles (b) SiC nano-particles
2.1.3 Zirconia nanoparticles (ZrO2)
Zirconia nanoparticles were purchased from Nano Labs, (India). The APS of zirconia is 30–
50 nm. The SEM of as-received particles is shown in Fig. 2.3.
Figure 2.3 SEM micrographs of as-received nano-zirconia (ZrO2) powders
2.1.4 Graphite particles
Graphite particles were purchased from Otto Chemicals ltd. Mumbai (India). The APS of
graphite is 37 µm. The SEM of as-received particles is shown in Fig. 2.4.
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Figure 2.4 SEM micrographs of as-received graphite powders
2.2 Experimental Set-up
The composites have been fabricated through powder metallurgy process, which
involves various stages viz. measurement of elemental powders, mixing of powders,
compaction and sintering.
2.2.1 Measurement and mixing of elemental powders
The required amount of aluminium powder and ceramic particles were weighed using digital
weighing machine having least count 0.01 mg. The digital weighing machined used during the
experimental work is shown in Fig. 2.5. The calculated ratio of soft aluminium powder and
ceramic particles were thoroughly mixed in centrifugal ball mill as shown in Fig. 2.6 in order
to get homogeneous mixing 10:1 ball to powder ratio (BPR) was maintained throughout mixing
[59]. The mixing speed and time were 150 rpm and 20 min. respectively. Uniformly mixed
powders were then compacted in uniaxial hydraulic pallet press machine as shown in Fig.
2.7(a). A suitable die and punch assembly and fabricated sample is shown in Fig. 2.7(b-c).
After every compaction process the die wall was cleaned and lubricated with zinc stearate
manually for proper functioning of the die
26 | P a g e
Figure 2.5 Digital weighing machine Figure 2.6 Centrifugal ball mill
2.2.2 Compaction of elemental powders
(a) (b)
(c)
Figure 2.7 Uniaxial hydraulic pallet press (a), Punch, die (b), and fabricated samples (c).
(Powder Metallurgy Lab. Mechanical Engineering Department, AMU)
27 | P a g e
2.2.3 Sintering of green pallets
The green specimens were sintered in tubular electric furnace attached with controlled
environment unit as shown in Fig. 2.8. The specimens were sintered at 450-470 0C for 60 min.
under the continuous flow of argon gas (flow rate=1litre/min.) for preventing the samples from
oxidation. The specimens were cooled down to the ambient temperature in the furnace itself.
Temperature controller
and flow regultor
Argon cylinder
Inlet tube
Figure 2.8 Electric tubular furnace for conventional sintering (PM Lab., MED)
25-Sep-18 7:09 PM 73
2.3 Morphological Characterizations
All the fabricated composites were characterized using most widely used characterization
techniques such as X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy
Dispersive Spectroscopy (EDS) and Elemental Mappings. They are discussed in detail in the
following sections.
2.3.1 X-Ray Diffraction
The X-ray diffraction measurements were carried out with the help of the XRD machine
(Bruker D8 Advance, XRD Lab, MED) using Cu Kα radiation (Kα= 1.54056À) at an
accelerating voltage of 40 kV and a current of 20 mA to analyze the XRD pattern of fabricated
composites. The XRD machine used for the analysis is shown in Fig. 2.9.
28 | P a g e
2.3.2 Metallographic Analysis
Metallographic analysis is very important investigation step to correlate the microstructure of

the material to the mechanical behaviour. In this investigation, composites microstructure were
studied using Scanning Electron Microscope at high magnification. Fig. 2.10 shows the
Scanning Electron Microscope (JEOL, Model No. JSM-6510LV, USIF, AMU). The Energy
Dispersive Spectroscopy (EDS) were also utilized to confirm constituents present in
specimens. Further, elemental mapping of the fabricated composites were also performed to
verify the distribution of reinforcement in the matrix material.
Figure 2.9 X -ray Diffraction machine
29 | P a g e
Figure 2.10 Scanning Electron Microscope
2.4 Density measurement
The densities of all fabricated composite were calculated using Archimedes’ principle, which
provides a convenient and accurate method for determining the volume of an irregular or
regular shaped object. The densities of the composite specimens were determined using a high
precision digital electronic weighing balance with an accuracy of 0.01 mg.
The experimental density was calculated using following relationship:
Mair
𝜌𝑐 = (M × 𝜌𝑤 ……………………………………………… [2.1]
air −Mwater )
Where, ρc is the density of composites, Mair is mass of composite in air, Mwater is mass of
composite in distilled water and ρw represents density of distilled water.
2.5 Rockwell Hardness Measurement
The hardness of the sintered composites were obtained using a Digital Rockwell hardness tester
(TRB-250 DM) with a steel ball of diameter of 1/8″ and a load of 600 N (Scale H). The tests
were performed at room temperature (i.e. 30 °C) and readings of hardness were taken at five
locations on every sintered sample to find a mean hardness value. The machine used for
measuring the hardness is shown in Fig. 2.11.
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2.6 Dry sliding wear test
A pin-on-disc apparatus (Ducom, Model No TR-201 CL, Bangalore, India), as shown in Fig.
2.12, was used to analyze the wear behaviour of fabricated composites. The test were
performed in accordance with the ASTM G99-95a (reapproved) standards. The wear tests were
performed at room temperature of 30°C and relative humidity of 60–65%. After every
experiment the specimen and counter disc were cleaned properly, using acetone to remove the
adhering wear debris. To determine the wear loss the specimens were weighed using a digital
weighing machine of least count 0.1 mg.
Figure 2.11 Digital Rockwell Hardness Figure 2.12 Pin-on-disc wear tester
PM Laboratory, MED Stress analysis and tribology laboratory, MED
31 | P a g e
3. Study of Mechanical and Tribological Behaviour of Al/SiC/ZrO2 Hybrid
Composites Fabricated Through Powder Metallurgy Technique
3.1 Introduction
In the last two decades, aluminium metal matrix composites has emerged as a promising
material because of its potential application in structural, aerospace and automobiles sectors
[58,61,63] The attractive properties of metal matrix composites (MMCs) such as low density,
high thermal conductivity and high specific strength along with comparatively low cost make
them as an attractive option. The final properties of the metal matrix composite depends upon
the uniform distribution of the reinforcement particle to achieve required mechanical properties
of the composites. So, in order to achieve homogeneous distribution many researcher adopted
different technique such as mechanical alloying, casting and powder metallurgy. Among all
fabrication technique, recently PM found more attention for MMCs synthesis because high
homogeneity, uniform reinforcement distribution and complex dimensional parts can be
produced. Due to this uniqueness, the cost involved in complex machining operation is almost
minimized and thus making the fabrication economical [64,65].
Currently, SiC [54], Al2O3 [66], B4C [67], Si3N4 [68], AIN [68], TiC [69] and ZrO2 [70] are
extensively used for reinforcing aluminium metal matrix composites to impart improved
mechanical properties. Moreover, aluminium matrix composite reinforced with combination
of micro-sized and nano-sized reinforcement have gained special research attention because of
improved mechanical and tribological properties. So, they are better alternative over single
reinforced composites [10]. Hybrid composite with micro-sized and nano-sized reinforcement
plays very important role when they are used as frictional materials. Nano particles enhances
the performance of the matrix due to Orowan strengthening mechanism. While, micro-sized
reinforcement supports the frictional load which improves the hardness and tribological
properties of the hybrid composites.
Among several ceramic reinforcements, SiC is widely used by recent researchers because it
has enhanced tribological and mechanical properties [54,71]. However, the enhancement in
properties of Al/SiC composites occur at the expense of ductility and fracture toughness.
Ductility and fracture toughness are important material properties that are necessary for
preventing catastrophic failure in service [72]. In addition, metal oxide shifts the brittleness of
32 | P a g e
SiC and enhances the fracture toughness of Al-SiC composites when used as a reinforcement
in hybrid composites as reported in the previous study [73,74]. Metal oxides are also
economical, widely available, environmental friendly and thus having potential to use as a
reinforcing material in the composites [73]. ZrO2 is a mineral metal oxide which is easily
available, less expensive, excellent thermal, mechanical and tribological properties [70].
Extensive survey on various research papers revealed that no detail findings are available for
Al-SiC-ZrO2 hybrid composites fabricated through powder metallurgy technique.
Therefore, in the present study the mechanical and tribological behaviour of Al/SiC/ZrO2
hybrid composites were investigated. The microstructure of the produced composites were
carried out using X-ray diffraction measurements (XRD), Scanning Electron Microscopy
(SEM), Energy Dispersive Spectroscopy (EDS) and elemental mapping. Furthermore, the
SEM morphology of worn surfaces were analyzed to understand the wear mechanism.
3.2 Experimental
3.2.1 Sample preparation
The details of reinforcement used in present work is given in Table 3.1. The size distribution
of the reinforcing particles were measured using particle size analyzer and shown in Fig. 3.1
[64]. For the analysis, the following combination of composites were fabricated.
i. Pure Al.
ii. Al+5%SiC.
iii. Al+5%SiC+3%ZrO2.
iv. Al+5%SiC+6%ZrO2.
v. Al+5%SiC+9%ZrO2.
Table 3.1 Details of reinforcement particles.
Reinforcement Mean diameter of powders Density, 𝐠/𝐜𝐦𝟑

SiC 37 µm 3.21
ZrO2 30-50 nm 5.89
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25 35
(a) (b)
30
20
Intensity percent
Intensity percent
25
15 20
10 15
10
5
5
0 0
13
15
21
28
34
41
55
70
0.04
0
2
5
9
200
0.1
0.6
0.5
0.4
0.9
1.7
13
18
25
45
0
2
5
9
100
Particle size, µm Particle size, µm
40
(c)
35
30
Intensity percent
25
20
15
10
5
0
1.9 8 17 25 31 37 44 49 53 60 78
Particle size, nm
Figure 3.1 The size distribution of as-received: (a) Aluminium powder, (b) SiC particles, (c)
ZrO2 particles.
The composites were fabricated through powder metallurgy technique. Firstly, the
predetermined amount of elemental powders were weighed by using a digital weighing
machine (Precisa, Swiss Made, ES 225SM-DR) having a least count 0.0001 g. The powders
were thoroughly mixed using a centrifugal type ball mill (FRITSCH, Germany) with 8 mm
diameter stainless steel balls with a ball to powder weight ratio of 10:1 to achieve
homogenization and to reduce the agglomeration of particles. The milling time and speed were
15 min and 100 rpm, respectively. In the next stage, the mixture of powders were compressed
in a uniaxial hydraulic pallet press (Type KE, Sr. No. 1327, Kimaya Engineers, India) at 585
MPa to obtain green compacts of 8 mm diameter and a height of 13 mm. The die wall was
lubricated manually using zinc stearate before every compaction process. The compacted
34 | P a g e
samples were sintered at 450-470 0C for 60 min. in a tubular furnace over argon atmosphere
(flow rate = 1.0 liter/min.), to avoid oxidation of aluminium matrix as suggested by
Umasankar [75]. The sintered samples were allowed to cool to the room temperature in the
furnace itself. The density of the samples were measured using Archimedes principle [65].
The measured density was compared to the value obtained using rule-of-mixture in order to
find out the porosity. The samples were weighed by using a digital weighing machine (Precisa,
Swiss Made, ES 225SM-DR) having a least count 0.001g. The hardness of sintered
composites were carried out by using a Digital Rockwell hardness tester (TRB-250 DM) with
a steel ball of diameter of 1/8” and a load of 600 N (Scale H). The tests were performed at
room temperature (i.e. 30 0C) and readings of hardness were taken at five different locations
on every sintered sample to find the mean hardness value. The XRD analysis of all the sintered
composites were performed using an X-ray diffractometer (D8 ADVANCE; Bruker AXS Inc,
Madison, WI, USA). A Cu Kα radiation (λ=1.5406 0A) X-ray source operating at 40mA and
40kV were used. XRD was performed in the 2θ range of 20°–70° with a step size of 0.01° and
a scanning rate of 0.02 steps/second.
3.2.2 Wear test
A pin-on-disc apparatus (Ducom, Model No: TR-201 CL, Bangalore, India) in accordance
with the ASTM G99-95a (reapproved) standards were used to analyze the dry sliding wear
behaviour of fabricated composites. The test condition and wear parameters are given in Table
3.2.
Table 3.2 Various wear test conditions and parameters.
Material and parameter Description

Composites All five synthesized composites
Pin dimension Diameter 8mm and height 13mm
Sliding velocity 1, 1.5, 2, 2.5 (m.s-1)
Sliding distance 300, 500, 700, 900 (m)
Applied load 20, 30, 40 (N)
Counter disc material EN31 grade steel, 65 HRC
35 | P a g e
The wear tests were performed at room temperature 300C and relative humidity of 60-65 %.
After every experiment the specimen and counter disc were cleaned properly by using acetone
to remove the wear debris adhered. To determine the wear loss the specimens were weighed
using a digital weighing machine of least count 0.1 mg.
3.3 Results and Discussion
3.3.1 Morphological study
Fig. 3.2 shows the XRD results of synthesized composites. The XRD gives the details about
the elements present in the manufactured composites. From XRD it can be concluded that
aluminum peak is largest among the identified compounds. The peaks of SiC and ZrO2 is also
found in the XRD gram. It is also evident from the XRD graph that no new peak is present.
Hence, the fabricated composites are reinforced with SiC and ZrO2. The calculations were
done using the software, DIFFRAC plus (Bruker AXS Inc).
The energy dispersive spectroscopy (EDS) analysis and the corresponding microstructure of
the synthesized composite is shown in Fig. 3.3. Al, Zr, Si, C and O peaks are observed in the
EDS analysis as shown in Fig. 3.3. So, EDS analysis confirms that SiC and ZrO2 particles are
present in the synthesized composites. Table 3.3 shows the elements present in the
Al+5%SiC+9%ZrO2 reinforced composites with their weight percentage and atomic
percentage.
36 | P a g e
Figure 3.2 XRD pattern of fabricated hybrid composites.
Figure 3.3 EDS spectrum of Al+5%SiC+9%ZrO2 reinforced composites.
Table 3.3 List of elements present in the Al+5%SiC+9%ZrO2 reinforced composites.
Elements Weight% Atomic%

C 34.22 51.15
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O 14.61 16.39
Al 44.82 29.82
Si 3.16 2.02
Zr 3.18 2.02
Total 100 100
Fig. 3.4 shows the elemental maps of Al+5%SiC+9%ZrO2 reinforced composite. From the
elemental maps of the composites it is obvious that Al, Zr, Si, C and O elements are present.
The elemental maps also confirms that the synthesized composite is reinforced with SiC and
ZrO2 particles.
38 | P a g e
Figure 3.4 Elemental maps of Al+5%SiC+9%ZrO2 hybrid composites.
3.3.2 Density, Porosity and Relative density measurement
Fig. 3.5 shows the variation of experimental and theoretical density with respect to micro and
nano- sized reinforcements. It has been observed that density of composites increase by the
addition of both SiC and ZrO2 particles. The reason of enhancement in the density is due to the
addition of higher density reinforcements in the aluminium matrix. Based on the theoretical
and experimental densities the porosity of all samples were measured and is shown in Fig. 3.6.
2.9
Theoritical density Experimental density

2.85
2.8
Density, g/cm3
2.75
2.7
2.65
2.6
2.55
Al Al+5%SiC Al+5%SiC+3%ZrO2 Al+5%SiC+6%ZrO2 Al+5%SiC+9%ZrO2
Figure 3.5 Influence of micro and nano reinforcements on densities of Al hybrid composites.
39 | P a g e
4
3
Porosity/ %
0
Al Al+5%SiC Al+5%SiC+3%ZrO2 Al+5%SiC+6%ZrO2 Al+5%SiC+9%ZrO2
Figure 3.6 Influence of micro and nano reinforcements on porosity of Al hybrid composites.
The addition of micro-sized SiC in aluminium matrix increases the porosity of the composite.
The increase in the porosity can be attributed to the high hardness of SiC which hinders the
proper compaction of composite powders. The increased porosity of Al/SiC composites has
also been reported by other researchers [6]. Furthermore, when nano ZrO2 particles are added
to the Al+5%SiC composite the porosity again shows increasing trend which can be explained
as follow: (a) Nano-sized reinforcements are more susceptible to agglomeration which in turn
inhibit effective densification. (b) Nano particle shows greater hardening effect as compared
to submicron particles which reduces the press ability of powders and hence a rise in porosity
is observed.
Fig. 3.7 shows the relative density of aluminium, aluminium composites and aluminium hybrid
nano composites. Relative density is defined as the ratio of experimental density to theoretical
density. Theoretical density is calculated using rule of mixture while experimental density is
calculated by Archimedes principal. The figure shows that as the SiC increases to 5 wt. %, the
relative density decreases sharply. The underlying reason of this decline is that hard SiC
particles do not flatten by plastic deformation during compaction and therefore creates the
inter-particle micro voids. Additionally, during sintering the SiC particles are very dense with
random distribution due to its high melting point. This dense network formed by micro SiC
particles prevents the specimen to be dense [6]. Further, addition of nano-ZrO2 in aluminium
composites decreases the relative density. This reduction in the relative density could be due
40 | P a g e
to the following reasons: (a) clustering and agglomeration of nanoparticles at high
concentration (b) high hardness of nano-ZrO2 particles hinders the compaction process [76].
100
Al
99.5
Al+5%SiC
99
Al+5%SiC+3%ZrO2
Relative density (%)
98.5 Al+5%SiC+6%ZrO2
98 Al+5%SiC+9%ZrO2
97.5
97
96.5
96
95.5
95
Figure 3.7 Variation of relative density of composites with ZrO2 addition.
3.3.3 Hardness measurement
Bar graph as shown in Fig. 3.8 illustrating the Rockwell hardness of the sintered aluminium
hybrid composites. Addition of 5 wt. % of SiC to aluminium matrix has resulted in increased
hardness of base material by 19 %. The higher hardness of the Al+5%SiC composite could be
attributed to the fact that SiC reinforcement is working as a barrier to the motion of dislocation
[77].
As the ZrO2 nanopowder content added in Al+5%SiC matrix sequentially in a step of 3 wt. %
further improvements in hardness have been observed. The enhanced hardness of the
composites may be due to the following reasons. (a) Uniform distribution of SiC and ZrO2 in
the composites. (b) High density of ZrO2 nanopowder. (c) Elevated hardness of ZrO2
nanoparticles.
41 | P a g e
Rockwell hardness No. 70
60
50
40
30
20
10
Pure Al Al+5%SiC Al+5%SiC+3%ZrO2 Al+5%SiC+6%ZrO2 Al+5%SiC+9%ZrO2
Figure 3.8 Influence of weight percentage of ZrO2 on hardness of Al hybrid composites
42 | P a g e
Table 3.4 Comprehensive look of previous works regarding ceramic reinforced aluminium matrix composites.
Previous Works Material used Methods of Parameters Inferences
preparations measured
Al2024 and SiC  Hardness increases with the increase in
Ma et al. (1996)  (0, 15, 20, and 30 vol.-%SiCp). Powder volume fraction of SiC.
Hardness
[78]  Mean sizes of 3.5, 10.0 and 20 metallurgy  Hardness decreases with the increase in
µm particle size.
 Hardness increases with the increase in
Al–SiC composites
Kassim et al. (1999) Powder volume fraction of SiC.
 5, 10 and 20 vol.%. Hardness
[38] metallurgy  Hardness decreases with the increase in
 10, 27 and 43 µm particles
particle size.
 Hardness increases with the increase in
Hassan et al. (2008) Al–Cu/SiC composites. Powder
Hardness volume fraction of SiC.
[41]  5 or 10 vol% SiC metallurgy
Veeresh Kumar et al Liquid Powder  Hardness increases with SiC.
Al6061 containing 2–6 wt% SiC Hardness
(2012) [43] metallurgy
Powder
Mosleh-shirazi et al. Al/SiC nanocomposits (1%, 2%  Hardness increases with nano SiC.
metallurgy Hardness
(2016) [45] and 3% (volume fraction)
Powder
Moazami-Goudarzi Al 5252 alloy (nanometric or  Nanocomposites are harder in comparison
metallurgy Hardness
et al. (2016) [46] micrometric SiC particles) to micro-composites.
Powder
Umasankar (2014) Density,  Hardness increases with increase in
AA6061-SiC composites. metallurgy
[75] Hardness compaction pressure and SiC amounts.
A356 alloy- nano SiC.
Mazahery et al.  Hardness is increased with increase in nano
 0, 1, 2, 3, 4 and 5 wt.% of nano Stir casting Hardness,
(2012) [44] SiC particles.
SiC
Kumar et al. (2016) Al−15%SiC- TiO2 (0, 4%, 8%, Powder Hardness  Hardness and density increases with the
[73] 12%, mass fraction) hybrid metallurgy increase in TiO2
composites  Al−15%SiC−12%TiO2 hybrid composites
is best in terms of hardness.
43 | P a g e
3.3.4 Sliding wear behaviour
3.3.4.1 Addition of silicon carbide and zirconium oxide

