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Int. J. Surface Science and Engineering, Vol. 13, Nos.

2/3, 2019 133

Dry sliding friction and wear behaviour of developed


copper metal matrix hybrid composites

Manvandra Kumar Singh* and


Rakesh Kumar Gautam
Department of Mechanical Engineering,
Indian Institute of Technology (Banaras Hindu University),
Varanasi, 221005, India
Email: mksingh.rs.mec13@itbhu.ac.in
Email: manvandra.iitbhu@gmail.com
Email: rkg.mec@itbhu.ac.in
*Corresponding author

Abstract: In the present investigation, dry sliding friction and wear behaviour
of developed copper-based hybrid composites were studied. Tungsten carbide
(WC), zirconia (ZrO2), alumina (Al2O3) of grade A6 and chromium (Cr) hybrid
reinforcements were utilised to develop various copper-based hybrid
composites using liquid stir-casting technique. The developed hybrid
composites were characterised by X-rays diffraction (XRD), high-resolution
scanning electron microscope (HR-SEM), energy-dispersive analysis of X-rays
(EDAX), relative density and Vickers hardness. Developed hybrid composites
show improved Vickers hardness compared to its copper matrix while relative
density was found lower. Dry sliding friction and wear behaviour of the
developed hybrid composites were studied using pin-on-disc tribometer at
variable normal load, constant sliding speed and sliding distance. Hybrid
composites exhibited low wear compared to its copper matrix, particularly
(WC + Al2O3 + Cr) hybrid reinforced composites revealed better wear
resistance among all. Fluctuating nature of the coefficient of friction was
observed in all the materials. However, developed hybrid composites revealed
higher coefficient of friction compared with its matrix. The worn surfaces were
analysed using scanning electron microscopy (SEM), EDAX and optical
profilometer to discuss the friction and anti-wear mechanism involved in
developed materials.

Keywords: metal matrix hybrid composite; stir-casting; X-ray diffraction;


wear; worn surface; hardness; coefficient of friction; dry sliding; profilometer;
colour-mapping; surface roughness.

Reference to this paper should be made as follows: Singh, M.K. and


Gautam, R.K. (2019) ‘Dry sliding friction and wear behaviour of developed
copper metal matrix hybrid composites’, Int. J. Surface Science and
Engineering, Vol. 13, Nos. 2/3, pp.133–155.

Biographical notes: Manvandra Kumar Singh is an Assistant Professor in the


Department of Mechanical Engineering, Mewar University-Chittorgarh, India.
He received his BTech in Mechanical Engineering from the Uttar Pradesh
Technical University (U.P.T.U.) Lucknow, India in 2009. He completed his
MTech in Materials Science from the Indian Institute of Technology (Banaras
Hindu University) Varanasi, India, in 2011. He received his PhD in Mechanical
Engineering (Design) from the Indian Institute of Technology (Banaras Hindu

Copyright © 2019 Inderscience Enterprises Ltd.


134 M.K. Singh and R.K. Gautam

University) Varanasi, India in 2018. His areas of research interest include study
of microstructural, physical, mechanical and tribological behaviours of metal
matrix composite and hybrid composite materials and its development.

Rakesh Kumar Gautam is an Associate Professor of Mechanical Engineering in


the Indian Institute of Technology (Banaras Hindu University) Varanasi, India.
He completed his BE from the Madan Mohan Malviya Engineering College,
Gorakhpur in 1999, MTech from the Institute of Technology in 2001 presently
Indian Institute of Technology (BHU) Varanasi and PhD from the Indian
Institute of Technology in 2009, Roorkee. He is working in the area of
development of different types of composites, alloys and their physical,
mechanical, and tribological properties for various applications. He is also
working on synthesis of new bio-materials and exploring its tribological and
mechanical behaviors. He has published more than hundred national,
international journals and conference papers.