The variation of wear loss of the pure aluminium along with synthesized hybrid composites is
shown in Fig. 3.9. The wear loss decreases by the increase in SiC addition. The wear loss of
Al+5%SiC composite is 0.0075 g which is 8.5% lower than the pure aluminium. The
considerable improvement in the wear properties can be attributed to the hardness provided by
SiC particles. Similar, observations have been made by the other researchers also [79,80].
Graphical analysis also reveals that the wear properties of the hybrid composites are further
improved when ZrO2 particulate content increases.
0.01
Al
0.009 Al+5%SiC
0.008 Al+5%SiC+3%ZrO2
Wear loss (gm)
0.007 Al+5%SiC+6%ZrO2
0.006 Al+5%SiC+9%ZrO2
0.005
0.004
0.003
0.002
0.001
0
Figure 3.9 Influence of weight percentage of ZrO2 on wear loss of Al hybrid composites.
Fig. 3.9 also confirms that the hybridization of ZrO2 to Al+5%SiC composite improves the
wear resistance of the composites. Improved wear behavior of the hybrid composite may be
due to the following reasons. (a) High hardness of ZrO2 and SiC which restrict the plastic flow
during sliding wear [81], (b) the spherical shape of ZrO2 particles tends to delay crack
initiation, (c) strong interface bonding between the matrix and reinforced particle.
3.3.4.2 Influence of sliding speed

Fig. 3.10 shows the influence of sliding speed on wear loss of the synthesized composites.
From Fig. 3.10 it can be concluded that wear loss is strongly related to the sliding speed. Fig.
3.10 also shows that as the percentage of ZrO2 particle increases the wear resistance of the
44 | P a g e
hybrid composite increases. The wear loss is low at low sliding speed and vice versa. The lower
wear loss at low sliding speed can be attributed due to the surface oxidation which improves
the hardness as well as the strength at the surface [82]. But at high sliding speed the wear loss
increases which may be due to the following reasons. (a) Micro-machining effect of reinforced
particle removes the hard oxide layer causing direct metal to metal contact thus enhancing the
wear loss[83,84] and (b) The rise in temperature of the rubbing surface softens the composites,
which further lowers the bonding of reinforced particle to metal matrix [85].
0.003
Al
Al+5%SiC
0.0025 Al+5%SiC+3%ZrO2
Al+5%SiC+6%ZrO2
Al+5%SiC+9%ZrO2
0.002
Wear loss (gm)
0.0015
0.001
0.0005
0
1 1.5 2 2.5
Sliding speed (m/s)
Figure 3.10 Influence of sliding speed on wear loss of Al hybrid composites.
3.3.4.3 Influence of sliding distance

The variation of wear loss of the pure aluminium along with synthesized hybrid composites
against different sliding distance is shown in Fig.3.11. The graphs shows that wear loss of
synthesized hybrid composites along with pure aluminium increases with sliding distance.
However, at a fixed sliding distance composite having 9% ZrO2 exhibit enhanced wear
properties than other fabricated composites. This improved wear properties can be understood
because of superior hardness possessed by ZrO2 particles. As the amount of ZrO2 increase in
the composite the disintegration of particles started under sliding condition. These fragmented
particles along with oxide layer forms a film, which diminishes the contact of rubbing faces
and wear loss. During sliding condition these disintegrated particle adheres to the counter disc.
Further increase in sliding distance causes the fracturing and smearing out of the implanted
45 | P a g e
particles form the counter disc. The remaining non-disintegrated particles increases the wear
loss by abrading the counter disc [80,82–86].
0.009
Al
0.008 Al+5%SiC
0.007 Al+5% SiC +3%ZrO2

Al+5%SiC+6%ZrO2
Wear loss (gm)
0.006 Al+5%SiC+9%ZrO2
0.005
0.004
0.003
0.002
0.001
0
300 400 500 600 700 800 900
Sliding distance (m)
Figure 3.11 Influence of sliding distance on wear loss of Al hybrid composites.
3.3.4.4 Influence of applied load

The variation of wear loss of the pure aluminium along with synthesized hybrid composites
against different applied load is shown in Fig. 3.12. The graphs shows that at constant sliding
speed, wear loss of synthesized hybrid composites along with pure aluminium increases with
applied load.
0.0025
Al
Al+5%SiC
0.002 Al+5% SiC+3%ZrO2
Al+5%SiC+6%ZrO2
Wear loss (gm)
Al+5%SiC+9%ZrO2
0.0015
0.001
0.0005
0
20 25 30 35 40
Applied load (N)
Figure 3.12 Influence of load on wear loss of Al hybrid composites.
46 | P a g e
From the graph it can be concluded that at high load the wear loss is greater and vice versa.
The results are in good agreement with the previous reported data by other researcher [85,87].
Furthermore, composites reinforced with 9%ZrO2 shows higher wear resistance than other
composites. This can be attributed because ZrO2 particles is acting as a load bearing element.
During sliding condition oxidation of specimen surface cannot be avoided and these oxide
layer forms a layer on the specimen surface. In this developed oxide layer distortion, spalling
and fracture takes place during sliding condition. When the load increases all the oxide layers
are not completely removed from the rubbing surface, some amounts present between the
mating surfaces offers wear resistance due to the dilution of metallic contact of the surface.
But as the load exceeded a certain value severe wear loss is observed in all composites because
gross damage occurs at rubbing surface [88].
The addition of particulate ceramic reinforcements greatly affect the wear resistance of
aluminium matrix composites. Both incorporation of micro- and nanoparticles ceramic
particles improves the wear behaviour of aluminium composites. The contributions of several
researchers regarding the effect of particulate reinforcement on the wear behaviour of the
AMCs have been summarized below.
47 | P a g e
Methods of Parameters
Previous Works Material used Inferences
Ma et al. (1996) Al2024 and SiC Powder Wear test.  Wear resistance is best for 30 vol.% SiC
[37]  (0, 15, 20, and 30 vol.- %SiCp). metallurgy composites.
 Mean sizes of 3.5, 10.0 and 20 µm
Kassim et al. Al–SiC composites Powder Wear test.  Wear resistance of the composites increased with
(1999) [38]  5, 10 and 20 vol.%. metallurgy increasing the volume fraction of SiC.
 10, 27 and 43 µm particles  At constant volume fraction of SiC reinforcement,
the wear resistance increased with an increase in
the reinforcement size.
Hassan et al. Al–Cu/SiC composites. Powder Wear test.  Al- 10 vol %SiC showed the maximum wear
(2008) [41]  5 or 10 vol% SiC metallurgy resistant behaviour.
Veeresh Kumar Al6061 containing 2–6 wt% SiC Liquid Powder Wear test.  Al-6 wt%. SiC is best in terms of wear resistance.
et al (2012) [43] metallurgy (applied load, sliding distance)
MOSLEH- Al/SiC nanocomposites(1%, 2% and 3% Powder Wear test.  Wear resistance increases increase in nano SiC.
SHIRAZI et al. (volume fraction) metallurgy
(2016) [45] (750MPa, 500
degree C)
Moazami- Al 5252 alloy (nanometric or Powder Wear test.  Both micro and nanocomposites showed improved
Goudarzi et al. micrometric SiC particles) metallurgy wear resistance.
[46] (600 MPa, 500C  Nanocomposite showed superior wear resistance
) at high loads.
Ravidran et al. Al 2024–5 wt% SiC–x wt% graphite Powder Density,  Composites with 5 wt% graphite had the lowest
(x¼0, 5, and 10) hybrid composites metallurgy Hardness and wear loss.
(2013) [59] (885 MPa and 530 wear test.
degree C)
Ünlü (2008) [80] Al-Al2O3–SiC hybrid composites Stir casiting and Wear  Wear resistance increases with the increase in
(0, 3 and 6 wt. SiC) Powder Al2O3 and SiC
(0,3 and 6 wt. Al2O3) metallurgy
KUMAR et al. Al−15%SiC- TiO2 (0, 4%, 8%, 12%, Powder Wear test  Wear resistance increases with the increase in
(2016) [73] mass fraction) hybrid composites metallurgy TiO2 particles.
 Al−15%SiC−12%TiO2 hybrid composits is best
among all developed compostits for all sliding
distance, speed and applied load.
48 | P a g e
3.3.4.5 Analysis of worn surface using SEM
SEM analysis of the worn surfaces of pure Al along with synthesized composites are given in
Figs. 3.1-3.17. The worn surface of pure aluminium in Fig. 3.13 (a-b) shows the morphological
pattern that includes craters and deep grooves. The frictional heat developed during sliding
condition caused plastic deformation. The developed heat also softens the surface and thus
causing the particle pulled out [89]. The delamination is also noticed in aluminium matrix.
a b c
Crater
s
Deep Craters
Grooves
Oxide
Delamination
Figure 3.13 SEM images of worn surface of aluminium matrix at 30 N load, 2 m/s sliding
magnification; (c) sample at 500× magnification.
a b c
Pits Deep Grooves

Plastic flow
Figure 3.14 SEM images of worn surface of Al+5%SiC at 30 N load, 2m/s sliding speed and
900 m sliding distance: (a) sample at 100× magnification; (b) sample at 200× magnification;
(c) sample at 500× magnification.
49 | P a g e
a b c Fractured debris
Grooves and
scratches
Adhesive layer
a b Smooth surface c
representing high Grooves with
wear resistance compacted particles
Oxide
layer
a b c
Oxide layer Smooth Grooves
Smooth surface representing
improved wear resistance
50 | P a g e
Fig. 3.14 is giving the details of worn surface of Al+5%SiC composites. The SEM of the
Al+5%SiC composite is having pits and grooves. The surface is also seems to be rough which
is due to the abrading nature of silicon carbide particles [35,90].
Fig. 3.15 shows the worn surface of Al+5%SiC+3%ZrO2 hybrid composites. Fig. 3.15 is
clearly showing numerous grooves and scratches parallel to the sliding direction, indicating
dominance of abrasion wear mechanism. On few locations of micrographs fractured particles
of reinforcement and matrix material is found, which is causing the deterioration in wear
resistance of the composites. The shallower scratches were also identified in Fig. 3.15 which
is supporting abrasive wear mechanism [91].
Fig. 3.16 depicts the worn surface of aluminium hybrid composites having 6% ZrO2 particle
content. Fig. 3.16(a) shows fretting wear which is confirmed by the presence of loose oxide
layer. The presence of loose oxide layer can be attributed due to the developed cyclic stress
under sliding environment. Further, it can be observed from Fig. 3.16 that scratches appear at
the worn surface of the composite. The scratches are minor which represents superior
hardness of composite imparted by the nano ZrO2 particles. It can be therefore inferred that
the presence of nano ZrO2 particles enhances the wear properties of synthesized hybrid
composites.
The wear pattern of Al+5%SiC+9%ZrO2 hybrid composite is presented in Fig. 3.17. The
hybrid composite is showing superior wear properties which can be confirmed by the presence
of restriction of grooves along the worn surface. The high content of ZrO2 and their uniform
distribution are the main cause of restriction of grooves. The hardness imparted by ZrO2
particle can also be considered as a reason of improved wear resistance properties. The
adhesive compacted particles and oxide layer is present in SEM morphgraphs which is
restricting plastic deformation, thereby lowering the wear loss [54]. Finally, the close
investigation of Fig. 3.17 is showing the evidence of adhesive wear mechanism.
3.4 Conclusions
In the present work, hybrid Al+SiC+ZrO2 composites containing 5 wt. % SiC microparticles
together with different weight fractions of zirconium oxide nanoparticle (0-9%, weight
fraction) were prepared by powder metallurgy. The morphological, mechanical and
51 | P a g e
tribological properties of the synthesized hybrid composites were also investigated. The
detailed findings can be summarized as follows:
i. As the amount of ZrO2 particle increases, the hardness value of the hybrid composites
increases. The hardness shows remarkable improvement of 43% with respect to pure
aluminium.
ii. The sliding wear behavior of the synthesized composites reveals that Al+SiC+ZrO2 hybrid
composites shows enhanced wear properties among all fabricated composites. However,
the wear resistance showed improvement with the increase in the amount of ZrO2. Hence,
Al+5%SiC+9%ZrO2 will be preferred option for high wear resistance applications.
iii. The SEM micrographs, XRD and elemental mapping confirms the validation of
synthesized composites.
iv. The elemental mapping of synthesized composite revealed a reasonably homogeneous
distribution of reinforced particle in the matrix.
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4. Analysis of Tribological Behaviour of Zirconia Reinforced Al-SiC
Hybrid Composites Using Statistical and Artificial Neural Network
Technique
4.1 Introduction
Aluminium matrix composites (AMCs) are favorable material due to its potential application
in automobiles, structural and aerospace industries [55,61,63,77,79,92] The aluminium matrix
composites attracted the recent researcher’s attention because of its catching properties such
as high strength to weight ratio, low density, high stiffness and wear resistance along with
relatively small fabrication cost [93]. The end mechanical behaviour of the metal matrix
composite depends upon fabrication technique, orientation and distribution of the reinforced
particles. Therefore, many researcher attempted various methods like mechanical alloying
[94], casting [95] and powder metallurgy [96] to accomplish desired mechanical properties.
Amongst different synthesis technique, powder metallurgy found more attention for AMCs
synthesis due to achievement of fair homogeneity of reinforcement in matrix phase along with
capability of producing near net shaped products. Therefore, costly machining operation is
minimized and making the manufacturing process economical [54,97].
Presently, ZrO2 [70,98], SiC [43,99,100], Al2O3 [66,101], B4C[67], Si3N4 [68], AIN [68] and
TiC [69,102] are extensively used for reinforcing the aluminium metal. Amongst numerous
ceramic reinforcements SiC, particle is most widely used because its density is very close to
aluminium matrix. Additionally, SiC possess higher stability, wear resistance and rigidity both
at room and elevated temperature [92,98,103]. This enhancement in properties are achieved at
the cost of ductility and fracture toughness. Further, addition of hard ceramic reinforcement
enhances the hardness which makes the machining difficult and uneconomical [73].
Furthermore, aluminium reinforced with micro and nano particles has got better mechanical
and tribological properties over single reinforcement because of following reasons:
(a) Nanoparticles increases the utility of the matrix due to Orowan strengthening
mechanism.
(b) Nanoparticles retains the ductility of the composites and improves fracture toughness.
53 | P a g e
(c) Micro particles withstand frictional loading, which affects the composites by increasing
its hardness and wear resistance.
(d) Nano particle creates obstruction for the movement of dislocation and promotes fine
grain structure.
Further, addition of oxide phase of metal also reduces brittleness and increases fracture
toughness of aluminium matrix composites [74,103]. They are economical, widely available
and eco-friendly therefore could be used as a reinforcing phase in aluminium matrix [104,105].
Zirconia (ZrO2) nano particle is portrayed to be an outstanding reinforcement in aluminium
matrix because zirconia exhibits outstanding mechanical, wear and thermal behaviour.
Therefore, combination of micro-SiC and nano-metal oxide (ZrO2) will be attractive option for
aluminium matrix to enhance tribological properties.
In recent years, researchers widely used artificial neural network (ANN) technique for
modelling the mechanical and tribological properties of composites. It is very promising tool
to find out behaviour of experimental trend much faster in comparison to other approaches
with the additional ability to learn from small data. The ANN approach is also capable of
establishing and predicting the relation between complex input and output data patterns [106].
Further, tribological behaviour of aluminium matrix composite is governed by many factors
like reinforcement concentration, sliding distance and applied load. Therefore, visualization of
each factor and their interaction is very important for complete study of wear behaviour. This
difficulty can be easily solved by using a statistical tool analysis of variance (ANOVA). This
approach is simple, efficient and widely accepted worldwide to get quantitative measurement
of each control variables on the output data [107].
From literature it has been noticed that no detail findings are available on tribological
behaviour of zirconia (ZrO2) reinforced Al-5%SiC hybrid nano-composites using ANN and
statistical approach. Therefore, in the current research work tribological behaviour of Al-SiC-
ZrO2 hybrid composites synthesized by powder metallurgy were explored. The effect of
zirconia concentration, sliding distance and applied load on wear behaviour of hybrid
composites were investigated using full factorial design of experiments. The percentage
contribution of different process parameters and their interaction were analyzed using analysis
54 | P a g e
of variance (ANOVA). Further, ANN prediction model is developed to find the role of
different control factors on wear behaviour of hybrid composites.
4.2 Experimentation
4.2.1 Fabrication of composites
The detail of reinforcing particles used in experimental study is shown in Table 4.1. For study
following combination of hybrid composites are synthesized through powder metallurgy
technique.
i. Al-5%SiC-0%ZrO2.
ii. Al-5%SiC-3% ZrO2.
iii. Al-5%SiC-6% ZrO2.
iv. Al-5%SiC-9% ZrO2.
Table 4.1 Information of reinforced particles.
Reinforced particles Average particle size Density, g/𝒄𝒎𝟑

SiC 37 µm 3.21
ZrO2 30-50 nm 5.89
Firstly, a digital weighing machine (Precisa, Swiss Made, ES 225SM-DR) with a least count
of 0.0001 gm. were used for measuring the weighed of used powders. A predetermined amount
of particles were mixed thoroughly using centrifugal type ball mill (FRITSCH, Germany).
While mixing, 8 mm diameter stainless steel balls were adopted with 10 BPR (Ball to powder
ratio) for the minimization of clustering of composite powders. The rotation speed and milling
time were fixed at 125 rpm and 20 min. respectively. Further, green pallets of dimensions
8mm and height 13 mm were fabricated at 585 MPa using uniaxial hydraulic pallet press (Type
KE, Sr. No. 1327, Kimaya Engineers, India) for sintering operation. After every compaction
process the die wall was cleaned and lubricated with zinc stearate manually for proper
functioning of the die. The green specimens were sintered in tubular electric furnace attached
with controlled environment unit. The specimens were sintered at 450-470 0C for 60 min. under
the continuous flow of argon gas (flow rate=1litre/min.) for preventing the samples from
oxidation [75]. The specimens were cool down to the ambient temperature in the furnace itself.
55 | P a g e
4.2.2 Wear analysis
A pin-on-disc equipment (Ducom, Model No: TR-201 CL, Bangalore, India) were adopted to
study tribological behaviour of synthesized hybrid composites according to ASTM G99-95a
(reapproved) standards. The wear variables and their respective levels are provided in Table
4.2.
Table 4.2 Test variables and process parameters.