1 Introduction

The particulate metal-matrix composites are extensively used for tribological applications
due to excellent wear resistance especially during sliding. Low density, high strength and
their ability to carry higher loads give them a cutting edge over their counterparts
(Rajaram et al., 2010). Ceramic-reinforced copper matrix composites (CMCs) have
attracted much attention during recent years in industrial applications as bearing, bushes,
electrical sliding contacts, resistance welding electrodes, and antifriction materials (Fathy
et al., 2012; Rajkumar and Arvindan, 2011; Hirotaka et al., 2003; Chen et al., 2016).
Copper-based metal matrix composites are having high potential properties for such
application (Zhan et al., 2006). Further, hybrid composites show enhanced properties
compared to single reinforced composites as it combines the advantages of its constituent
reinforcements (Ramesh et al., 2009; Ahamed et al., 2009). Moreover, hybrid metal
matrix composites with two or more reinforcements have high degree of freedom in
materials design. This is due to tailorable coefficient of thermal expansion, better wear
resistance, self-lubrication, good impact strength and good mechanical behaviour at
higher temperatures. Currently, to enhance the wear resistance property, many hybrid
composites reinforced with hard ceramic particles like-SiC and Al2O3 are added as
reinforcements (Murthy et al., 2017). Therefore, more attention are being paid for the
development of hybrid metal matrix composites which are considered as a new
generation of composite materials and could potentially replace the composites with
mono reinforcements due to their improved physical and mechanical properties.
Furthermore, compared with a single enhancing phase, the combination of hybrid
reinforcements can be tailored to achieve an optimisation of material properties (Singh
and Chauhan, 2016; Alidokht et al., 2011; Alaneme and Olubambi, 2013; Show et al.,
2014; Tan et al., 2017). In metal matrix composites, where a high stiffness ceramic
reinforcement is embedded in a metallic matrix, the thermal mismatch between the high
expansion metallic matrix and the low expansion ceramic is typically quite high. Thus,
upon cooling, dislocations form at the reinforcement/matrix interface due to the thermal
mismatch. In this manner, thermally induced dislocations punching results in
strengthening of the metallic matrix (Chawla and Metzger, 1972; Chawla, 1973;
Vogelsang et al., 1986; Arsenault and Shi, 1986). Electrical sliding contact or bushes
Dry sliding friction and wear behaviour 135

material requires not only good electrical conductivity, high wear resistance and self
lubrication property but also high temperature strength properties (Keun et al., 2007). The
effectiveness of dispersed particles in matrix depends primarily on particle characteristics
such as size, distribution, spacing, thermodynamic stability, low solubility and diffusivity
of its constituent elements in the matrix (Nasiri et al., 2011; Groza and Gibeling, 1993;
Sauer et al., 1998). Various ceramic-reinforced composites such as SiC or Al2O3-copper
composites show the high heat, electrical conductivity, high toughness of copper to be
combined with the high stiffness and hardness of Al2O3 (Diemer et al. 1999; Winzer
et al., 2011; Park et al., 1999; Motta et al., 2001; Lee et al., 2001). The wear resistance
behaviour of the ceramic-reinforced copper metal matrix composites is also much better
(Tjong and Lau, 2000a, 2000b; Zhu et al., 2007a, 2007b).
The objective of the present investigation is to study the dry sliding friction and wear
behaviour of developed copper-based composite and hybrid composites using various
reinforcing particles such as WC, ZrO2, Al2O3 of grade A6 and Cr by using the liquid
stir-casting technique. Significant improved results are observed during the
characterisation and analysis of the developed copper-based metal matrix composite and
hybrid composites.

2 Experimental details

The stir-casting technique was utilised to develop the copper metal matrix composite and
hybrid composites. Commercial copper was taken as the matrix; however WC, ZrO2,
Al2O3 of grade A6 and Cr were taken as hybrid reinforcements according to weight
percentage as given in Table 1. Grade A6 of Al2O3 (purity~99.0%) is specifically chosen
because of its very good mechanical and electrical properties compared to its other
grading. To develop the copper-based composite and hybrid composites, small pieces of
commercial copper in appropriate amount were kept in a graphite crucible and then put
into an electrical muffle furnace. The furnace temperature was set to 1,200ºC whereas
heating rate and holding time of furnace were 300ºC/hr and 30 min, respectively. The
commercial copper completely converted into molten metal as furnace temperature
reached to its preset temperature of 1,200ºC. Thereafter, the reinforcements of WC, ZrO2,
Al2O3 (A6) and Cr were poured into molten metal simultaneously as per the
compositional details. These reinforcement particles were poured by wrapping in copper
foil, with the help of tong and continuously stirred for 5 min. After stirring, it was poured
into a permanent steel mould and kept in air for cooling and after cooling, the cast ingot
was ready for various characterisations. In metal matrix composites and hybrid
composites, there must be some bonding exist between the ceramic reinforcement and the
metal matrix for load transfer to occur from matrix to reinforcement. The two main
categories of bonding are mechanical and chemical. Here, during development of copper-
based metal matrix composite and hybrid composites using the stir-casting technique, the
reinforcement mechanism of ceramics in copper matrix is that the reinforcing particles
are mechanically bonded with the metal matrix instead of chemical bonding due to high
melting temperature of reinforcing particles. The interface between the reinforcement and
matrix is the key feature of the composite and hybrid composites that play a crucial role
in dictating the behaviours. Since, there is a large difference in coefficient of thermal
expansion between metal matrix and reinforcements that develop significant number of
136 M.K. Singh and R.K. Gautam