Test variables Explanation
Samples dimension Diameter 8mm and height 13mm
Sliding distance 300,600,900 (m)
Applied load 20, 40 (N)
Counter disc material EN31 steel, 65 HRC
Temperature and Relative humidity 30 0C and 60-65 %.
The specimens and counter disc surface were cleaned with acetone to eliminate adhered wear
particles. The wear loss is determined by measuring weighed of specimens after every test runs
with electronic weighing balance.
4.3 Results and discussion
4.3.1 Experimental design and ANOVA analysis
The experiments were performed according to the general full factorial design. The various
chosen control factors and their respective levels is shown in Table 4.3. The general full
factorial design having 24 rows and 3 columns is shown in Table 4.4. The results of all 24 set
of experiments were subjected to analysis of variance (ANOVA). All the result tables and plots
are calculated with the help of Minitab-16 software [108].
Table 4.3 Process parameters with their different levels.
Process parameters Units Level 1 Level 2 Level 3 Level 4

Zirconia reinforcements (A) wt. % 0 3 6 9
Sliding distance (B) m 300 600 900
Applied Load (C) N 20 40
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To find influence of each process parameters on tribological behaviour of fabricated
composites ANOVA analysis have been performed and shown in Table 4.5. The sliding
distance is showing highest effect on wear loss and contributing 79.45%. The zirconia
concentration (10.35%) and applied load (6.7%) revealed a lesser amount of contribution to
the wear loss. The interaction between zirconia concentration and sliding distance is 3% while
the other interactions like zirconia concentration *Applied load (0.1%) and sliding
distance*applied load (0.1%) on wear is marginal. The error contribution is 0.24 % only.
Table 4.4 General full factorial design

Concentration Sliding distance Applied load
S.No. (wt. %) (m) (N) Wear loss (mg)
(A) (B) (C)
1 0 300 20 0.9
2 0 300 40 1.9
3 0 600 20 3.6
4 0 600 40 4.9
5 0 900 20 6.8
6 0 900 40 8.5
7 3 300 20 0.4
8 3 300 40 1.7
9 3 600 20 3.5
10 3 600 40 4.2
11 3 900 20 5.2
12 3 900 40 7.0
13 6 300 20 0.2
14 6 300 40 1.6
15 6 600 20 2.6
16 6 600 40 3.6
17 6 900 20 5.2
18 6 900 40 6.5
19 9 300 20 0.1
20 9 300 40 0.9
21 9 600 20 2.1
22 9 600 40 3.0
23 9 900 20 3.7
24 9 900 40 4.6
Table 4.5 Results for ANOVA for wear loss (mg)
SOURCE D.F Seq Adj.SS Adj.MS Fvalue Pvalue Percentage

SS contribution
A 3 12.86 12.89 4.28 97.71 0.000 10.35
B 2 99.00 99.0 49.50 1127.89 0.000 79.45
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C 1 8.28 8.28 8.28 188.74 0.000 6.7
A×B 6 3.75 3.75 0.62 14.27 0.003 3.0
A×C 3 0.1979 0.1979 0.0660 1.50 0.306 0.1
B×C 2 0.21 0.21 0.1050 2.39 0.172 0.1
Error 6 0.26 0.26 0.0439 0.24
Total 23 124.57
S = 0.000209497 R-Sq = 99.79% R-Sq(adj) = 99.19%
4.3.2 Effect of different process parameters on wear loss
The effect of each process parameters (zirconia concentration, sliding distance and applied
load) on wear behaviour can be analyzed with the help of main effect plot, interaction plot and
scatter plot. These plot also helps to identify optimum value of process parameter to reduce the
wear loss. Fig. 4.1 is main effect plot and is showing the effect of different process parameters
on the wear loss. According to the theory if a line of any process parameter in the main effect
plot is low variation to the mean value, then it concludes that the given plotted process
parameter has no significant effect. On the other hand, plot of any process parameter is having
the highest slope i.e. most significant effect. So, it is evident form the main effect plot that the
sliding distance is the most Influential parameter followed by zirconia concentration and
applied load. The main effect plot also confirms that as the concentration of zirconia increases
in aluminium composites its wear resistance increases. This enhancement in the wear
resistance can be attributed to the following reasons: (a) high hardness imparted by zirconia
particle which is restricting plastic flow during sliding condition, and (b) strong interfacial
bond between particle and matrix phase. The interaction plot (Fig. 4.2) shows that optimum
values for best wear resistance occurred when zirconia was at level 3, sliding distance was at
level 1 and applied load at level 1. Similarly, scatter plot shown in Fig. 4.3 confirms that the
best combination for lowest wear loss is achieved at 9 wt. % zirconia concentration for lowest
sliding distance (300m) and applied loads (20N).
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Main Effects Plot for Wear loss
Data Means
Zirconia Concentration S liding Distance

6
Mean 2
0 3 6 9 300 600 900

Applied load
6
20 40
Figure 4.1 Main effect plot for process parameters on wear loss of Al-SiC-ZrO2 hybrid
composites.
Interaction Plot for Wear loss

Data Means
300 600 900
8
Zirconia
Concentration
0
4
Zir conia C oncentr ation 3
6
9
0 8
Sliding
Distance
300
4
Sliding Distance 600
900
8 0
Applied
load
20
4
A pplied load 40
0
0 3 6 9 20 40
Figure 4.2 Interactions of various process parameters on wear loss.
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Scatterplot of Wear loss vs Zirconia Concentration
9 Sliding Applied
Distance load
8 300 20
300 40
7 600 20
600 40
6 900 20
900 40
Wear loss
0
0 1 2 3 4 5 6 7 8 9
Zirconia Concentration
Figure 4.3 Scatter plot for wear loss
Probability Plot of Residuals

Normal
99
95
90
80
70
Percent
60
50
40
30
20
10
1
-0.3 -0.2 -0.1 0.0 0.1 0.2 0.3
Residuals
Figure 4.4 Normal probability plot for residuals of fabricated composites.
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4.3.3 Linear regression model
The empirical relationship between wear loss and various control factors (viz. zirconia
concentration, sliding distance and applied load) is calculated using multiple linear regressions
with the help of Minitab 16 software.
Wear loss (g) = -3.50417 + 0.047*Zirconia Concentration + 0.010*Sliding Distance +

0.058*Applied load – 0.00043*Zirconia Concentration*Sliding Distance [4.1]
When the values of different process parameters are substituted in Eqn. 4.1, wear loss of hybrid
composites can be easily calculated within the range of process parameters investigated. The
adequacy of the model represented by Eqn. 4.1 is verified by normal probability plot of
residuals as shown in Fig. 4.4. It is clear from normal probability plot that points are very close
to line which also validates the adequacy of model developed.
4.3.4 Artificial neural network modelling (ANN)
ANN mainly consists of three main layers: input layer, hidden layer and output layer as shown
in Fig. 4.5. The input layer consists of input nodes which receives the data from the user and
transfer it to the output layer through hidden layer. Depending upon the complexity of available
data the number of hidden layer can be varied [106].
Hidden layer
Input layer
Output layer
Zirconia Conc.
Wear loss
Applied Load
Sliding distance
Figure 4.5 Neural network with 4-10-1 topology.
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In the current developed model three layer architecture is chosen: one input layer having
zirconia concentration, sliding speed, sliding distance and applied load as the input nodes,
hidden layer with ten hidden nodes and the output layer with only one output node namely
wear loss. A feed forward back propagation ANN model was used to train the network. The
training and testing of the data was performed using MATLAB (2016) software package. Due
to reliability and processing time Levenberg-Marquardt (LM) algorithm was used in this
modelling research work [109]. According to the previous literatures again in modelling tansig
transfer function and purelin transfer were used in the hidden and output nodes [110]. From
the total experiment run as given in Table 4.4, 70% data are used for training the model and
rest of the data is equally divided for testing and validating the developed model. The inputs
given to ANN model were in the range of [0-1], so that all process variables have equal
importance to the response. The normalization of the data have been performed using equation
give below.
Input value−Minimum value

Normalized value = Maximum value−minimum value………………………………………[4.2]
The training of the ANN model have been performed with 1000 iterations and 1000 epochs.
Mean square error (MSE) have been used to evaluate the performance of the proposed ANN
prediction technique. Further, number of nodes in the hidden layer have been varied and mean
absolute error (MAEs) of the corresponding models were calculated with the formula as shown
in Eqn. 4.3, to find the best model.
|ai −bi |
MAE=∑ni=1 ………………………………………………………………………… [4.3]
n
Where, ai= Predicted ANN output, bi= Corresponding experimental readings and n is total no
samples selected. The MAEs comes out to be 0.0041 for hidden layer with ten number of
nodes, which is lowest amongst the different number of nodes tested for hidden layer.
Therefore, it has been decided that ANN model with feed forward back propagation with 4-
10-1 topology would be the best in terms of predictability. For validation and accuracy of the
developed ANN model, the remaining four readings (Readings 3, 9, 16 and 21) were fed to the
model which was not used for training purpose are simulated and shown in Fig. 4.6. The
experimental results and ANN predicted results as shown in plot are close to each other
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showing low error difference. So, it be concluded that the selected model can be effectively
used to predict the wear loss of developed hybrid composites.
4
Experimental values ANN pridiction
3.5
3
Wear loss (mg)
2.5
1.5
0.5
0
3 9 16 21
Experimental trials
Figure 4.6 Experimental and predicted results of wear loss form ANN developed model.
4.3.5 Verification of sliding wear behaviour with ANN
The developed model is further used to analyze the influence of each process parameters on
the wear properties of the fabricated composites. For finding out the influence of ZrO2
concentrations on the wear loss, the ANN is simulated with the data having variation in zirconia
concentration from 0 to 9%, keeping the remaining process parameters like sliding distance
and applied load as constant. Similarly, influence of other process parameters are investigated
and shown in Fig. 4.7 (a-c). The trends are in accordance with that obtained by general full
factorial design.
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6
5
(a) 4.5
5 (b)
4
Wear loss (mg)

Wear loss (mg)
4 3.5
3
3 2.5
2
2 1.5
1
1
0.5
0 0
0 3 6 9 300 600 900
Zirconia concentration (wt. %) Sliding distance (m)
3.5
(c)
3
2.5
Wear loss (mg)
1.5
0.5
0
20 40
Applied load (N)
Figure 4.7 ANN model results of various process parameters (a) Effect of ZrO2
concentration. (b) Effect of sliding distance (c) Effect of applied load.
4.4 Conclusions
The following major conclusions can be drawn by using statistical and ANN approach on
zirconia reinforced Al-5%SiC hybrid composites fabricated by powder metallurgy technique.
i. General full factorial analysis suggested that the most significant process parameter
affecting the wear loss is sliding distance followed by zirconia reinforcement and
applied load.
ii. ANOVA analysis provided the exact amount of percentage contribution of each
factor on wear loss: Sliding distance (79.47%), ZrO2 reinforcement (10.35%) and
applied load (6.7%) in the composites. The sliding distance and applied load
interaction is only 3%, within the selected range of investigation.
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iii. The ANN model with 4-10-1 topology showed satisfactory prediction capability
between experimental and predicted values. Hence, this network can be used to
study the factors influencing the wear loss.
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5. Morphological and Wear Behaviour of New Al-SiCmicro-SiCnano Hybrid
Nanocomposites Fabricated Through Powder Metallurgy
5.1 Introduction
Recently, the material scientists are heavily indulged in developing new and advanced material
matrix hybrid nanocomposites all around the globe. Due to exposure of harsh engineering
environment a single metal/alloys are failing to achieve the requirements. This initiates the
need of fabrication of metal matrix hybrid nanocomposites with certain specific property to
meet future engineering challenges.
In the last few decades, aluminium metal composites have found potential application in
aerospace, automobiles and structural sectors because of its low density and high strength.
Further, reduction in weight of composites by the use of aluminium matrix produces great
economic advantage. However, use of pure aluminium in many engineering and tribological
application is difficult because of its low strength and wear properties. In past, a vast
experimental studies have been performed on addition of hard ceramic particle to aluminium
matrix to enhance its strength, hardness and wear resistance under ambient and elevated
temperature applications [55,61,63,77,79,92].
The target properties of composites depends upon combined effect of reinforced particle and
fabrication technique. As far as fabrication technique is concern several techniques are
available such as spray deposition, squeeze casting, compo casting, stir casting and powder
metallurgy [111]. The conventional stir casting process involves some major drawbacks like
inadequate wettability between reinforcement and matrix, inhomogeneous distribution and
formation of brittle intermetallic compound at the reinforcement and matrix interface. In order
to overcome these serious drawbacks, powder metallurgy can be used because of following
advantages: (a) low processing temperature (b) homogeneous distribution of reinforcement and
matrix particle (c) fabrication of near net shaped product [92].
At present, aluminium matrix hybrid composites reinforced with micro and nanoparticles have
gained increased application because of enhanced mechanical and tribological properties [5].
The reason of enhancement in properties could be attributed due to the following reasons:
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(e) Incorporation of uniformly dispersed nanoparticles improves the performance of
matrix due to Orowan strengthening mechanism.
(f) Better microstructure and mechanical properties can be achieved by changing particle
size from micro to nano level [6].
(g) Nano particle also retains the ductility of composites and improves fracture toughness
[7].
(h) Micro particle works as a skeleton for aluminium matrix and enhances the hardness
and wear properties [8,9].
However, aluminium reinforced with single ceramic micro particles deteriorates the ductility
of composite because their tendency to crack during loading condition, when their
concentration is high in the matrix. Further, incorporating nanoparticles enhances the
mechanical properties of composites by obstructing dislocation movement and promoting fine
grain structure. Therefore, overall enhancement in the performance of composites can be
achieved by reducing the concentration of micro particles and increasing the amount of
nanoparticles to get synergistic improvement in mechanical and tribological properties [112].
Presently, SiC [5,6,77,79,92,111], B4C [7,61], Al2O3 [55] and TiC [69] are widely used as a
reinforcement in aluminium matrix composite because of its enhanced mechanical and
tribological properties. Among various available reinforcing particles, SiC particles are
preferred because its density is very close to aluminium matrix. Additionally, SiC possess
higher stability and rigidity both at room and elevated temperature along with high hardness
and increased wear resistance. The mechanical and wear behaviour of aluminium matrix
reinforced with two ceramic (SiC+TiB2, SiC+Al2O3 etc.) particles were studied in literature.
However, study on sliding wear behaviour of AMHCs (Aluminium matrix hybrid composites)
reinforced with micro and nano SiC particles are not yet explored.
Therefore, the present investigation aimed to fabricate micro and nano silicon carbide
dispersion strengthened aluminium hybrid composites by powder metallurgy technique. The
XRD, EDS, SEM and elemental mapping of samples have been performed. The sliding wear
behaviour of nanocomposites have been investigated to find out the influence of
67 | P a g e
reinforcement, sliding distance and applied load using pin-on-disc wear tester. Further, SEM
analysis is performed to find out the wear mechanism.
5.2 Experimentation
5.2.1 Fabrication of composites
The detail of reinforcing particles used in experimental study is given in Table 5.1. For the
analysis, following combination of samples were synthesized through powder metallurgy
technique.
i. Al (Pure).
ii. Al+10% SiCµm.
iii. Al+10% SiCµm+1%SiCnm.
iv. Al+10% SiCµm+3%SiCnm.
v. Al+10% SiCµm+5%SiCnm.
vi. Al+10% SiCµm+7%SiCnm.
Table 5.1 Information of experimental particles.
Experimental particles Average particle size Density, g.𝒄𝒎−𝟑

Al 10 µm 2.71
SiC 37 µm 3.21
SiC 50 nm 3.21
Firstly, a digital weighing machine (Precisa, Swiss Made, ES 225SM-DR) with a least count
of 0.0001 g. were used for measuring the weighed of experimental particles. A predetermined
amount of particles were mixed thoroughly using centrifugal type ball mill (FRITSCH,
Germany). While mixing, 8 mm diameter SS (Stainless steel) balls were adopted with 10 BPR
(Ball to powder ratio) for the minimization of clustering of composite powders. The rotational
speed and milling time were fixed at 125 rpm and 20 min. respectively. Further, green pallets
of dimensions 8mm and height 13 mm were fabricated at 585 MPa using uniaxial hydraulic
pallet press (Type KE, Sr. No. 1327, Kimaya Engineers, India) for sintering operation. After
every compaction process the die wall was cleaned and lubricated with zinc stearate manually
for the proper functioning of die. The green specimens were sintered in tubular electric furnace
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attached with controlled environment unit. The specimens were sintered at 450-470 0C for 60
min. under the continuous flow of argon gas (flow rate=1litre/min.) to prevent the samples
from oxidation [75]. The specimens were cool down to the ambient temperature in the furnace
itself. A Rockwell hardness tester (TRB-250 DM, Digital) with a steel ball of diameter of 1/8”
and a load of 60 kgf (Scale H) were utilized to evaluate the hardness of sintered specimens.
Three indentations were taken at the ambient temperature (30 0C) to find out the mean hardness
of specimens.
5.2.2 X-ray diffraction
The XRD of sintered specimens were conducted under the following conditions whose
description is given in Table 5.2.
Table 5.2 XRD experimental description.
Equipment conditions Specifications/Description

2θ range 20°–700
Cu Kα radiation (λ=1.5406 0A)
Scanning rate 0.02 steps/second
Step size 0.01°
X-ray diffractometer (D8 ADVANCE) Bruker AXS Inc, Madison, WI, USA
X-ray source 40mA and 40kV
5.2.3 Dry sliding wear test
A pin-on-disc equipment (Ducom, Model No: TR-201 CL, Bangalore, India) were adopted to
study tribological behaviour of synthesized hybrid composites according to ASTM G99-95a
(reapproved) standards. The wear variables and their respective levels are provided in Table
5.3.
Table 5.3 Test variables and process parameters.

Pin dimension Diameter 8mm and height 13mm
Sliding distance 300, 600 900 and 1200 (m)
Applied load 20, 30 and 40 (N)
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Counter disc material EN31 grade steel, 65 HRC
The specimens and counter disc surface were cleaned with acetone to eliminate the adhered
wear particles. The wear loss is calculated by measuring the weight of samples after every test
runs with electronic weighing unit with 0.1 mg least count.
5.3.1 Characterization of composites
Fig. 5.1 displays the XRD plot of manufactured hybrid composites. The given XRD gram
confirms the presence of reinforcement in the fabricated composites. The peak of aluminium
is highest amongst all identified elements present in the samples. The evidence of SiC peaks
are also found in Fig.5.1.
Figure 5.1 XRD pattern Al+10%SiCµm, Al+10%SiCµm+1%SiCnm, Al+10%SiCµm+3%SiCnm,

Al+10%SiCµm+5%SiCnm, Al+10%SiCµm+7%SiCnm.
Hence, it can be concluded that synthesized composites have been reinforced with SiC. The
energy dispersive spectroscopy (EDS) study of the fabricated composite is given in Fig. 5.2.
From EDS analysis the peaks of Al, Si, C, Fe and O are observed as shown in Fig. 5.2. Further,
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Table 5.4 displays elements present in Al+10%SiCµm+5%SiCnm composites with their weight
and atomic percentages. Therefore, presence of Al and SiC particles are again validated in
fabricated composites. Fig. 5.3 shows the elemental maps of Al+10%SiCµm+5%SiCnm hybrid
composite. From the elemental maps of the composites it is obvious that Al, Si, C and O
elements are present. The elemental maps also confirms the uniform distribution of ceramic
particles in aluminium matrix.
Figure 5.2 EDS spectrum of Al+10% SiCµm+5%SiCnm nanocomposites.
Table 5.4 Details of elements present in Al+10%SiCµm+5%SiCnm nanocomposites.

O 22.12 42.72
Al 41.86 27.98
C 28.45 42.72
Si 6.01 3.86
Fe 1.55 0.50
Total 100 100
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Al
Si C O
Figure 5.3 Elemental maps of Al+10%SiCµm+5%SiCnm hybrid composites.
5.3.2 Relative density
Fig. 5.4 shows the relative density of aluminium, aluminium composites and aluminium hybrid
nano composites. Relative density is defined as the ratio of experimental density to theoretical
density. Theoretical density is calculated using rule of mixture while experimental density is
calculated by Archimedes principal. The figure shows that as the SiC increases to 10 wt. %,
the relative density decreases. The underlying reason of this decline is that hard SiC particles
do not flatten by plastic deformation during compaction and therefore creates the inter-particle
voids [92]. Additionally, during sintering the SiC particles are very dense with random
distribution due to its high melting point. This dense network formed by micro SiC particles
prevents the specimen to be dense [6]. Further, addition of nano-SiC in aluminium composites
a slight improvement in relative density is observed upto 3 wt. %. This improvement can be
attributed due to the fact that nano reinforcement particles size is much smaller than matrix
and micro SiC particles, hence interfacial micro voids have been occupied by nanoparticles
[76]. However, in higher concentration of nanoparticles composites relative density decreases
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more sharply. This reduction in the relative density could be due to the following reasons: (a)
clustering and agglomeration of nanoparticles at high concentration (b) high hardness of nano-
SiC particles hinders the compaction process [76].
100
98
96
Relative density (%)
94
92
90
88
86
84
82
80
Pure Al Al+10%SiC
Al+10%SiC+1%SiC Al+10%SiC+3%SiC
Al+10%SiC+5%SiC Al+10%SiC+7%SiC
Figure 5.4 Variation of relative density of composites with SiC concentration.
The measurement of hardness of all fabricated samples were performed on digital Rockwell
hardness tester. To achieve the accuracy in the experimental readings, three indentations were
taken on sample and their average value have been plotted in Fig. 5.5. It is obvious from figure
that as amount of nano SiC increases hardness of composites increases. This result can be
understood by rule of mixture formula.
Hc=HmVm+HrVr………………………………………………………………………… [5.1]
Where, Hc= Hardness of composite
Hm=Hardness of matrix.
Hr= Hardness of reinforcement.
Vm= volume fraction of matrix.
Vr=volume fraction of reinforcements.
Further, from experimental work it has been found that hardness of pure aluminium is 28.86
but on the addition of 10 wt. % SiC in matrix hardness of composite reaches to 47 which is
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approximately 62% higher in comparison to base aluminium matrix. This remarkable
enhancement in the hardness could be attributed due to the following reasons: (a) high hardness
and density of SiC particle (b) uniform distribution of micro and nano SiC in aluminium matrix
(c) high amount of SiC (ceramic) causes more dislocation which enhances hardness [6] (d)
Hall-patch and Orowan strength mechanisms as well as good interfacial bond between the
nanoparticles and aluminium matrix [7].
Further, addition of nano silicon carbide from 5 wt. % to 7 wt. % to aluminium matrix
composites reduces the hardness from 65 to 59. The hardness is reduced by approximately
10%. This reduction in the hardness could by attributed due to sudden decline in relative
density caused by agglomeration and clustering of nanoparticles [113].
70
Pure Al
Al+10%SiC
60 Al+10%SiC+1%SiC
Al+10%SiC+3%SiC
Al+10%SiC+5%SiC
Rockwell Hardness No.
Al+10%SiC+7%SiC
50
40
30
20
10
0
Figure 5.5 Variation of hardness of composites with SiC concentration.
5.3.4 Dry sliding wear behaviour
5.3.4.1 Influence of silicon carbide addition

Fig. 5.6 shows the influence of micro and nano SiC addition on the wear behavior of aluminium
composites. It is clearly evident from the graph, wear loss reduces sharply as the amount of
SiC reinforcement increases. The wear loss of Al+10%SiCµm is 0.0075 g. which is 53% lower
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in comparison to pure aluminium. This significant improvement in wear resistance could be
due to the high hardness imparted by SiC micro particle to soft aluminium matrix. This results
are in line with the previous researcher findings [103]. Further hybridizations of Al+10%SiC
micro composite with nano SiC upto 5 wt. % enhances the wear resistance. This considerable
amount of improvement can be due to the following reasons.
0.018
Pure Al
0.016 Al+10%SiC
Al+10%SiC+1%SiC
0.014
Al+10%SiC+3%SiC
0.012 Al+10%SiC+5%SiC
Wear loss (gm)
Al+10%SiC+7%SiC
0.01
0.008
0.006
0.004
0.002
Figure 5.6 Variation of wear loss with varying concentration of SiC particles.
(a) Nano reinforcement in composite increases the hardness that leads to reduction in wear
loss.
(b) High hardness of SiC nanoparticles hinders the plastic flow during sliding condition
[114].
(c) High concentration of SiC increases the ratio of area of contact of hard surface to soft
aluminium matrix. Hence SiC particle supports more load during sliding environment.
(d) Better interfacial bonding between matrix and reinforcement increases the shear strain
required for plastic flow, which further enhances the wear resistance of composites
[81].
The graph shows that as the concentration of nano SiC particles increases from 5 wt. % to 7
wt. % the loss of composite due to wear increases. The increase in wear loss may have been
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caused by the following reasons: (a) high concentration of nanoparticles leads to the
heterogeneous distribution of particles in aluminium matrix (b) clustering and agglomeration
of nanoparticles at high concentration cannot be avoided this leads to the formation of porosity
in composites and porosity is considered to be as zero mechanical strength (c) high amount of
ceramic reinforcement deteriorates the particle bonding during sintering resulting in enhanced
material loss due to severe delamination [92].
5.3.4.2 Influence of sliding distance

The influence of sliding distance on wear loss of all fabricated composites and pure aluminium
are shown in Fig.5.7. It is obvious from the plot as sliding distance is increasing the wear loss
of all fabricated composites and aluminium matrix is also increasing. This wear patterns are in
well accordance with the general trend of wear loss as suggested by Archard wear equation.
Further, composite reinforced with 5 wt. % nano SiC concentration is offering best wear
resistance among all fabricated composites. This result is validating the general rule, high
hardness material will show superior wear and abrasive resistance. Additionally, during sliding
environment the SiC particle gets fragmented due to high concentration in aluminium matrix
and hard SiC from composite wear the counterface leading to the formation of iron oxide.
These fragmented SiC powder, iron oxide and aluminium oxide from pin form a stable
mechanically mixed layer (MML). The MML is having superior hardness in comparison to pin
and counterface and acts as protecting layer between mating surface. Thus, the wear loss of
Al+10%SiCµm+5%SiCnm composite is less compared with other composite materials tested.
However, it is evident form the Fig. 5.7 that the wear loss of 7 wt. % nano SiC reinforced
aluminium matrix composites increases. The presence of micro porosity and low hardness is
the major reason for decreased wear resistance.
Further, increment in sliding distance increases the wear loss which can be attributed due to
the following reasons: (a) thermal softening phenomena occurs at large sliding distance (b) rise
in temperature at rubbing surface makes protecting oxide layer unstable [115].
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0.018
Pure Al
0.016 Al+10%SiC
Al+10%SiC+1%SiC
0.014 Al+10%SiC+3%SiC
Al+10%SiC+5%SiC
0.012
Wear loss (gm)
Al+10%SiC+7%SiC
0.01
0.008
0.006
0.004
0.002
0
200 400 600 800 1000 1200 1400
Figure 5.7 Variation of wear loss with varying sliding distance for all fabricated composites.
5.3.4.3 Influence of applied load

The influence of applied load on all the fabricated composites and pure aluminium are shown
in Fig. 5.8. From the plot it is obvious that wear loss is low at low loads and vice versa. Similar
findings have been reported by the previous researchers [85,87]. The wear loss of the
composites decreases as the amount of nano-SiC increases from 1 to 5 wt. % for any fixed load
which confirms the load bearing capacity of SiC particles. Further, increment of nanoparticles
reduces the wear resistance due to presence of micro porosity and deterioration of particle
bonding during sintering operation. However, as the load increases wear loss increases for all
fabricated samples. This rise in wear loss could be attributed due to the following reasons: (a)
increase in load causes more delamination [116] (b) high load develops more frictional heat
which lowers down the bond strength between reinforcement and matrix (c) increased
temperature also softens the mating surface and enhances the probability of penetration of
asperities.
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0.012
Pure Al
Al+10%SiC
0.01 Al+10%SiC+1%SiC
Al+10%SiC+3%SiC
Al+10%SiC+5%SiC
0.008 Al+10%SiC+7%SiC
Wear loss (gm)
0.006
0.004
0.002
0
15 20 25 30 35 40 45
Applied load (N)
Figure 5.8 Variation of wear loss with varying applied load for all fabricated composites.
5.3.4.4 Wear mechanism study with SEM

The worn surface of all fabricated composites and pure aluminium have been analyzed using
scanning electron microscopy as shown in Fig. 5.9-5.10. It is observed from the worn surface
that composite reinforced with nanoparticles exhibit different wear pattern when compared
with pure aluminium. This shows the change in wear mechanism. The enhanced wear
resistance of composites are supported by worn morphology of mating surface. The worn
surface of aluminium displayed presence of pits, grooves and craters as shown in Fig. 5.9 (a-
b). During sliding environment heat is generated due to friction which causes the extensive
plastic deformation on the pure aluminium surface leading to high wear loss when compared
with the developed aluminium composites and aluminium hybrid nanocomposites. The mating
surface also gets softened due to rise in temperature and hence rise in wear loss is observed on
contact surface [89]. The worn surface pattern of aluminium is confirming the evidence of
extensive delamination.
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(a) (b)
Pits and grooves
Delamination
Figure 5.9 SEM of worn surface of pure aluminium: (a) Low magnification; (b) High
magnification.
The wear pattern of Al+10% SiCµm using scanning electron microscopy is shown in Fig. 5.10.
The visible sign of permanent grooves and micro pits are present on the mating surface. The
presence of 10 wt. % SiC dramatically reduces the development of delamination mechanism
which can be due to the high hardness imparted by silicon carbide particles. Further, silicon
carbide particles reduces the matrix adhesion to counterface leading to decrease in wear loss
[117]. Existence of fractured layer is also evident which may be the possible reason of
improvement of wear resistance of the composites [118].
(a) (b)
Micro pits
Figure 5.10 SEM morphologies of worn surface of Al+10% SiCµm: (a) Low magnification;
(b) High magnification.
The worn surfaces of hybrid composites are shown from Fig. 5.11-5.14. The composite
reinforced with 1 wt. % SiC nanoparticles is displaying apparent sign of various scratches and
grooves in wear track direction which verifies existence of abrasion wear mechanism. Further,
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Fig. 5.11 (b) is showing presence of fractured particles and shallower scratches that validates
loss of material also due to abrasive wear mechanism [91,119]. However, further addition of
SiC nanoparticles in the composites causes development of loose oxide layer of aluminium
and iron along with fragmented SiC particles on Al+10% SiCµm+3%SiCnm hybrid composites
worn surface (Fig. 5.12 a-b) due to development of cyclic stress on rubbing surface. This
developed layer is known as mechanically mixed layer which enhances the wear resistance of
hybrid composites because MML works as lubricating agent as reported in previous literatures
[7,120]. Fig 5.13 (a-b) shows worn surface of hybrid composites containing 5 wt. % of nano-
SiC reinforcement. The worn pattern is indicating that surface is relatively smooth and grooves
are mostly restricted because of following reasons: (a) uniform distribution of reinforcement
particles as supported by elemental mapping images, (b) hardness imparted by micro-SiC and
nano-SiC particles to soft aluminium matrix, (c) presence of oxide layer (MML) on mating
surface [69]. Fig 5.14(a-b) shows worn surface of hybrid composites containing highest
amount of nano-SiC reinforcement. The worn surface of Al+10%SiCµm+7%SiCnm is showing
the evidence of debonding/pullout of reinforcement from the matrix which is the main cause
of increased wear loss. Further, at high concentration of nanoparticles the clustering and
agglomeration cannot be avoided which deteriorates the sintering operation [92]. Therefore,
interfacial bond between matrix and reinforcements reduces which is also the main reason of
gross material loss due to severe delamination under sliding environment.
(a) (b)
Shallower scratches
High magnification.
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(a) (b)
Patches of oxide
layer
Figure 5.12 SEM of worn surface of Al+10% SiCµm+3%SiCnm (a) Low magnification; (b)
High magnification.
(a) Finished surface (b)
Grooves are mostly restricted
representing high wear
resistance
High magnification.
(a) (b)
Debonding/Pullout
Severe delamination
High magnification.
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5.4 Conclusions
In the experimental work, Al-SiCmicro-SiCnano hybrid composites containing 10 wt. % SiCµm

together with different weight fractions of SiCnm (0-7 wt. %) were fabricated by powder
metallurgy method. The important conclusions are given below:
i. SEM, XRD and EDS confirmed the synthesis of hybrid nanocomposites.

ii. Elemental mapping of the fabricated hybrid nanocomposites validated the uniform
distribution nano SiC particles in aluminium matrix.
iii. Inclusion of nano SiC increases the hardness of hybrid composites up to 5 wt. % addition.
However, hardness of hybrid composite reinforced with 7 wt. % nano-SiC is decreased
due to low relative density at high particle concentration.
iv. The nanocomposites reinforced with 5 wt. % SiC nanoparticles are most wear resistant
than other hybridized and non-hybridized composites. Further reinforcement reduced the
wear behaviour due to poor compaction, clustering and deterioration of particle bonding
during sintering operation.
v. The wear behaviour of all fabricated composites are directly related to sliding distance and
applied load.
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6. Surface Characterization, Wear Investigation and Statistical Modelling
of Micro and Nano-SiC Reinforced Aluminum Hybrid Composites
6.1 Introduction
The demand of high performance composite materials have been exponentially rising due to
exposure to harsh engineering environments. Therefore, extensive research work have been
directed on the development of Aluminium Matrix Composites (AMCs) due to their high
specific strength, stiffness, good wear resistance, better thermal conductivity and lower thermal
expansion [1,2]. These exceptional properties of have provided a major space for the
production of various parts in aerospace, defense and automotive industries [77,111]. Apart
from these superior properties, the enhancement in wear behaviour of AMCs has attracted great
attention in the field of tribology. The material loss due to wear in many engineering
applications is most commonly encountered phenomena that creates the requirement of
replacement of parts and assemblies of working plants. Further, the operating economy is also
severely affected by wear due to following reasons: (a) due loss of materials, (b) high fuel
usage, and (c) frequent replacement of engineering components. Thus, appropriate assessment
of tribological behaviour of AMCs is very essential.
In this context, both tribological and mechanical behaviour of aluminium matrix composites
have been improved by reinforcing various hard ceramic particles like SiC [79], B4C [61],
Al2O3 [55] and TiC [69] etc. Amongst these, most widely used ceramic particles are SiC due
to its density, which is comparable to aluminium. Further, SiC projects various outstanding
features like high hardness, high wear resistance and fair thermal stability. In addition, SiC
does not react with aluminium at low temperatures thus preventing the growth of unwanted
brittle reaction at interfaces [103,121].
In tribological applications, micro and nano particles reinforced aluminium matrix composites
have been increasingly explored because of following reasons: (a) soft aluminium matrix
skeleton is supported by micro particles [8,9], (b) nanoparticles addition controls the loss of
fracture toughness and ductility, which prevents catastrophic failure during service [7], (c)
overall performance of the composites can be enhanced by the uniform distribution of
nanoparticles due to Orowan strengthening mechanism, (d) when the reinforcement size
reduces from micro to nano, enhanced microstructure and mechanical behaviour can be
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obtained [6], and (e) nanoparticles also enhance mechanical properties by encouraging fine
grain structure and obstructing dislocation movement. However, at relatively high
concentration of micro particles the composite losses its ductility because cracks occur during
bearing load. Therefore, synergistic enhancement in the tribological behaviour can be
accomplished by decreasing the amount of micro particles and raising the concentration of
nanoparticles.
Amongst numerous synthesis techniques of aluminium matrix composites, powder metallurgy

is most preferred option because processing temperature is low which restricts the propagation
of interface reactions [103,121]. Further, uniform distribution of reinforcements in matrix and
development of near net shaped products are the added advantages of powder metallurgy
technique. However, assessment of tribological behaviour of composites is a complex
phenomenon because it depends upon various factors like reinforcement [122] (volume
fraction, size, shape and nature), sliding distance [115], sliding speed [123] and applied load
[124]. Therefore, scientific assessment of tribological behaviour of AMCs are very important
using statistical technique in order to reduce time and cost.
Further, the exhaustive literature survey reveals that use of statistical approach is very limited
to analyze the tribology behaviour of aluminium matrix nanocomposites. Therefore, the
present work has the following objectives: (a) To investigate the effect of nano-silicon carbide,
sliding distance and applied load using full factorial experimental design, (b) To analyze the
wear phenomena using both SEM and EDS technique, (c) To develop models to estimate the
tribological behaviour of aluminium matrix composites fabricated through powder metallurgy
technique, and (d) To recognize the best model for prediction of wear loss using statistical
analysis.
6.2 Materials and Methods
For investigation five combinations of powders given below were thoroughly mixed in
centrifugal ball mill (FRITSCH, Germany).
 Al+10%SiCµm,
 Al+10%SiCµm+1%SiCnm,
 Al+10%SiCµm+3%SiCnm,
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 Al+10%SiCµm+5%SiCnm and
 Al+10% SiCµm+7%SiCnm
The rotational speed and ball to powder ratio were 125 rpm and 10:1, respectively to prepare
homogeneous mixture. The mixed powders were compressed in uniaxial hydraulic machine to
prepare green samples. Green pallets of dimensions 8 mm and height 13 mm were fabricated
at 585 MPa compaction pressure. The die and plungers were cleaned and lubricated with
acetone and zinc stearate respectively to prevent the jamming along with easy removal of
pallets. The samples were then sintered at 450 °C in electric tubular furnace for 1 hour. The
sintering is performed under constant flow of argon gas (flow rate=1litre/min.) to safeguard
the composites from oxidation [75]. The dry sliding wear test of the specimens were performed
on pin-on-disc equipment (Ducom, Model No: TR-201 CL, Bangalore, India) according to full
factorial design given in Table 6.1. Prior to each experiment specimens were polished and
cleaned thoroughly with acetone to remove adhered wear debris.
The weight of the specimens were noted before and after the test using an electronic balance
with an accuracy of 0.1 mg. For every set of experimental conditions the test were performed
three times and average value is considered as wear loss.
6.3 Experimental Plan
For investigation, the experiments were conducted according to full factorial design [58].
Three factors were chosen in which one factor has five levels, whereas other two factors have
three and two levels respectively. Concentration of nano silicon carbide, sliding distance and
applied load were the three independent factors. Table 6.1 shows the magnitude and different
levels of each independent variables. The full factorial design finds huge application in early
stages of experimental work, particularly when the number of independent variables are less
than or equal to 4. The current full factorial design consists of 30 rows and 3 columns as shown
in Table 6.2.
Table 6.1 Full factorial design (5×3×2) of experiments and their respective.
Level Level
Control factors Unit Level I Level II Level V
III IV
SiC reinforcements
Wt. % 0 1 3 5 7
(A)
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Sliding distance (B) m 300 600 900 - -
Applied Load (C) N 20 40 - - -
Table 6.2 Multilevel factorial design of experiments.
SiC concentration
S.No. Sliding distance (m) Applied load (N) Wear loss (mg)
(wt. %)
1 0 300 20 3.0
2 0 300 30 4.7
3 0 600 20 4.1
4 0 600 30 5.3
5 0 900 20 5.6
6 0 900 30 5.9
7 1 300 20 2.7
8 1 300 30 3.5
9 1 600 20 2.7
10 1 600 30 4.2
11 1 900 20 4.7
12 1 900 30 5.1
13 3 300 20 1.8
14 3 300 30 3.1
15 3 600 20 2.3
16 3 600 30 3.6
17 3 900 20 4.3
18 3 900 30 4.5
19 5 300 20 1.1
20 5 300 30 1.7
21 5 600 20 1.6
22 5 600 30 2.5
23 5 900 20 3.5
24 5 900 30 3.9
25 7 300 20 1.3
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26 7 300 30 2.1
27 7 600 20 1.7
28 7 600 30 3.1
29 7 900 20 3.7
30 7 900 30 4.1
6.4.1 Porosity and Hardness measurements
Fig. 6.1 displays the percentage porosity and hardness of all fabricated composites with respect
to nano-SiC addition. It has been found that as the micro-SiC particles are added to aluminium
matrix the porosity of the composites increases. The rise in porosity is due to the hard nature
of SiC which hinders the compaction process and creates the micro porosities [92]. However,
addition of nano-SiC particles reduces the porosity upto 3 wt. % because the available micro
porosities are filled up by the nanoparticles [76]. Further, increment in nanoparticles drastically
grows the porosity because of the following reasons: (a) clustering and agglomeration at high
concentration of nanoparticles, and (b) dense, random distribution and high melting point of
silicon carbide particles hinders the effective sintering operation [6].
7 75
Porosity (%) Rockwell hardness 70
6
65
Rockwell hardness
5 60
Porosity (%)
4 55
50
3 45
2 40
35
1
30
0 25
Figure 6.1 Porosity and Hardness variation with respect to silicon carbide addition.
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The variation of hardness of all fabricated composites have been plotted in Fig. 6.1. The
hardness of pure aluminium is 28.86 which reaches 47 when 10 wt. % of SiC micro particles
are reinforced in aluminium matrix. The rapid escalation in the hardness is because of the hard
nature of SiC particles. Further, addition of nano-SiC particles in aluminium increases the
hardness of the composites up to 3 wt. %. Uniform distribution, reduced porosity, enhanced
dislocation caused by hard ceramic particles and good interfacial bonding between
reinforcement and aluminium are the underlying reasons for the remarkable enhancement in
hardness. These results are in accordance with findings of previous research work [6,7].
However, further addition of nanoparticles declines the hardness due to rise in porosity and
clustering of nanoparticles [113].
6.4.2 Analysis of variance (ANOVA)
The experiments were performed as per full factorial design of experiments and their
corresponding wear values have recorded in Table 6.2.
Table 6.3 Analysis of variance for the wear loss.
Source DF Seq SS Adj SS Adj MS F P Pr
SiC concentration (wt. %) 4 21.77 21.77 5.4 114.79 0.000 42.4
Sliding distance (m) 2 21.68 21.68 10.85 228.8 0.000 42.3
Applied load (N) 1 5.8 5.8 5.80 122.49 0.000 11.3
SiC concentration (wt. %)*