strain field or dislocation density around the reinforcing particles. Therefore, it can be
inferred that the same reinforcing mechanism would be involved during the
reinforcement of Al2O3 and ZrO2 in copper matrix with constant content of WC and Cr.
But, the Al2O3 reinforced hybrid composites will have the higher mechanical bonding
and strength due to larger strain around its interfaces compared with ZrO2 reinforced
hybrid composites. It is attributed to the rougher surface morphology of Al2O3 compared
to smooth and shiny surface of ZrO2, i.e., the rougher the interface, the stronger the
mechanical bonding (Chawla, 2012).
These developed materials were designated as Cu-1WC-2Cr (composite),
Cu-1WC-1ZrO2-2Cr [hybrid composite (HC)-1], Cu-1WC-1Al2O3-2Cr (HC-2),
Cu-1WC-2ZrO2-2Cr (HC-3), Cu-1WC-2Al2O3-2Cr (HC-4). Assay correction was done to
achieve the exact proportion of materials weight in the compositions to be developed.
100
Weight after assay correction ×wt. of materials taken (g)
purity of materials
Table 1 Compositional detail of the developed materials

Purity Weight Weight (g)


S. no. Developed materials Compositions
(%) (%) after assay
1 Pure copper Commercial copper (CC) 99.5 100.0 1,005.02
2 Cu-1WC-2Cr CC 99.5 97.0 974.87
(composite) WC 98.0 1.0 10.20
Cr 99.0 2.0 20.20
3 Cu-1WC-1ZrO2-2Cr CC 99.5 96.0 964.82
(HC-1) WC 98.0 1.0 10.20
ZrO2 99.5 1.0 10.05
Cr 99.0 2.0 20.20
4 Cu-1WC-1Al2O3-2Cr CC 99.5 96.0 964.82
(HC-2) WC 98.0 1.0 10.20
Al2O3 (A6) ~99.0 1.0 10.10
Cr 99.0 2.0 20.20
5 Cu-1WC-2ZrO2-2Cr CC 99.5 95.0 954.77
(HC-3) WC 98.0 1.0 10.20
ZrO2 99.5 2.0 20.10
Cr 99.0 2.0 20.20
6 Cu-1WC-2Al2O3-2Cr CC 99.5 95.0 954.77
(HC-4) WC 98.0 1.0 10.20
Al2O3 (A6) ~99.0 2.0 20.20
Cr 99.0 2.0 20.20

The X-ray machine was used to characterise the specimens. The XRD characterisation
utilised the specimens with dimension of 20 × 20 mm2 of pure copper, composite and
hybrid composites, from 10 to 100º of incident angles. Cu KD radiations were used in the
diffraction to observe the different phases involved in the materials. High-resolution
scanning electron microscope (HR-SEM) was also utilised to characterise the developed
Dry sliding friction and wear behaviour 137