8 0.34 0.34 00.043 0.92 0.546 0.5
SiC concentration (wt. %)*
4 0.148 0.148 0.0372 0.78 0.566 0.1
Applied load (N)
Sliding distance (m)*
2 1.154 1.154 0.5770 12.17 0.004 2.3
Applied load (N)
Error 8 0.379 0.379 0.0474 0.7
Total 29 51.30
𝑅 − 𝑆𝑞 = 99.26% 𝑅 − 𝑆𝑞(𝑎𝑑𝑗) = 97.32%
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Analysis of variance is a statistical tool which is used to find out the influence of independent
variables (SiC reinforcements, sliding distance and applied load) and their percentage
contributions on the experimental results (wear loss). ANOVA calculations were performed
using MINITAB-17 software. This analysis was undertaken for a level of significance of 5%.
Analysis of variance finds the F-ratio, which gives the level of significance of independent
variables by considering the variance of all terms included in the error term at desired
significance level. Table 6.3 provides the ANOVA results for the wear loss of all the
composites. The percentage contribution of each independent factors are also incorporated in
the last column of Table 6.3. Table 6.3 clearly shows that concentration of nano silicon carbide
(42.4 %) and sliding distance (42.3 %) has the highest contribution on the wear loss. While,
the applied load has only 11.3 % contribution to the wear loss which is relatively less. The
contribution of interaction between these parameters have further shown relatively less
significance. However, the greatest influence of interaction is sliding distance and applied load
which is 2.3 %, whereas the other interactions concentration*sliding distance and
concentration*load are contributing only 0.5 and 0.1 % only. Therefore, the investigation
revealed that the selected independent variables (silicon carbide reinforcement, sliding distance
and applied load) and their respective interactions have statistical and physical significance on
the wear behaviour of fabricated hybrid composites [62,118].
The effect of each independent variables on wear behaviour can be analyzed with the help of
main effect plot and interaction plot. Fig. 6.2 is the main effect plot, depicts the effect of
different process parameters on the wear loss. According to the theory if a line of any process
parameter in the main effect plot has a low variation with respect to the mean value, then it
interpreted that the given process parameter has no significant effect [59]. On the other hand,
plot of any process parameter having a higher slope with respect to the mean value provides a
significant effect. So, it is evident from the main effect plot that the SiC concentration is the
most influential parameter followed by sliding distance and applied load. The main effect plot
also confirms that as the concentration of SiC increases in aluminium composites its wear
resistance increases. Further, main effect plot depicts that the wear resistance of composite
increases drastically by the addition of nano-SiC particles up to 5 wt. %. This enhancement in
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the wear resistance can be attributed to the following reasons: (a) Hardness imparted by
nanoparticles to soft aluminium matrix, (b) plastic flow of the material during sliding
environment is restricted by nanoparticles [114], and (c) ratio of hard to soft surface is
increased which supports the sliding load at high concentration. However further addition of
nanoparticles suddenly declines the wear resistance of nanocomposites because of sharp
growth in porosity. Additionally, heterogeneous distribution, clustering of nanoparticles and
inefficient sintering process at high concentrations causes severe material loss due to
delamination [92].
The influence of sliding distance and load for all synthesized composites can be inferred from
interaction plot (Fig. 6.3). The interaction plot confirms that as sliding distance increases the
wear loss of all composites also increases which follows the trend proposed by Archard wear
equation. Moreover, wear loss have a direct relation with sliding distance because of following
factors: (a) protective oxide layer becomes unstable with increment in sliding distance [92,115]
and (b) interfacial bonding of reinforcements and matrix becomes weak due to thermal
softening. However, the nanocomposites containing 5 wt. % of nano-SiC particles exhibits best
wear resistance. This fashion follows the general rule, harder the material superior would be
the abrasive and wear resistance. With the help of interaction plot it can be inferred that
material loss due to wear is low at low applied load and vice-versa. The outcomes are following
the trends suggested by earlier literature [85,87]. However, at high applied load greater amount
of frictional heat is developed which lowers the interfacial bond and increases the chance of
severe delamination [116]. Softened mating surfaces also enhances the probability of
penetration of asperities.
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Main Effects Plot for Wear loss (mg)
Data Means
SiC concentration (wt. %) Sliding distance (m)
4.5
4.0
3.5
3.0
2.5
Mean
0 1 3 5 7 300 600 900

Applied load (N)
4.5
4.0
3.5
3.0
2.5
20 30
Figure 6.2 Main effect plot for independent variables on wear loss of Al-SiCmicro-SiCnano
nanocomposites.
Interaction Plot for Wear loss (mg)

Data Means
300 600 900
6
S iC
concentration
4 (w t. % )
SiC concentr ation (wt. % ) 0
1
2 3
5
6
S liding 7
distance
4 (m)
Sliding distance (m) 300
600
2 900
6
A pplied
load (N )
4 20
A pplied load (N) 30
0 1 3 5 7 20 30
Figure 6.3 Interactions of various independent variables on wear loss.
6.4.4 Investigation of wear mechanism by SEM
To analyze the wear mechanism Scanning Electron Microscopy have been performed for all
synthesized nanocomposites and aluminium as displayed in Fig. 6.4(a-f). The worn surface
morph graphs of composites reinforced with nano particles exhibits dissimilar wear profile
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when matched to unreinforced aluminium matrix. This verifies the variation in wear
mechanism. Large amount of craters, pits and grooves have been observed on pure aluminium
surface as shown in Fig. 6.4(a). Severe plastic deformation also occurs on aluminium surface
due to generation of frictional heat and hence escalated wear loss in comparison to other micro
and nanocomposites [89]. Existence of severe delamination on worn surface of pure aluminium
is confirmed by SEM morph graphs.
Fig. 6.4(b) shows the presence of micro pits and permanent grooves on worn surface of Al-
10% SiCµm composite. Addition of silicon carbide particles diminishes the wear loss of
composites due to increased hardness. Additionally, decline in wear loss is because of reduced
adhesion of matrix material on counter disc due to presence of silicon carbide particles [117].
Fig. 6.4(c-f) exhibit the worn morphologies of composites reinforced with nanoparticles. At 1
wt. % SiC nanoparticles addition, the morph graphs (Fig. 6.4 c) displays the obvious sign of
grooves and shallower scratches that confirms material loss due to abrasion [119]. The
development of oxides of aluminium and iron occurs along with fragmented silicon carbide
particles on further addition SiC nanoparticles (Fig. 6.4d) because of frictional heat and cyclic
stress developed at mating surfaces. The oxides of aluminium, iron and fragmented silicon
carbide particles are together, known as mechanically mixed layer (MML) that reduces wear
loss of nanocomposites. MML is hard in nature that inhibits direct metallic interaction as
reported in previous literature [7]. The worn surface of composite having 5 wt. % of SiC
nanoparticles is displayed in Fig. 6.4(e). This surface appears to be even and grooves are mostly
controlled as suggested by SEM morph graphs. Homogeneous distribution of micro and
nanoparticles, enhanced hardness and presence of MML at the mating surfaces are the major
reason for enhanced wear resistance [69]. The worn surface of Al+10% SiCµm+7%SiCnm
nanocomposites is shown in Fig. 6.4(f). The morph graphs display that reinforced particles are
debonded/pulled out from the aluminium matrix, thus, reduces wear resistance. Proper
sintering operation is hindered due to clustering and agglomeration of nanoparticles at high
concentrations [92]. Moreover, escalated porosity, reduced hardness and poor interfacial bond
between aluminium and silicon carbide particles are principally responsible for sudden drop in
wear resistance.
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(a) (b)
Delamination and grooves
(c) (d)
Shallower scratches
MML
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(e) (f)
Grooves are limited signifying
Debonding/Pullout and
reduced wear loss
Severe delamination
composites.
6.4.5 Wear debris analysis
The mechanism of wear have been also studied by performing Scanning Electron Microscopy
of wear debris. The fragmented particles micrographs obtained from wear test for all fabricated
composites and nanocomposites are presented in Fig 6.5 (a-f). Fig 6.5(a) exhibits the wear
debris of aluminium which is in the form of thin sheets/elongated debris. These
sheets/elongated debris are the clear indication of severe plastic deformation and determines
wear due to delamination. The wear debris of Al-10%SiC composites is shown in Fig 6.5(b),
which contains particles with thin adhered fragments. Further, it is observed that average size
of debris obtained have reduced because of hard SiC reinforcements. Some evidence of loose
particles and thin sheets are obvious in wear debris of composite reinforced with 1wt. % of
SiC nanoparticles as shown in Fig. 6.5(c). At few locations evidence of grooved sheets are
found, confirming wear loss due to abrasion. The wear debris of Al+10% SiC µm+3%SiCnm
nanocomposites is shown in Fig 6.5(d). SEM micrographs shows that as the quantity of SiC
nanoparticles is enhanced from 1 to 3 wt. %, the size of the wear debris collected reduces.
Further, clusters of particles are evident which is due to the effect of micro machining during
sliding environment. Fig 6.5(e) shows the wear debris of nanocomposites containing 5 wt. %
of SiC nanoparticles. The micrographs indicates that debris consists of fine particles of uniform
size. Further, decrease in debris size may due to following factors: (a) enhanced hardness
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imparted by nanoparticles, (b) reduction in porosity, and (c) development of protective
mechanically mixed layer. Fig. 6.5(f) shows the wear debris of nanocomposites containing
highest amount of silicon carbide nanoparticles. The wear debris consists of combination of
large amount of coarse particles (large strip debris) with irregular shapes. Hence, it can be
concluded that amount of silicon carbide concentration dictates the size and morphology of
wear debris. The EDS of Al+10%SiCµm+5%SiCnm and Al+10% SiCµm+7%SiCnm
nanocomposites wear debris have been shown in Figs. 6.6(a-b). The high intensity of Si and
low intensity of Al validates the smearing of silicon carbide particles from the sample during
sliding environment. Further, peaks of Fe are also evident in both the EDS spectrum because
hard SiC particles abrades the counter disc material. In both the EDS results, peak of oxygen
is also observed because of development of aluminium oxide and iron oxides due to combined
effects of frictional heat and environmental reactions [58].
(a) (b)
Elongated debris
Loose particles and thin

sheets
(c) Fine abraded particles (d) Clusters of particles
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(e) (f)
Uniform size debris
Severe delamination
composites.
(a) (b)
Figure 6.6 EDS of wear debris: (a) 5 wt. % SiCnano and (b) 7 wt. % SiCnano reinforced Al
composites.
6.4.6 Mathematical modelling and statistical analysis of models
Linear regression models were developed using a statistical software, MINTAB 17 for
predicting wear loss. The regression models describes the relationship between independent
variables and output value by fitting a linear and quadratic equations [58,62]. The statistical
analysis revealed that wear loss is dependent on following factors viz. SiC reinforcement,
sliding distance and applied load, which are independent variables. The standard Archard wear
equation [52] suggests that the wear loss is directly proportional to sliding distance and external
load. However, it does not include the factors of reinforced particles in any metal matrix
composites. Additionally, interaction of these factors are also difficult to calculate. To
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encounter such a complex tribological phenomenon, a number of efforts have been directed to
empirically model the wear behaviour in terms of independent factors and their interactions
[58,62]. Aligned with this, under the current approach, different empirical correlations have
been developed which highlight the significance of input variables and their interactions on the
wear behaviour of aluminium nanocomposites within the considered range of interest. Further,
only those factors and interactions are considered which are significant on the basis of ANOVA
analysis (as depicted in Table 6.3) namely, SiC concentration, sliding distance, applied load
and their interactions. The analysis comprises the development of five different predictive
models in which one was linear and four were quadratic in nature.
The models for prediction of wear loss is given below:
Model 1
𝑊𝑙𝑜𝑠𝑠 = 0.113902 − 0.30122 × 𝐴 + 3.38333 × 10−3 𝐵 + 0.088 × 𝐶 [6.1]
Model 2
𝑊𝑙𝑜𝑠𝑠 = −1.6361 − 0.30 × 𝐴 + 0.0063 × 𝐵 + 0.158 × 𝐶 − 1.16667 × 10−4 𝐵𝐶 [6.2]
Model 3
𝑊𝑙𝑜𝑠𝑠 = 0.46 − 0.750 × 𝐴 + 3.3 × 10−3 𝐵 + 0.088 × 𝐶 + 0.064 × 𝐴2 [6.3]
Model 4
𝑊𝑙𝑜𝑠𝑠 = 1.46 − 0.30 × 𝐴 − 0.002 × 𝐵 + 0.088 × 𝐶 + 4.5 × 10−6 × 𝐵 2 [6.4]
Model 5
𝑊𝑙𝑜𝑠𝑠 = 0.062 − 0.75 × 𝐴 + 0.0009 × 𝐵 + 0.158 × 𝐶 + 0.065 × 𝐴2 + 4.5 × 10−6 𝐵 2 −
1.16667 × 10−4 𝐵𝐶 [6.5]
Using equations from (6.1-6.5), wear loss of all fabricated composites were estimated for all
30 set of experiments. The experimental wear loss and all models predicted values are plotted
in Fig. 6.7. The predicted wear loss form the model and experimental data are very close to
each other. Further validation of predicted values and experimental values is shown in Fig. 6.8
by scatter diagram.
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0.007
Experimental data
Predicted data (Model-1)
0.006 Predicted data (Model-2)
0.005
Wear loss(g)
0.004
0.003
0.002
0.001
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
Experimental trials
Figure 6.7 Estimated values of wear loss from prediction models and experimental readings.
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Figure 6.8 Scatter plot between experimental wear loss and estimated values from models.
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6.4.7 Statistical analysis of regression models
Five most commonly used statistical indicators were adopted to perform the statistical analysis
of developed regression models. The mathematical equations of these indicators are given
below:
 WLoss (i,exp.)  WLoss (i ,mod el ) 

1 m
i. MBE  [6.6]
m i 1
1/2
1 m 2

ii. RMSE    WLoss (i ,exp.)  WLoss (i ,mod el   [6.7]
 m i 1 
100 m WLoss (i ,exp.)  WLoss (i ,mod el )

iii. MAPE  |
m i 1 WLoss (i ,exp.)
| [6.8]

1 m
iv. MAE  [6.9]
m i 1
 W  WLoss ( i ,exp.) 
m
2
Loss ( i ,mod el )
v. R  1 i 1
[6.10]
 W  WLoss ( i , avg .) 
m
2
Loss ( i ,mod el )
i 1
The results of all statistical indicators [Eqs. (6.6) - (6.10)] of developed regression models have
been shown in Table 6.4. The significant value of each statistical indicators are marked bold
in the Table 6.4. The value of MBE lies in the range of -9.20E-10 to -4.00E-09 which is
showing negative sign, which means the underestimation of data. However, the overall value
of MBE for all model are significantly small and close to zero. Finally, model 3 exhibits the
significant value of MBE (closest to zero). RMSE values of all models are found to be small
having the least value 0.000272 for Model 5. The range of MAPE values were observed as
7.9045% to 14.8269% with Model 5 demonstrating the least value. Correlation Coefficient (R)
of all models lies in the range 0.9289-0.9932 which validates the good fitting of data. The
highest value of R is observed for Model 2. The values of MAE were found in the range from
0.00022535 to 0.00040356 with least observed for Model 5.
Within each developed models, the MBE value of Model 1 is least. The coefficient of
determination of Model 2 is lowest, while RMSE, MAPE and MAE of Model 5 is lowest
among all developed regression analysis. This signifies the satisfactory performance of all
models as compared to the experimental data. However, which model is best among all is still
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not confirmed because all the statistical error is not going in favor of one specific regression
model. Due to this reason, in the next section the further analysis of the developed models have
been considered.
Table 6.4 Statistical indicators of developed regression models.
Model MBE RMSE MAPE R MAE

M1 -4.00E-09 0.000484 14.8269 0.9289 0.00040356
M2 -9.00E-09 0.000463 14.2106 0.9931 0.00037844
M3 -9.20E-10 0.000362 9.5729 0.9600 0.00028667
M4 -6.00E-09 0.000445 12.8691 0.9549 0.00036211
M5 -4.22E-09 0.000272 7.9045 0.9613 0.00022535
6.4.8 Ranking of models by Global Performance Indicator (GPI)
It is interesting to see that all statistical indicator is showing different patterns and hence failing
to identify a best predictive model. Therefore, this difficulty is removed with further
improvement in the results of statistical analysis using Global performance indicator (GPI).
Global performance indicator is a useful technique developed by Despotovic et al. [125] that
accumulates the effect of all the individual statistical indicators. In this technique, all the
statistical indicators are scaled-down in such a way that all values lies between zero and one
[126]. The scaled-down values are then deducted from their corresponding medians,
respectively. Lastly, with the appropriate weight factors all the calculated values are added
together. The mathematical equation of GPI for ith model may be defined as:
5
GPI i    k ( yk  yik ) [6.11]
k 1
Where, 𝛼𝑘 equals to -1 for the indicator R only, however for remaining indicator its value is
recommended as 1. yk represents median of scaled values of indicator k, yik is scaled value of
indicator k for model i. The model completing the highest GPI value means more accurate
model.
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Table 6.5 Statistical indicator (Scaled), GPI and Ranking of the models
Model MBE RMSE MAPE R MAE GPI Rank

M1 0.6188 1.0000 1.0000 0.0000 1.0000 -1.2120 5
M2 0.0000 0.8984 0.9109 1.0000 0.8590 0.7384 3
M3 1.0000 0.4227 0.24102 0.4845 0.3441 0.8835 2
M4 0.3713 0.8151 0.7172 0.4051 0.7674 0.1409 4
M5 0.5916 0.0000 0.0000 0.5052 0.0000 2.3204 1
The scaled value (between 0 and 1) of all statistical indicators along with their corresponding
GPI and subsequent ranking for all developed models are tabulated in Table 6.5. The GPI
values lies between -1.2120 and 2.3204. The maximum GPI is found to be 2.3204 for Model
5, which consist of all independent terms viz. silicon carbide concentrations, sliding distance,
applied load and interactions (sliding distance and applied load) as was previously suggested
by ANOVA analysis (as depicted in Table 6.3). Among all the models, the top performer is
Model 5. Therefore, this model can be used to estimate the wear loss of aluminium matrix
nanocomposites with high level of accuracy within the selected range of investigations.
6.5 Conclusions
In this investigation the full factorial design have been successfully implemented and described
to comprehend the tribological behavior of aluminium hybrid nanocomposites. The following
major conclusions are described below:
i. Addition of SiC nanoparticles reduced the porosity and enhanced the hardness. The
nanocomposites reinforced with 5 wt. % SiC showed superior hardness among all
fabricated nanocomposites.
ii. The increase in sliding distance and applied load leads to an increase in the wear
loss of the composites. An addition of SiC nanoparticles reduces the wear loss and
it reaches to minimum at 5 wt. %. Further addition of SiC increases the wear loss
due to sudden rise in porosity.
iii. The most significant factors influencing the wear behavior were deduces based on
ANOVA as silicon carbide concentration (42.4%), sliding distance (42.3%) and
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applied load (11.3%), together with the interaction effect of the sliding distance and
applied load (2.3%), within the selected span of interest.
iv. SEM of worn surfaces exhibit that delamination and abrasion are dominant wear
mechanism. EDS analysis confirmed the formation of mechanically mixed layer
(MML) at mating surfaces, responsible for enhanced wear resistance.
v. Five different regression models were developed using MINITAB 17 software for
estimation of wear loss as a function of silicon carbide concentration, sliding
distance and applied load.
vi. For models under consideration, the GPI was found in the range between -1.2120
and 2.3204. The GPI of model 5 was highest, hence the best model to estimate the
wear loss.
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7. Characterization of Surface Morphology, Wear Performance and
Modelling of Graphite Reinforced Aluminium Hybrid Composites
7.1 Introduction
Aluminium matrix composites (AMCs) have become a revolutionary materials all around the
globe for its wide application in structural, automobile and aerospace industries
[1,55,77,79,97,103]. The important features such as low density, improved mechanical
properties, and high wear resistance are the major reason for the acceptance of AMCs in large
engineering applications where customized properties are required [93]. The fabrication
process, size, distribution and orientation of reinforced particles dictates the final properties of
AMCs. Numerous available fabrication techniques, such as mechanical alloying [94], stir
casting [95] and powder metallurgy [96] have been adopted by recent researchers to fabricate
enhanced wear resistance AMCs. However, powder metallurgy (PM) gained more attention to
produce AMCs because of its potential advantages such as homogeneous distribution of
reinforcement in matrix and minimum possibility of development of intermetallic phases (due
to low processing temperature). Further, on large scale production, PM is economical because
costly machining processes are minimized due to production of near net shaped products
[97,118].
In tribological applications, micro and nano particles reinforced AMCs, known as hybrid
composites, have been increasingly explored because of following reasons: (a) soft aluminium
matrix skeleton is supported by micro particles [8,9], (b) nanoparticles addition controls the
loss of fracture toughness and ductility, which prevents catastrophic failure during service [7],
(c) overall performance of the composites can be enhanced by the uniform distribution of
nanoparticles due to Orowan strengthening mechanism, (d) when the reinforcement size
reduces from micro to nano enhanced microstructure and mechanical behaviour can be
obtained [6], and (e) nanoparticles also enhance mechanical properties by encouraging fine
grain structure and obstructing dislocation movement. However, at relatively high
concentration of micro particles the composite losses its ductility because crack occurs during
bearing load. Therefore, synergistic enhancement in the tribological behaviour can be achieved
by reducing the concentration of micro particles and raising the amount of nanoparticles.
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In this context, both tribological and mechanical behaviour of AMCs have been improved by
reinforcing various hard ceramic particles like ZrO2 [70,98], SiC [77,79], B4C [93], and Al2O3
[55] etc. Amongst these available particles, Zirconia (ZrO2) is least investigated ceramic
particles despite of having various attracting features such as less expensive, easily available,
having high strength, hardness and excellent wear resistance. In addition, ZrO2 does not react
with aluminium at lower temperature thus preventing the growth of unwanted brittle reaction
at interfaces. Further, reinforcing zirconia in aluminium matrix will reduce catastrophic failure
during service condition due to its high fracture toughness in comparison to other available
ceramic particles [103].
AMCs reinforced with graphite is one of the most preferred combination because graphite
enhances both wear resistance and machinability of the composites. During sliding condition
graphite forms a thin layer which prevents direct metal to metal contact and thus reducing wear
loss. Further, graphite prevents severe wear loss at high temperature and its content delays the
commencement of seizure. This high temperature wear and seizure resistance is attributed to
the formation of tribolayer at mating surfaces. So, it would be advantageous to use nano-
zirconia along with micro-graphite as a reinforcement in the aluminium matrix to enhance wear
behaviour. However, assessment of wear behaviour of composites is a complex phenomenon
because it depends upon various factors like reinforcement [123] (volume fraction, size, shape
and nature), sliding distance [115], sliding speed [123] and applied load [124]. Therefore,
scientific assessment of wear behaviour of AMCs are very important using statistical technique
in order to reduce time and cost. Further, the exhaustive literature survey reveals that no
experimental and statistical work is directed towards the study of morphological
characterization and wear behaviour of Al-ZrO2-Gr hybrid composites fabricated through PM
technique. Therefore, the present work has the following objectives: (a) To investigate the
effect of graphite addition, sliding distance and applied load using full factorial experimental
design, (b) To analyze the wear mechanism by investigating the micrographs of worn surfaces
and wear debris using both SEM and EDS technique, (c) To develop models to estimate the
wear behaviour of aluminium matrix composites and (d) To recognize the best model for
prediction of wear loss using statistical analysis.
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7.2 Materials and Methods
The feature of purchased powders are given in Table 7.1

Table 7.1 Feature of reinforced particles.
Reinforced particles Average particle size Density, g.𝒄𝒎−𝟑

Gr 37 µm 3.21
ZrO2 30-50 nm 5.89
The following six combinations were fabricated through PM process
i. Al (Pure).
ii. Al+10%ZrO2.
iii. Al+10%ZrO2+2%Gr.
iv. Al+10%ZrO2+4%Gr.
v. Al+10%ZrO2+6%Gr.
vi. Al+10%ZrO2+8%Gr.
Initially, required amount of powders containing aluminium, zirconia and graphite were
measured using a digital weighing machine with least count of 0. 1 mg. These calculated
powder were mixed thoroughly in centrifugal ball mill for 20 min. at a speed of 125 rpm at
room temperature. While mixing, 10:1 BPR (Ball to powder ratio) were fixed to reduce the
possibility of clustering of used powders. Both mixing chamber and balls were made of
hardened steel. Further, mixed powders were consolidated using uniaxial hydraulic pallet press
at 585 MPa load at room temperature. Cylindrical pallets of dimension 8 mm diameter and 13
mm height were fabricated for sintering operation. Both plungers and die were properly
cleaned and lubricated manually with zinc stearate after each compaction for appropriate
working of die. After cold compaction samples were sintered at 450-470 0C for 1 hour under
constant flow of argon gas (flow rate=1 litre/min.) in tubular electric furnace [75]. The samples
were left in the furnace to cool down to room temperature. The hardness of composites were
calculated using a Rockwell hardness machine with a hardened steel balls (indenter) of
diameter 1/8” (inch). The load and dwell time for hardness measurement were 60 kgf (Scale
H) and 8 seconds respectively. Three indentations were taken on the samples to find the
average hardness at room temperature. The following conditions given in Table 7.2 were used
for performing XRD of fabricated composites. The wear behaviour of composites were
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analyzed on pin-on-disc wear apparatus (Ducom, Model No: TR-201 CL, Bangalore, India)
according to ASTM G99-95a (reapproved) standards. The wear test conditions and their levels
are specified in Table 7.3.
Table 7.2 X-ray diffractometer description.
Equipment conditions Specifications/Description

X-ray diffractometer (D8 ADVANCE) Bruker AXS Inc, Madison, WI, USA
Cu Kα radiation (λ=1.5406 0A)
X-ray source 40mA and 40kV
2θ range 20°–700
Step size 0.01°
Speed of scanning 0.02 steps/second
Table 7.3 Sliding wear test variables.

Sample dimension Diameter 8mm and height 13mm
Sliding distance 400, 600, 800 (m)
Applied load 30, 40 (N)
Disc material 65 HRC, EN31 grade steel
7.3 Experimental Plan
The experiments were performed according to full factorial design of experiments [58]. Three
factors were chosen in which one factor has five levels, whereas other two factors have three
and two levels respectively. Concentration of graphite, sliding distance and applied load were
the three independent factors. Table 7.4 shows the magnitude and different levels of each
independent variables. The full factorial design finds huge application in early stages of
experimental work, especially when the number of independent variables are less than or equal
to 4. The current full factorial design consists of 30 rows and 3 columns as shown in Table 7.5.
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Table 7.4 Full factorial design (5×3×2) of experiments and their respective.
Level Level
Control factors Unit Level I Level II Level V
III IV
Gr reinforcements
Wt. % 0 2 4 6 8
(A)
Sliding distance (B) m 400 600 800 - -
Applied Load (C) N 30 40 - - -
Table 7.5 Multilevel factorial design of experiments.

Gr concentration
S.No. Sliding distance (m) Applied load (N) Wear loss (mg)
(wt. %)
1 0 400 30 5.4
2 0 400 40 5.6
3 0 600 30 5.7
4 0 600 40 6.1
5 0 800 30 6.5
6 0 800 40 6.9
7 2 400 30 4.1
8 2 400 40 4.4
9 2 600 30 4.8
10 2 600 40 5.2
11 2 800 30 5.5
12 2 800 40 5.8
13 4 400 30 3.0
14 4 400 40 3.6
15 4 600 30 4.1
16 4 600 40 4.4
17 4 800 30 4.8
18 4 800 40 4.9
19 6 400 30 1.5
20 6 400 40 1.8
21 6 600 30 1.9
22 6 600 40 2.7
23 6 800 30 2.7
24 6 800 40 3.1
25 8 400 30 2.0
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26 8 400 40 2.4
27 8 600 30 3.1
28 8 600 40 3.7
29 8 800 30 3.6
30 8 800 40 4.4
7.4.1 Morphological characterization of composites
The XRD graphs of fabricated composites are shown in Fig. 7.1. From XRD plot the presence
of zirconia and graphite are confirmed from their respective peaks. The aluminium shows the
highest peak followed by zirconia and graphite. The peak intensities of ZrO2 and graphite is
low in comparison to aluminium peak because of their low concentration. Therefore, it can be
determined that fabricated samples are reinforced with ZrO2 and graphite. The software,
DIFFRAC plus (Bruker AXS Inc.) is used for calculations.
The Energy Dispersive Spectroscopy analysis and their respective microstructure of
Al+10%ZrO2+6%Gr hybrid composite is shown in Fig. 7.3. The peaks of Al, Zr, C and O are
obtained from EDS study and shown in Fig.7.2. Further, Table 7.6 displays elements present
in Al+10%ZrO2+6%Gr composites with their weight and atomic percentage in composite.
Hence, evidence of zirconia and graphite particles are again confirmed in synthesized
composites.
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Figure 7.1 XRD of Al+10% ZrO2, Al+10% ZrO2+2% Gr, Al+10% ZrO2+4% Gr, Al+10%
ZrO2+6% Gr and Al+10% ZrO2+8% Gr hybrid nanocomposites.
Figure 7.2 EDS of Al+10%ZrO2+6%Gr reinforced composites.
Table 7.6 Elements present in Al+10%ZrO2+6%Gr hybrid nanocomposites.
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C 32.63 49.90
O 14.38 16.51
Al 46.18 31.44
Zr 8.30 3.05
Total 100 100
Fig. 7.3 displays the elemental mapping of Al+10%ZrO2+6%Gr reinforced composite. The
elemental mapping confirms the existence of zirconia (ZrO2) and graphite along with their fair
distribution in aluminium matrix.
(Al)
(Zr) (O)
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(C)
Figure 7.3 Elemental maps of Al+10%ZrO2+6%Gr hybrid composites.
The hardness of Al/ZrO2/Gr hybrid composites with increasing graphite concentration are
shown in Fig. 7.4. The hardness value of Al+10%ZrO2 composite is increased with respect to
pure aluminium matrix because of considerable hard nature of zirconia nanoparticle. The
increment in hardness can be attributed due to subsequent reasons: (a) nanoparticles acts as an
obstacle in the motion of dislocation, (b) elevated hardness of ZrO2 nanoparticle as compared
to matrix material, (c) uniform distribution of nanoparticles in the matrix system, and (d) high
density of ZrO2 nanoparticles [103]. Further, addition of graphite particles reduces hardness of
hybrid composite because of soft nature of graphite. The similar results have been reported by
former researcher [54,79,92].
70
Al
Al+10%ZrO2
60 Al+10%ZrO2+2%Gr
Rockwell Hardness
Al+10%ZrO2+4%Gr
Al+10%ZrO2+6%Gr
50
Al+10%ZrO2+8%Gr
40
30
20
10
Figure 7.4 Variation of hardness with graphite reinforcement in composites.
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7.4.3 Sliding wear behaviour
7.4.3.1 Effect of graphite addition

The wear loss pattern of the fabricated composites with increasing graphite content are shown
in Fig. 7.5. This is obvious form the bar graph as the graphite content is increased in hybrid
composites its wear resistance have been enhanced. The enhancement in the wear resistance
can be attributed due to the formation of tribolayer under the presence of graphite particle
which is released during sliding condition. Similarly, as the graphite concentration is increased
the probability of releasing graphite particles is increased on mating surface and thus further
enhancing the wear resistance [34,89,127–129].
Further, graph shows that wear loss of hybrid composites increases when Gr particles
reinforcement increases from 6 to 8 wt. %. The main possible reason for the increase in wear
loss could be as follows: (a) escalated amount of graphite leads to the heterogeneous
distribution in aluminium matrix (b) decrease in fracture toughness of hybrid composites at
higher graphite concentration [59].
25
Pure Al
Al+15%ZrO2
Al+15%ZrO2+2%Gr
20
Al+15%ZrO2+4%Gr
Al+15%ZrO2+6%Gr
Wear loss (mg)
Al+15%ZrO2+8%Gr
15
10
Figure 7.5 Variation of wear loss with concentration of graphite reinforcement in

composites.
7.4.3.2 Effect of sliding distance

The wear loss pattern of the fabricated composites with increasing sliding distance are shown
in Fig. 7.6. It is obvious from the plot that the wear resistance of Al+15%ZrO2+6%Gr hybrid
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composites is significantly higher than the other hybridized or non-hybridized composites.
This improvement is achieved by presence of graphite particle which is released during sliding
condition and formed a protecting tribolayer between pin and counter disc surface[89,130].
Another reason for the improvement in wear behaviour can be attributed to the fact that
increased percentage of graphite reduced the friction between the rubbing surfaces
consequently reducing the temperature rise. So, the thermal softening phenomena reduces
which lowers the wear loss.
However further addition of graphite from 6 to 8 wt. % to aluminium composite the wear loss
of hybrid composite increases at all sliding distance. This deterioration in wear properties is
due to the following reasons: (a) high concentration of graphite reduces the fracture toughness
of composites [59] (b) reduction in hardness due to soft nature of graphite particles [92].
20
Pure Al
18 Al+10%ZrO2
16 Al+10%ZrO2+2%Gr
Al+10%ZrO2+4%Gr
14
Al+10%ZrO2+6%Gr
Wear loss (mg)
12 Al+10%ZrO2+8%Gr
10
0
100 200 300 400 500 600 700 800 900
Figure 7.6 Influence of sliding distance on wear loss of hybrid composites.
7.4.3.3 Effect of applied load

The effect of applied load on wear loss of all fabricated samples are shown in Fig. 7.7. The
graphs shows an increasing trend in wear loss of all synthesized composites with respect to
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increase in applied load. When the load increases, it has been found that the wearing of all the
hybrid composites increases slowly upto load 30 N, but when the load increases above this
value the slope of the wear loss rises by a great amount. This rise in the wear loss can be
attributed due large amount of plastic deformation and delamination occurred on the mating
surface. These results are in good agreement with the previous researchers findings [55,59,89].
It can be concluded form the graph that among all the applied loads and different
concentrations of graphite, Al+15%ZrO2+6%Gr hybrid composites displayed lowest wear
loss. But when the graphite concentration increases to 8 wt. % the wear loss increases sharply
because of reduced fracture toughness of hybrid composites.
19
Pure Al
17
Al+15%ZrO2
15 Al+15%ZrO2+2%Gr
Al+15%ZrO2+4%Gr
13
Wear loss (mg)
Al+15%ZrO2+6%Gr
11 Al+15%ZrO2+8%Gr
1
5 10 15 20 25 30 35 40 45
Applied load (N)
Figure 7.7 Influence of applied load on wear loss of hybrid composites.
The addition of graphite as a solid lubricants greatly affect the wear resistance of aluminium
matrix composites. Further, the literature reveals that addition of graphite reinforcement
enhances the wear resistance of composites due to the development of tribolayer. This
developed tribolayer remains stable upto a certain concentration of graphite. Further addition
of graphite diminishes the wear resistance shaply due to reduced hardness and fracture
toughness. The contributions of several researchers regarding the effect of particulate
reinforcement on the wear behaviour of the AMCs have been summarized below in Table 7.7.
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Methods of Parameters
Previous Works Material used Inferences
Basavarajappa et Al 2219/SiCp-Gr Hybrid liquid metallurgy Wear test.  Al/15SiCp/3Gr hybrid composite showed
al. (2006) [52] Composites technique superior wear behaviour.
 (0, 5 and 10 wt.%.)  Wear loss increases with sliding distance,
 Graphite (3 wt. %) applied load and sliding speed.
Radhika et al Al-Al2O3-Gr hybrid composites liquid metallurgy Wear test.  Aluminium alloy reinforced with 9 wt-%
(2013) [53]  3, 6 and 9 wt-% alumina. route alumina and 3 wt-% graphite has highest
 3 wt-% Graphite. wear resistance compared to unreinforced
alloy.
.
Ravindran et al. Al2024-SiC-Gr hybrid Powder metallurgy Wear test.  Hardness increases with increase in SiC
(2013) [54] composites. (845 MPa, 530 C contents.
 0, 5,10,15 and 20 wt.% for 60 min)  Addtion of graphite enhances the wear
SiC resistance of hybrid composites.
 5 wt.% graphite
Baradeswaran et Al7075/Al2O3/graphite hybrid Stir Casting Wear test.  Presence of graphite reduces the wear loss
al. (2014) [55] composites. due to development of tribolayer.
 2, 4, 6 and 8 wt.% of
Al2O3.
 5 wt.% graphite
Ravidran et al. Al 2024–5 wt% SiC–x wt% Powder metallurgy Wear test and  Composites with 5 wt% graphite showed
graphite (x=0, 5, and 10) hybrid (885 MPa and 530 Hardness the lowest wear loss.
(2013) [59] composites degree C)
Mahdavi et Al6061/SiC/Gr hybrid In situ Powder Wear test  The best wear resistance is achieved in
al.(2011) [92] composites. Metallurgy (IPM) the hybrid composite containing 20 vol.%
 0, 10, 20, 30, 40 vol% SiC, 9 SiC particles.
vol% Gr
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7.4.4 Analysis of variance (ANOVA)
The experiments were performed as per full factorial design of experiments and their
corresponding wear values have recorded in Table 7.5.
Table 7.8 Analysis of variance for the wear loss.
Source DF Seq SS Adj SS Adj MS F P Pr
Gr concentration (wt. %) 4 51.59 51.58 12.896 629.09 0.000 80.59
Sliding distance (m) 2 10.4007 10.4007 5.2003 253.67 0.000 16.25
Applied load (N) 1 1.3230 1.3230 1.3230 64.54 0.000 2.06

Gr concentration (wt. %)*
8 0.4227 0.4227 0.0528 2.58 0.101 0.6
Gr concentration (wt. %)*
4 0.0920 0.0920 0.0230 1.12 0.411 0.1
Applied load (N)
Sliding distance (m)*
2 0.0260 0.0260 0.0130 0.63 0.004 0.04
Applied load (N)
Error 8 0.1640 0.1640 0.0205 0.25
Total 29 64.0137
𝑅 − 𝑆𝑞 = 99.74% 𝑅 − 𝑆𝑞(𝑎𝑑𝑗) = 99.
Analysis of variance is a statistical tool which is used to find out the influence of independent
variables (Gr reinforcements, sliding distance and applied load) and their percentage
contributions on the experimental results (wear loss). ANOVA calculations were performed
using MINITAB-17 software. This analysis was undertaken for a level of significance of 5%.
Analysis of variance finds the F-ratio, which gives the level of significance of independent
variables by considering the variance of all terms included in the error term at the desired
significance level. Table 7.8 provides the ANOVA results for the wear loss of all the
composites. The percentage contribution of each independent factors are also incorporated in
the last column of Table 7.8. Table 7.8 clearly shows that concentration of graphite (80.59 %)
and sliding distance (16.25 %) has the highest contribution on the wear loss. While, the applied
load has only 2.06 % contribution to the wear loss which is relatively less. The contribution of
interaction between these parameters have further shown relatively less significance. However,
the greatest influence of interaction is graphite concentration and sliding distance which is only
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0.6 %, whereas the other interactions Gr concentration*applied load and sliding distance*
applied load are contributing only 0.1 and 0.04 % respectively. Therefore, the investigation
revealed that the selected independent variables (Graphite reinforcement, sliding distance and
applied load) and their respective interactions have statistical and physical significance on the
wear behaviour of fabricated hybrid composites.
The effect of each independent variables on wear behaviour can be analyzed with the help of
main effect plot and interaction plots. Fig. 7.8 is the main effect plot and is depicting the effect
of different process parameters on the wear loss. According to the theory if a line of any process
parameter in the main effect plot has a low variation with respect to the mean value, then it can
be interpreted that the given process parameter has no significant effect [58]. On the other
hand, plot of any process parameter having a higher slope with respect to the mean value
provides a significant effect. So, it is evident from the main effect plot that the Gr concentration
is the most influential parameter followed by sliding distance and applied load. The main effect
plot also confirms that as the concentration of Gr increases in aluminium composites its wear
resistance increases. Further, main effect plot depicts that the wear resistance of composite
increases drastically by the addition of graphite particles up to 6 wt. %. This enhancement in
the wear resistance can be attributed to the following reasons: (a) during sliding environment
graphite form a thin lubricating film, which prevents direct metal to metal contact [54,79,92],
(a) hardness imparted by nanoparticles to soft aluminium matrix [103], and (c) graphite
reduced the probability of thermal softening, which reduces the chance of interfacial debonding
of matrix and reinforcements. Further addition of graphite particles suddenly declines the wear
resistance of hybrid composites because of following reasons: (a) sudden decline in hardness
due to soft nature of graphite particles [79,92] and (b) increased reinforcement of graphite
reduces the fracture toughness of hybrid composites [54,58,79,92]. Additionally,
heterogeneous distribution and inefficient sintering process at high concentrations causes
severe material loss due to delamination [92].
The influence of sliding distance and applied load for all synthesized composites can be
inferred from interaction plot (Fig. 7.9). The interaction plot confirms that as sliding distance
increases the wear loss of all composites also increases which follows the trend proposed by
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Archard wear equation. Moreover, wear loss have a direct relation with sliding distance
because of following factors: (a) protective oxide layer becomes unstable with increment in
sliding distance [92,115] and (b) interfacial bonding of reinforcements and matrix becomes
weak due to thermal softening. However, the hybrid nanocomposites containing 6 wt. % of
graphite particles exhibits best wear resistance. With the help of interaction plot it can be
inferred that material loss due to wear is low at low applied load and vice-versa. The outcomes
are following the trends suggested by earlier literatures [54,103,124]. However, at high applied
load greater amount of frictional heat is developed which lowers the interfacial bond and
increases the chance of severe delamination [116]. Softened mating surfaces also enhances the
probability of penetration of asperities.
Main Effects Plot for Wear loss (mg)

Data Means
Gr concentration (wt.%) Sliding distance (m)
6
2
Mean
0 2 4 6 8 400 600 800

Applied load (N)
6
2
30 40
Figure 7.8 Main effect plot for independent variables on wear loss of Al-ZrO2-Gr hybrid
composites.
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Interaction Plot for Wear loss (mg)
Data Means
400 600 800
Gr concentration
6
(wt.%)
0
4 G r concentration (wt.% ) 2
4
6
2
8
6 Gr concentration
Sliding
distance
Sliding distance (m) 4
(m)
400
2 600
800
6
Sliding
Applied
4 Applied load (N) load (N)
30
2 40
Applied
0 2 4 6 8 30 40
Figure 7.9 Interactions of various independent variables on wear loss.
7.4.6 Investigation of wear mechanism by SEM
To analyze the wear mechanism, Scanning Electron Microscopy have been performed for all
synthesized hybrid composites and aluminium as displayed in Fig. 7.10(a-f). The worn surface
morph graphs of composites reinforced with zirconia particles and graphite particles exhibits
dissimilar wear profile when matched to unreinforced aluminium matrix. This verifies the
variation in wear mechanism. Large amount of craters, pits and grooves have been observed
on pure aluminium surface as shown in Fig. 7.10(a). Severe plastic deformation also occurs on
aluminium surface due to generation of frictional heat and hence escalated wear loss in
comparison to other hybrid composites [89]. Existence of severe delamination on worn surface
of pure aluminium is confirmed by SEM morph graphs.
The SEM of the Al+10%ZrO2 nanocomposites is having pits and grooves. The surface is also
showing presence of oxide layer which enhances the wear resistance of composite because
oxide layer is hard in nature. Further, rise in wear resistance is due to following factors: (a)
increased hardness imparted by zirconia nanoparticles, (b) plastic flow of the material during
sliding environment is restricted by nanoparticles [114], (c) ratio of hard to soft surface is
increased which supports the sliding load, and (d) reduction of adhesion of matrix material to
counter disc due to zirconia nanoparticles.
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Fig. 7.10(c-f) exhibit the worn morphologies of hybrid composites reinforced with graphite
particles. The surface of the graphite mixed hybrid composites are relatively smooth in nature
because of the presence of graphite reinforcements. The worn surface of Al+ZrO2+2%Gr (Fig.
7.10 c) hybrid composite is showing evidence of plastic deformation ploughing and smearing
which is causing greater amount of wear loss in comparison to the other two high graphite
reinforced hybrid composites. According to the previous literature, it has been studied that
small concentration of graphite shows little amount of solid-lubricant behaviour
[89][127][128].
The SEM of worn surface of Al+ZrO2+4%Gr is shown in Fig. 7.10(d), which is indicating
different wear pattern. From SEM morphology it can be concluded that the Al+ZrO2+4%Gr
hybrid composite is covered with black layer and groves are mostly restricted which are filled
with lubricating layer. The worn surface of Al+ZrO2+4%Gr is shown in Fig. 7.10(d) appears
to be having very small grooves due to the increased graphite content. The wearing pattern is
also very small in dimension at the sliding surface as the graphite content enhanced. As the
graphite concentration increases in case of Al+10%ZrO2+6%Gr (Fig. 7.11e) hybrid composites
more amount of graphite appears on the surface during sliding wear environment [127–129].
This releasing graphite content during sliding form a lubricating layer on the rubbing surface
and thus preventing direct contact between the pin and counter face.
Fig. 7.10 (f) shows the worn surface pattern of Al+10%ZrO2+8%Gr hybrid composites. The
SEM displays the indication of debonding/pullout of reinforcement from the matrix due to loss
in fracture toughness. Additionally, at high concentration of graphite agglomeration and
clustering cannot be avoided which hinders the effectiveness of sintering operation. Therefore,
the interfacial bonding between matrix/reinforcement is reduced and hence severe
delamination phenomena occurred during sliding environment. So, it can be concluded from
the whole SEM analysis of worn surfaces that appropriate amount of graphite plays a very
significant role in enhancing wear properties of hybrid composites.
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(a) (b)
Delamination and grooves
(c) (d)
ploughing and smearing
Shallower scratches
122 | P a g e
(e) (f)
Grooves are limited signifying
reduced wear loss Debonding/Pullout and
Severe delamination
Figure 7.10 SEM morph graphs of worn surface: (a) Pure aluminium, (b) 10 wt. % ZrO2, (c)
2 wt. % Gr, (d) 4 wt. % Gr, (e) 6 wt. % Gr and (f) 8 wt. % Gr reinforced Al composites.
7.4.7 Wear debris analysis
The mechanism of wear have been also studied by performing Scanning Electron Microscopy
of wear debris. The fragmented particles micrographs obtained from wear test for all fabricated
composites and pure aluminium are presented in Fig 7.11(a-f). Fig 7.11(a) exhibits the wear
debris of aluminium which is in the form of thin sheets/elongated debris. These
sheets/elongated debris are the clear indication of severe plastic deformation and determines
wear due to delamination. The wear debris of Al+10%ZrO2 composites is shown in Fig 7.11(b),
which contains particles with thin adhered fragments. Further, it is observed that average size
of debris obtained have reduced because of hard zirconia reinforcements. Fig. 7.11(c) depicts
the wear debris of 2 wt. % of graphite reinforced composites, contains the presence of thin
sheet of aluminium along with some loose particles. This confirms the material loss due to
abrasion because protecting graphite film is ineffective at lower concentrations. The wear
debris of Al+10%ZrO2+4% Gr hybrid composites is shown in Fig. 7.11(d). The collected wear
debris size have been reduced because of addition of graphite particles. Fig. 7.11(e) displays
the wear debris of hybrid composites containing 6 wt. % of graphite particles. This
micrographs indicates the clear sign that collected wear debris have become fine and uniform
is size. Further, decrease in debris size may due to following factors: (a) development of
protective lubricating graphite layer, and (b) thermal softening of mating surfaces have been
reduced due to reduced friction force.
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Fig. 7.11(f) shows the wear debris of hybrid composites containing highest amount of graphite
particles. SEM micrographs shows the evidence of large strip debris with irregular shape
because of severe delamination. Therefore, the investigation concludes that presence of
zirconia and graphite controls the size and morphology of wear debris.
The EDS of Al+10%ZrO2+6%Gr and Al+10%ZrO2+8%Gr hybrid composites wear debris
have been shown in Figs. 7.12(a-b). The high intensity of carbon and low intensity of Al
validates the severe smearing of graphite particles from the sample during sliding environment.
Further, peaks of iron (Fe) are also evident in both the EDS spectrum because hard zirconia
particles abrades the counter disc material. In both the EDS results, peak of oxygen is also
observed because of development of aluminium oxide and iron oxides due to combined effects
of frictional heat and environmental reactions [115].
(a) (b)
Elongated debris
Fine particles and thin fragments

sheets
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(c) (d)
Loose particles and Al sheets Fine abraded particles
(e) (f)
Uniform size debris
Severe
delamination
Figure 7.11 SEM morph graphs of wear debris: (a) Pure aluminium, (b) 10 wt. % ZrO2, (c) 2
wt. % Gr, (d) 4 wt. % Gr, (e) 6 wt. % Gr and (f) 8 wt. % Gr reinforced Al composites.
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(a) (b)
Figure 7.12 EDS spectrum of wear debris: (a) 6 wt. % Gr and (b) 8 wt. % Gr reinforced Al
hybrid composites.
7.4.8 Mathematical modelling and statistical analysis of models
Linear regression models were developed using a statistical software, MINTAB-17 for
predicting wear loss. The regression models describes the relationship between independent
variables and output value by fitting a linear and quadratic equations [58,62]. Previously
discussed, statistical analysis revealed that wear loss is dependent on following factors viz.
graphite reinforcement, sliding distance and applied load, which are independent variables.
Further, the standard Archard wear equation [52] suggests that the wear loss is directly
proportional to sliding distance and external load. However, it does not include the factors of
reinforced particles in any metal matrix composites. Additionally, interaction of these factors
are also difficult to calculate. To encounter such a complex tribological phenomenon, a number
of efforts have been directed to empirically model the wear behaviour in terms of independent
factors and their interactions [58,62]. Aligned with this, under the current approach, different
empirical correlations have been developed which highlight the significance of input variables
and their interactions on the wear behaviour of aluminium hybrid composites within the
considered range of interest. Further, only those factors and interactions are considered which
are significant on the basis of ANOVA analysis (as depicted in Table 7.7) namely, graphite
concentration, sliding distance, applied load and their interactions. The analysis comprises the
development of five different predictive models in which one was linear and four were
quadratic in nature.
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The models for prediction of wear loss is given below:
Model 1
𝑊𝑙𝑜𝑠𝑠 = 2.16333 − 0.4175 ∗ 𝐴 + 0.0036 ∗ 𝐵 + 0.042 ∗ 𝐶 [7.1]
Model 2
𝑊𝑙𝑜𝑠𝑠 = 2.58476 − 0.838929 ∗ 𝐴 + 0.0036 ∗ 𝐵 + 0.042 ∗ 𝐶 + 0.0526786 ∗ 𝐴 ∗ 𝐴 [7.2]
Model 3
𝑊𝑙𝑜𝑠𝑠 = 1.58 − 0.4175 ∗ 𝐴 + 0.0057 ∗ 𝐵 + 0.042 ∗ 𝐶 − 0.00000175 ∗ 𝐵 ∗ 𝐵 [7.3]
Model 4
𝑊𝑙𝑜𝑠𝑠 = 2.00143 − 0.838929 ∗ 𝐴 + 0.0057 ∗ 𝐵 + 0.042 ∗ 𝐶 + 0.0526786 ∗ 𝐴 ∗ 𝐴 −
0.00000175 ∗ 𝐵 ∗ 𝐵 [7.4]
Model 5
𝑊𝑙𝑜𝑠𝑠 = 2.47833 − 0.49625 ∗ 𝐴 + 0.003075 ∗ 𝐵 + 0.042 ∗ 𝐶 + 0.00013125 ∗ 𝐴 ∗ 𝐵 [7.5]
8
Experimental data
7 Predicted data (Model-2)
6 Predicted data (Model-5)
5
Wear loss (mg)
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
Experimetna trials
Figure 7.13 Estimated values of wear loss from all prediction models and experimental
readings.
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Using equations from (7.1-7.5), wear loss of all fabricated composites were estimated for all
30 set of experiments. The experimental wear loss and all models predicted values are plotted
in Fig. 7.13. The predicted wear loss form the model and experimental data are very close to
each other. Further, validation of predicted values and experimental values is shown in Fig.
7.14 by scatter diagram.
Figure 7.14 Scatter plot between experimental wear loss and estimated values from all
models.
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7.4.9 Statistical analysis of regression models
Five most commonly used statistical indicators were adopted to perform the statistical analysis
of developed regression models. The mathematical equations of these indicators are given
below:

1 m
i. MBE  [7.6]
m i 1
1/2
1 m 2

ii. RMSE    WLoss (i ,exp.)  WLoss (i ,mod el   [7.7]
 m i 1 
100 m WLoss (i ,exp.)  WLoss (i ,mod el )

iii. MAPE  |
m i 1 WLoss (i ,exp.)
| [7.8]

1 m
iv. MAE  [7.9]
m i 1
 W  WLoss ( i ,exp.) 
m
2
Loss ( i ,mod el )
v. R  1 i 1
[7.10]
 W  WLoss ( i , avg .) 
m
2
Loss ( i ,mod el )
i 1
The results of all statistical indicators [Eqs. (7.6) - (7.10)] of developed regression models have
been shown in Table 7.8. The significant value of each statistical indicators are marked bold
in the Table 7.8. The value of MBE lies in the range of -3.3333E-06 to 4E-07 which is showing
negative sign, which means the underestimation of data. However, the overall value of MBE
for all model are significantly small and close to zero. Finally, model 3 exhibits the significant
value of MBE (closest to zero). RMSE values of all models are found to be small having the
least value 0.473 for Model 4. The range of MAPE values were observed as 11.13 % to 15.67
% with Model 2 demonstrating the least value. Correlation Coefficient (R) of all models lies
in the range 0.9144-0.9669 which validates the good fitting of data. The highest value of R is
observed for Model 4. The values of MAE were found in the range from 0.3979 to 0.4351 with
least observed for Model 2.
Within each developed models, the MBE value of Model 3 is least. The coefficient of
determination of Model 4 is lowest, while RMSE, MAPE and MAE of Model 4, Model 2 and
Model 2 are lowest respectively among all developed regression analysis. This signifies the
satisfactory performance of all models as compared to the experimental data. However, which
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model is best among all is still not confirmed because all the statistical error is not going in
favor of one specific regression model. Due to this reason, in the next section the further
analysis of the developed models have been considered.
Table 7.9 Statistical indicators of developed regression models.
Model MBE RMSE MAPE R MAE

M1 -3.3333E-06 0.591 15.67 0.9144 0.4351
M2 -2.9333E-06 0.474 11.13 0.9668 0.3979
M3 3.10862E-16 0.590 13.52 0.9665 0.4290
M4 4E-07 0.473 11.16 0.9669 0.3995
M5 -3.3333E-06 0.588 13.72 0.9656 0.4351
7.4.10 Ranking of models by Global Performance Indicator (GPI)
It is interesting to see that all statistical indicator is showing different patterns and hence failing
to identify a best predictive model. Therefore, this difficulty is removed with further
improvement in the results of statistical analysis using Global performance indicator (GPI).
Global performance indicator is a useful technique developed by Despotovic et al. [125] that
accumulates the effect of all the individual statistical indicators. In this technique, all the
statistical indicators are scaled-down in such a way that all values lies between zero and one
[126]. The scaled-down values are then deducted from their corresponding medians,
respectively. Lastly, with the appropriate weight factors all the calculated values are added
together. The mathematical equation of GPI for ith model may be defined as:
5
GPI i    k ( yk  yik ) [7.11]
k 1
Where, 𝛼𝑘 equals to -1 for the indicator R only, however for remaining indicator its value is
recommended as 1. yk represents median of scaled values of indicator k, yik is scaled value of
indicator k for model i. The model completing the highest GPI value means more accurate
model.
The scaled value (between 0 and 1) of all statistical indicators along with their corresponding
GPI and subsequent ranking for all developed models are tabulated in Table 7.9. The GPI
values lies between -1.55 and 2.33. The maximum GPI is found to be 2.33 for Model 2, which
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consist of all independent terms viz. graphite concentrations, sliding distance and applied load
as was previously suggested by ANOVA analysis (as depicted in Table 7.7). Among all the
models, the top performer is Model 2. Therefore, this model can be used to estimate the wear
loss of aluminium matrix nanocomposites with high level of accuracy within the selected range
of investigations.
Table 7.10 Statistical indicator (Scaled), GPI and Ranking of the models.
Model MBE RMSE MAPE R MAE GPI Rank

M1 3.96E-11 1 1 0 1 -1.55 5
M2 0.10 0.0097 0 0.999 0 2.33 1
M3 0.89 0.9921 0.526 0.994 0.835 -0.80 4
M4 1 0 0.006 1 0.041 1.40 2
M5 0 0.9735 0.570 0.975 1 -0.12 3
7.5 Conclusions
In this work, graphite have been successfully reinforced in aluminium hybrid nanocomposites
using powder metallurgy technique. Further, full factorial design have been successfully
implemented and described to comprehend the wear behavior of aluminium hybrid
nanocomposites. The following major conclusions are described below:
i. The morphological study like XRD and EDS validated the presence of graphite and
zirconia in fabricated composites. Further, Elemental Mappings confirms the uniform
distribution of reinforced particles in aluminium matrix.
ii. The increase in sliding distance and applied load leads to an increase in the wear loss
of all fabricated samples. An addition of graphite to the composites reduces the wear
loss and it reaches to minimum at 6 wt. %. However, a further addition of graphite
particles to composite increases the wear loss.
iii. SEM investigation of worn surfaces and wear debris revealed that delamination and
abrasion are the major wear mechanism. Further, development of mechanically mixed
layer (MML) and graphite film at the mating surfaces are the predominant factors for
the enhancement in wear resistance as suggested by EDS analysis.
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iv. The most significant variables influencing the wear behavior (in terms of their
individual percentage contributions) were deduces based on ANOVA as graphite
concentration (80.59%), sliding distance (16.25%) and applied load (2.06%) within
the selected range of investigations.
v. Five different regression models were developed using MINITAB-17 software for
estimation of wear loss as a function of graphite concentration, sliding distance and
applied load.
vi. For models under consideration, the GPI was found in the range between -1.55 and
2.33. The GPI of model 2 was highest, hence the best model to estimate the wear loss.
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8. Micro and Nano Silicon Carbide Reinforced Aluminium Matrix
Composite Prepared By Conventional and Electric Resistance Sintering
Processes
8.1 Introduction
Metal matrix composites (MMCs) possess unique physical and mechanical behaviour over
conventional monolithic metallic alloys, required for automotive and aerospace industries
[61,63]. MMCs found wide usages in aerospace, automobiles, medical science and defense
sectors because of its remarkable physical, mechanical and wear behaviour. However, among
these available metal matrix composites, aluminium has got great engineering application in
automobile and aerospace industries due to its attracting features such as low density, improved
toughness, escalated mechanical behaviour and wear resistance [55][77].
Further, micro and nano-sized particles reinforced aluminium composites have been
increasingly used because of escalated mechanical and wear behaviour. Followings are the key
factors for the enhancement in properties: (a) micro particles supports the aluminium skeleton
thereby increasing hardness and wear resistance, (b) ductility and fracture toughness is
controlled by nanoparticles, (c) Orowan strengthening mechanism comes into play due to
uniformly dispersed nanoparticles, and (d) nanoparticles hinders dislocation movement and
develops fine grain microstructure. Therefore, synergistic improvement in mechanical and
wear behaviour can be obtained by the combined effect of micro and nanoparticles [7,112].
The distribution, orientation and fabrication techniques dictates the final properties of
aluminium matrix composites. To achieve the above said features many researcher attempted
different fabrication process viz. stir casting, compo-casting and powder metallurgy. Powder
metallurgy is the only process which gives the following key advantages that is difficult to
achieve by other processes such as: (a) uniform distribution of reinforcement in matrix, (b) low
processing temperature diminishes the probability of unwanted intermetallic reactions, and (c)
near net shaped product can be fabricated. Currently, SiC [103,121], Al2O3 [55], TiC [69] and
B4C [61] are extensively reinforced in aluminium matrix to improve wear and mechanical
properties. However, silicon carbide is most widely used ceramic due to small density
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difference with aluminium metal. Additionally, at low temperature, SiC does not react with
aluminium to develop unwanted intermetallic phase.
During sintering, heat energy is utilized to facilitate the sintering reactions like homogenization
of grain, mass transfer and fusion etc. These reactions particularly occur at particle surfaces of
powder component. Conventionally, sintering of powder component is done through tubular
furnace heating. In tubular furnace heating technique, surface of the component is heated first
followed by heat transfer to the core by mechanism of conduction and radiation. Therefore,
there exist a temperature gradient from surface to the core in the component. These temperature
gradient is significant when the size of the component is large [131]. High sintering time and
low heating rate in conventional sintering process also effect the mechanical and
microstructural properties of produced composites. Apart from that, in conventional sintering
process there is no any provision to apply external load at the time of heating. So, composites
fabricated through conventional sintering process possesses following drawbacks such as: (a)
coarse microstructure, (b) difficult to achieve dense structure, and (c) poor adhesion between
reinforcement and matrix. Additionally, greater amount of porosity due to pressure less
sintering leads to reduced mechanical and wear behavior, as porosity is considered as zero
mechanical strength. In order to overcome the above-mentioned drawbacks some fast non-
conventional sintering is required to achieve fully dense and controlled microstructure.
Recently, electric resistance sintering (ERS) of powder metallurgy metal composites is a novel
integrated manufacturing method in which heating of metal powder is done by passing an
electric current through the sample [132]. Essentially, the ERS entails the application of a low-
voltage and high intensity alternating current through a powder mass contained in an insulating
die, while pressure is simultaneously applied to the powder. Because the electrical
requirements of low-voltage and high-intensity current are perfectly satisfied by a resistance
welding equipment, this equipment can serve as the basis for the implementation of the ERS
technique. The typical duration of the ERS process is approximately 5 min. During this time,
the applied voltage and mechanical load induce powder densification due to softening. The
softening occurs as a result of the temperature increase that, in turn, is caused by the current
passing through the powders and the energy released by the Joule effect. Electric resistance
sintering has become popular due to its inherent advantages such as: (a) accelerated
densification, (b) controlled grain growth and uniform microstructure, and (c) high heating rate
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and shorter processing time [133,134]. Further, this process takes few minutes for sintering
therefore need of protective environment is eliminated. Hence, Electric resistance sintering is
a potential candidate for producing high wear resistance products due to time and energy
saving dimensions [17–19].
The rigorous literature survey reveals there is no literature is available on characterization and
wear behavior of micro and nano SiC reinforced aluminium composites fabricated through
electric resistance sintering methods. Hence, this investigation focusses the comparative study
of morphological and wear behaviour of composites fabricated through conventional and
electric resistance sintering methods.
8.2 Experimental
8.2.1 Sample preparation
Subsequent combination of samples, as given in Table 8.1, were synthesized through

conventional and electric resistance sintering process.
Table 8.1 Details of samples prepared.
S.No Conventional sintering Electric resistance sintering

1 Pure Al Pure Al
2 Al+10% SiCµm Al+10% SiCµm
3 Al+10% SiCµm+1%SiCnm Al+10% SiCµm+1%SiCnm
4 Al+10% SiCµm+3%SiCnm Al+10% SiCµm+3%SiCnm
8.2.2 Conventional sintering
The required amount of aluminium, SiCµm and SiCnm particles were measured accurately using
electronic balance (Precisa, ES 225SM-DR) of least count 0.01 mg. To get the homogeneous
mixture powders were mixed in centrifugal ball (FRITSCH, Germany) mill by maintaining
10:1 ball to powder ratio. Powders were mixed at 125 rpm for a time period of 20 minutes.
The thoroughly mixed powders were compacted, at 585 MPa pressure, in uniaxial hydraulic
press machine (Type KE, Sr. No. 1327, Kimaya Engineers, India). For the effective working
of die and punches externally solid lubricant (zinc stearate) was applied after each compaction
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step. Finally, to achieve the required strength the green samples were sintered at 450 0C in
electric tubular furnace for 1 hour [75]. During sintering inert environment were created by
argon gas (flow rate=1litre/min.) to protect the samples from oxidation. All samples were
made with fixed dimensions (8 mm diameter and 13 mm height) for further investigations.
8.2.3 Electric resistance sintering
The experimental setup used for electrical sintering process is shown in Fig. 8.2. initially,
green compact possesses large porosity and high electrical resistance and could not be sintered
by Electric resistance sintering (ERS) processes. Because, ERS process is based upon low
voltage and high intensity of current, and low voltage is unable to push the electron as a result
of that flow of current is restricted through the sample. So, before sintering the sample through
ERS process, mechanically interlocked powder compacts were pre-sintered at 2000C in a
tubular furnace for a predetermined period. After pre-sintering, porosity and resistance of the
green samples are slightly reduced and then the pre-sintered samples are held between copper
electrodes in an insulating die and current is allowed to flow through the sample while 2.55
MPa pressure is simultaneously applied to the sample which enhances the sintering reaction as
a result of that dense compact is obtained. Due to the flow of current, the temperature of sample
increases by Joule heating [135] when its surface temperature reaches at a 350℃ then further
increment in the current intensity is stopped and it is maintained for 5 minute. Now, the current
flow is stopped to avoid the further rise of temperature and the sample is allowed to cool to the
room temperature. A k-type digital thermocouple measuring probe was fixed on the samples
to read the temperature of pallets. The densities of samples prepared by both the technique
were calculated using Archimedes principle. The hardness of the respective samples were
calculated using digital Rockwell hardness apparatus (TRB-250 DM). Three indentations were
taken on each sample to get the actual hardness values. To identify the phases present in
fabricated composites X-ray diffraction (Bruker diffractometer system, (D8 ADVANCE-
40mA and 40kV) with Cu Kα radiation (wavelength = 1.5406 0A)) analyses were performed.
Morphological examinations of samples were performed using scanning electron microscope
(JOEL-JSM 6510 LV). The dry sliding wear test of the fabricated samples were performed
using a pin-on-disc wear tester (Ducom, Model No: TR-201 CL, Bangalore, India). The ASTM
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G99-95a (reapproved) standards were adopted to perform wear test. To remove the adhered
debris the disc and the specimens were cleaned with acetone after each wear test.
Figure 8.1 Electric resistance sintering setup.
8.2.4 Steps involved in fabrication of sample through electric resistance sintering process
Typical sequence involve in the fabrication of sample through electric resistance sintering
(ERS) process is shown in the Fig. 8.2. Where t1 represent the start of the cold-pressing period.
During this period no current passes through the powder and only pressure is applied. This
process is carried out in a manual hydraulic press. t2 represents the start of the presintering
period. During this period no pressure and current are applied and the sample is placed in a
tubular furnace at a predetermined temperature. Where t3 represent the start of the heating
period, during which both pressure and electrical current are applied to the sample. Where t4
represent the start of constant intensity of current through the sample. t5 represents the end of
the heating period and after that, the sample is allowed to cool itself to the room temperature.
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Figure 8.2 Typical sequence in an ERS process
8.3.1 Characterization of composites
Fig. 8.3 (a and b) displays the XRD pattern of composites prepared by both conventional
and electric resistance sintering technique. The XRD plot verifies that Al and SiC peaks are
present in all fabricated composites. From the graph it is also concluded that the aluminium
peak is the largest among the identified compounds. Further, diffraction peak of SiC increases
with the increase in SiC content in samples fabricated by both the techniques. The intensity
and sharpness of SiC is less in samples fabricated through electric resistance sintering process
because electric resistance sintering promotes fine grain structure. Additionally, electric
resistance sintering requires low sintering temperature and soaking time in comparison to
conventional sintering. Hence, bulk size nanocomposites can be fabricated without much grain
coarsening [136].
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(a)
(b)
Figure 8.3 XRD pattern of fabricated composites: (a) Conventional sintered samples and (b)
Electric resistance sintered samples.
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8.3.2 Scanning Electron Microscopy (SEM) of composites
The SEM of composites prepared by both the techniques are shown in Fig. 8.4(a-h). The fair
distribution of reinforcement in aluminium matrix is observed. However, in Fig. 8.4(e and g)
the clustering of silicon carbide is evident due to high concentrations of SiC nanoparticles. The
micrographs of samples fabricated through conventional sintering displays clear sign of pores
and improper interfacial bonding. The presence of porosity is attributed to the following
reasons: (a) slow heating rate, (b) long soaking time, and (c) pressure less sintering. However,
the composites fabricated through electric resistance sintering exhibit remarkable reduction in
porosity. Additionally, there composite exhibits improved interfacial bonding between
reinforcement and matrix. This reduction in porosity and improved interfacial bonding is due
to fast heating and cooling rate [137–139]. Further, low sintering temperature (350°C) have
not promoted the interfacial reaction between aluminium and SiC particles. The application of
external pressure and localized heating between contact surfaces of particle has led to a pore-
free microstructure.
(a) (b) Pores

SiC particles
140 | P a g e
(c) (d)
Coarse grain structure Poor interfacial bonding
(e) (f)
Pores
Proper interfacial bonding
(g) (h)
Clusters of particles
Fine grain structure
Figure 8.4 SEM micrographs of conventional (a, c, e and g) and electric resistance sintered
samples (b, d, f, and h).
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8.3.3 Porosity and Hardness measurement
Fig. 8.5 displays the percentage porosity of all composites fabricated by conventional and
electric resistance sintering process. There is a difference between the experimental density
and the theoretical density values for all samples. This indicates that porosity is present in the
fabricated composites. The bar graph shows that as the micro silicon carbide is added to the
composite the porosity increases sharply. It is observed that the Al+10 SiCµm fabricated by
conventional sintering technique composite exhibited a maximum porosity of∼3.75%. The
sudden rise in porosity is due to addition of hard ceramic particles which is difficult to deform
under compaction. The presence of porosity reduced the densification in sintered aluminium
composites. However, addition of nano silicon carbide reduced to available pores present
inside the matrix. The reduction in porosity is achieved because available micro pores are filled
up by nano particles [76]. In case of conventional sintering process, addition of 3% SiCn to
Al+10wt. % SiCm reduces pores from 3.75% to 2.9% which is about 17.14% reduction of
pores. Further, the porosity of electric resistance sintered samples are found to be low. Pure
Al fabricated through ERS process exhibited lowest porosity among all other fabricated
composites approximately of 0.9%. Al+10%SiCm+ 3%SiCn fabricated through conventional
and ERS sintering process have approximately of 2.60% and 1.40% porosity respectively
which is about 46.15% reduction of pores in ERS as compared to conventional sintering
process.. This change in microstructure and porosity is attributed to the different heating
mechanism and external pressure applied at the time of heating enhances the sintering reaction
at the contact surface of particles lead to reduction of pores. In electric resistance sintering the
heating of samples were achieved by Joule’s heating, which causes the sudden rise of
temperature at the particle surface. Therefore, localized heating takes place, which promotes
fast neck formation, hence reduced porosity in short interval of time [140].
142 | P a g e
4
Conventional Sintering
3.5 Non-conventional Sinterng
2.5
Porosity (%)
1.5
0.5
0
Pure Al Al+10%SiC Al+10%SiC+1%SiC Al+10%SiC+3%SiC
Figure 8.5 Porosity (percentage) of samples fabricated through conventional and electric
resistance sintering.
Fig. 8.6 shows the hardness of all composites fabricated by conventional and electric resistance
sintering process. The graph displays addition of silicon carbide enhance the hardness of
composites processed by both processes. Pure Al fabricated through conventional sintering
process exhibited lowest hardness among the fabricated composite is of 29 HR. Addition of
10%SiCm+3%SiCn to pure Al and fabricated through conventional sintering process increases
hardness value approximately 100% with respect to pure Al. The increase in hardness value
can be attributed to the: (a) presence of harder SiC reinforcement, (b) higher constraint to the
localized matrix deformation during indentation as a result of the presence of reinforcement,
(c) nano particles hinders the dislocation motion [6, 7].
This increase in trend was observed in ERS sintered composites from 31 to 66 HR for pure Al
matrix materials to 10%SiCm+3%SiCn reinforced composite, respectively.
Al+10%SiCm+3%SiCn fabricated through ERS process exhibited highest hardness value of
66 HR which is approximately 14.79% improvement in ERS as compared to conventional
sintered composite. Comparatively higher hardness values were obtained for the ERS sintered
samples as compared to the conventional sintered samples. Higher hardness of the ERS
sintered composites as compared to conventional sintered composites are attributed to the
143 | P a g e
following reasons: (a) development of fine grain structure, (b) fast heating and cooling rate,
(c) reduction in porosity, and (c) simultaneous heating and compaction of samples during the
process [140].
80
Conventional sintering Non-conventional sintering
70
Rockwell Hrdness
60
50
40
30
20
Figure 8.6 Rockwell hardness of samples fabricated through conventional and electric
8.3.4 Wear behaviour
Fig. 8.7 shows the comparison of conventional and electric resistance sintered samples wear
behaviour reinforced with micro and nano SiC to aluminium matrix. The bar graph verifies
that inclusion of silicon carbide drastically reduces the wear loss of composites for both the
processes. In case of conventional sintering process, addition of 10% micro size SiC to pure
Al shows drastic reduction of mass loss from 0.016 mg to 0.0075 mg which is about 53.13%
reduction in mass loss. The substantial enhancement in wear resistance is attributed to the high
hardness of silicon carbide particles. Further, addition of nano SiC reduces the wear loss due
to the following factors: (a) presence of nano SiC improved the hardness and reduced the
porosity [103], (b) during sliding environment, plastic flow is restricted by nano particles
[121], and (c) ratio of hard surface area to soft surface area is increased due to addition of
nanoparticles. Further, for all the combinations the samples prepared by electric resistance
sintering showed escalated wear resistance as compared to conventional sintered composites.
Al+10%SiCm+3%SiCn fabricated through ERS process shows lower mass loss of 0.004 mg
among all the fabricated composites which is about 20% reduction in mass loss as compared
to conventional sintered composite. This improvement is due to the following reasons: (a)
144 | P a g e
reduced porosity, (b) better interfacial bonding between reinforcement and matrix material and
(c) escalated hardness [103].
0.018
Conventional Sintering
0.016
Non-conventional sintering
0.014
0.012
Wear loss (g)
0.01
0.008
0.006
0.004
0.002
0
Figure 8.7 Wear behaviour of samples fabricated through conventional and electric
8.3.5 Analysis of Worn surface by SEM
The SEM micrographs of the worn surfaces of pure Al and synthesized composites processed
by both the techniques are given in Figs 8.8(a-f). It is perceived from micrographs, electrical
resistance sintered samples worn surface exhibits changed wear profile when compared with
conventionally sintered samples. Figs 8.8(a and c) shows the worn surface of conventionally
sintered samples indicating evidence of plastic deformation due generation of frictional heat..
Evidence of crater, pits and grooves were also found on pure aluminium worn surface due to
large wear loss [89]. Further, composite reinforced with both 10 wt. % micro and 1 wt. % nano
SiC particles showed reduction in plastic deformation phenomena due to hardness imparted by
ceramic particles. Fig 8.8(e and f) shows worn surfaces of composites, fabricated through
conventional and electric resistance sintering process, containing 3 wt. % of nano-SiC. The
worn surface of electric resistance sintered samples appears to be smooth and grooves are
mostly restricted representing high wear resistance and this should be ascribed to two reasons
- are reduced because of following causes: (a) due to homogeneous distribution of micro and
nano particles, (b) strong interfacial bonding between Al and SiC due to localized heating at
145 | P a g e
the contact surface of the particles (c) due to reduction in porosity, and (d) due to development
of fine grain structure [140].
(a) (b)
Pits and grooves
Delamination
(c) (d)
Shallower scratches
(e) (f)
Figure 8.8 SEM micrographs of worn surface of conventional (a, c and e) and electric
resistance (b, d and f) sintered samples.
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8.4 Conclusions
In the experimental work, micro and nano silicon carbide reinforced aluminium composites
were fabricated by both conventional and electric resistance sintering method. The important
conclusions are given below:
i. XRD analysis confirms the presence of silicon carbide particles in composites prepared
by both the techniques.
ii. Reduced porosity and escalated hardness were achieved by electric resistance sintering
technique.
iii. The electric resistance sintering samples exhibited enhanced wear properties in
comparision to conventioanlly sintered samples. The significant reduction in wear loss
of the composites are due to development of fine grain structure, reduced porosity and
strong interfacial bond between Al matrix and SiC reinforcement.
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9. Recommendations for Future Work
The future work for this study can be classified into the following research areas:
i. The similar study can be performed by channging the size and class of ceramic
particles.
ii. Impact of process parameters such as compaction pressure, sintering time and sintering
environment can also be included for futher study.
iii. Other mechanical properties such as compressive strength, tensile strength and impact
strenght can also be calculated for the developed aluminium composites.
iv. Investigation of corrosion behaviours of composites are also required for potential
engineering applications.
v. Friction and wear behaviour of composites can also be performed at high ambient
temperature inorder to check the potential of fabricated composites at high temperature
applications.
vi. The impact of current density, sintering time, sintering temperature and applied
pressure during flow of current can also be selected as process parametes.
vii. Other non-conventional sintering processes such as vacuum sinteing, microwave
sintering and spark plasma sintering can also be adopted for the comparative study of
sinteing technique.
148 | P a g e
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List of Publications
International Journal Articles

1. Sajjad Arif, Md Tanwir Alam, Akhter H Ansari, M Arif Siddiqui and Mohammad Mohsin
“Study of mechanical and tribological behaviour of Al/SiC/ZrO2 hybrid composites
fabricated through powder metallurgy technique”, Materials Research Express, Volume
4, Issue 7, July 17. (Science citation index. Impact factor 1.151)
2. Sajjad Arif, Md Tanwir Alam, Tariq Aziz and Akhter H Ansari “Morphological and Wear
behaviour of new Al-SiCmicro-SiCnano hybrid nanocomposites fabricated through powder
metallurgy”, Materials Research Express, Volume 5, Issue 4, April 27. (Science citation
index, Impact factor 1.151)
3. Sajjad Arif, Md. Tanwir Alam, Akhter Hussain Ansari, Mohd Bilal Naim Shaikh and M.
Arif Siddiqui “Analysis of tribological behaviour of zirconia reinforced Al-SiC hybrid
composites using statistical and artificial neural network technique” Materials Research
Express, Volume 5, Issue 4, May 2. (Science citation index, Impact factor 1.151)
4. Sajjad Arif , Bashrat Jamil, Akhter H. Ansari “Application of Full Factorial Design to
Study the Wear Behaviour of Aluminum Hybrid Nanocomposites”, Tribology -
Materials, Surfaces & Interfaces, Taylor and Francis (Under review, TRB599)
5. Sajjad Arif, Basharat Jamil, Tariq Aziz, Akhter H Ansari “Characterization of Surface
Morphology, Wear Performance and Modelling of Graphite Reinforced Aluminium
Hybrid Nanocomposites” Engineering Science and Technology, an International Journal.
Elseviers, (Ready for decision, JESTCH_2018_1849).
6. Sajjad Arif, Tariq Aziz, Akhter H Ansari “Micro and Nano Silicon Carbide Reinforced
Aluminium Matrix Composite Prepared By Conventional and Electric Resistance
Sintering Processes” Materials Focus, American Scientific Publisher. (Accepted)
Paper presented at conferences

 Sajjad Arif, Md Tanwir Alam, Akhter Husain Ansari, M Arif Siddiqui, Mohammad
Mohsin “Investigation of Mechanical and Morphology of Al-SiC composites processed
by PM Route” IOP Conference Series: Materials Science and Engineering, Volume 225,
conference 1.
162 | P a g e
Reprints of Published Papers
163 | P a g e

Experimental Investigation of Processes and Properties-Thesis

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Experimental Investigation of Processes and Properties-Thesis

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Experimental Investigation of Processes and Properties

of Aluminum Matrix Composites

Under the Supervision of

Akhtar Husain Ansari

Department of Mechanical Engineering

Date: (Signature of the candidate)

CERTIFICATE FROM THE SUPERVISOR

Signature of the Supervisor Signature of the Co-Supervisor

Name and Designation: Name and Designation:

(Signature of the Chairman of the Department with seal)

Date: (Signature of the Chairman of the Department with seal)

Title of the Thesis: Experimental Investigation of Processes and Properties of Aluminium

Candidate’s Name: Sajjad Arif

Signature of the candidate

CANDIDATE’S DECLARATION ......................................................................................... i

Figure 1.1 Schematic representation of the abrasive wear mechanism [24]............................. 9

Table 3.1 Details of reinforcement particles. .......................................................................... 33

1.1 Brief introduction

1.2.1 Aluminium matrix composites (AMCs)

1.2.2 Types of AMCs

 Particle-reinforced AMCs (PAMCs)

1.2.2.1 Particle-reinforced AMCs (PAMCs)

1.2.2.2 Whisker-or short fibre-reinforced AMCs (SFAMCs)

1.2.2.3 Continuous fibre-reinforced (CFAMCs)

1.2.2.4 Mono filament reinforced AMCs (MFAMCs)

1.3.1 Liquid state processing

1.3.1.1 Stir casting

1.3.1.2 Infiltration process

1.3.1.3 Spray deposition

1.3.2.1 Diffusion bonding

1.3.2.2 Physical vapour deposition

1.3.2.3 Powder metallurgy (PM)

1.4.1 Adhesive wear

Figure 1.1 Schematic representation of the abrasive wear mechanism [24].

1.4.2 Abrasive wear

1.4.3 Erosive wear

Figure 1.3 Schematic representation of the erosive wear mechanism[26].

1.4.4 Surface-fatigue wear

1.5 Need of reinforcements

1.5.1 Silicon carbide (SiC) as a reinforcement

1.5.3 Graphite as a reinforcement

In general, addition of graphite particles as reinforcement to an aluminum matrix enhances

1.6 Fabrication of aluminium matrix composites

Jiménez et al. [48] fabricated aluminium matrix-zirconia nanoparticles reinforced composites

1.7 Research gap related to aluminium matrix composites

Further, special attention is given to literature which emphasizes the enhancement of

1.8 Objectives of the research work

2.1.1 Aluminium Powder

Figure 2.1 SEM micrographs of as-received aluminium powders.

2.1.2 Silicon Carbide (Micro and Nanoparticles)

2.1.3 Zirconia nanoparticles (ZrO2)

Figure 2.3 SEM micrographs of as-received nano-zirconia (ZrO2) powders

2.1.4 Graphite particles

2.2 Experimental Set-up

2.2.1 Measurement and mixing of elemental powders

2.2.2 Compaction of elemental powders

(Powder Metallurgy Lab. Mechanical Engineering Department, AMU)

2.3 Morphological Characterizations

2.3.1 X-Ray Diffraction

Metallographic analysis is very important investigation step to correlate the microstructure of

Figure 2.9 X -ray Diffraction machine

2.4 Density measurement

2.5 Rockwell Hardness Measurement

PM Laboratory, MED Stress analysis and tribology laboratory, MED

Wear loss (g) = -3.50417 + 0.047Zirconia Concentration + 0.010Sliding Distance +