materials. The scanning electron microscope (SEM) with energy dispersive analysis of
X-rays (EDAX) analysed the morphology of the reinforcing powders, its particles size
and the worn surfaces of the pure copper, composite and hybrid composites. Archimedes
principle was utilised to measure the experimental density of specimens. Theoretical
density of pure copper, composite and hybrid composites was calculated by using rule of
mixture (ROM). Relative density of materials was evaluated using the experimental and
theoretical density. Three tests were performed for each specimen to achieve
reproducibility of results of density. The Vickers hardness tester under the normal load of
100 g measured the hardness of the specimens for dwell time of 15 s. Ten indentations
were performed on each specimen for repeatability of hardness result and average value
was reported.
Dry sliding friction and wear test of pure copper, composite and hybrid composites
were studied as per the standard using pin-on-disc tribometer. Pins of pure copper,
composite, HC-1, HC-2, HC-3, and HC-4 having the dimension of diameter 8 mm and
height 30 mm were used as wear specimens. EN31 hardened steel disc of 60 ± 2 HRC
was used as rotating counter disc. The pin and disc surfaces were polished with the help
of emery papers with 1,200 and 1,600 grit size and followed by the acetone cleaning to
remove any possible traces of oil/grease and other surface contaminations. Wear pin was
properly placed in the pin holder so there could be proper normal contact of the pin with
counter disc. The test was performed for 60 min in the interval of 6 min, under normal
loads of 9.81, 19.62, 29.43, and 39.24 N at constant sliding speed of 2.43 m/s against the
rotating counter disc at 500 rpm. After each interval of 6 min the wear pin was weighted
and mounted again in the pin holder to precede the test. Same process was adopted for
each wear pin till accomplishment of test. In order to ascertain reproducibility of results,
each test was done for three times and average value was reported. SEM and optical
profilometer were used to observe the worn surfaces to understand the wear mechanism
and friction.

3 Results and discussion

3.1 Reinforcing particles analysis


Figures 1(a) to 1(d) show the morphology and EDAX spectrum of WC, Cr, ZrO2, and
Al2O3 of grade A6 reinforcing particles, respectively. Figure 1(a) shows uniform
spherical geometry of WC powder with particle size range of 5–15 µm. However, the
morphology of the Cr particles show resemble of fractured stone with particle size range
of 10–50 µm as shown in Figure 1(b). SEM morphology of ZrO2 powder shows shiny
and quite agglomerated particles with particle size range of 5–15 µm as shown in
Figure 1(c). Figure 1(d) shows the plate like morphology of the Al2O3 reinforcing
particles with a particle size range of 5–20 µm without any agglomeration. The
reinforcing powders have different shape, size and morphology that will play a vital role
to influence the mechanical and other properties of the developed materials. The
respective EDAX spectrum of the reinforcing particles shows the intensity peak of each
element, and present elements are categorised by their atomic and weight %. The EDAX
spectrum confirms the presence of each element in the respective reinforcing particles. It
was observed that the presence of elements with 24.63 wt % of carbon and 75.37 wt % of
tungsten, 11.05 wt % of carbon and 88.95 wt % of chromium in EDAX spectrum of WC
138 M.K. Singh and R.K. Gautam

and Cr, respectively. However, 31.20 wt % of oxygen, 68.80 wt % of zirconium and


50.09 wt % of oxygen, 49.91 wt % of aluminium are found in the EDAX spectrum of
ZrO2 and Al2O3, respectively.

Figure 1 SEM morphology and EDAX spectrum of reinforcing particles, (a) WC-particles
(b) Cr-particles (c) ZrO2-particles (d) Al2O3-particles (see online version for colours)

3.2 XRD analysis


Figure 2 shows the XRD pattern of the pure copper, composite and hybrid composites.
Here, the presence of strong intensity peak of only copper in XRD spectra of the pure
copper, composite and hybrid composites is observed while there is no significant
intensity peaks observed of the reinforcing materials such as WC, Cr, ZrO2 and Al2O3.
Dry sliding friction and wear behaviour 139

This can be attributed to the strong intensity peaks of copper (Zhang et al., 2016). The
absence of intensity peak of the reinforcing particles is attributed to the addition of low
weight percentage of the reinforcing materials with respect to its matrix weight
percentage (Gu et al., 2006). If a new phase or reaction is there with less than 5 % (wt/wt)
of reinforcement in the matrix, it is beyond the detection limit of X-rays diffraction
(Samal et al., 2013). However, the effect of ceramic reinforcement in copper matrix can
be observed in form of diffraction peak broadening and its intensity. They are different
from its matrix peaks intensity and broadening. The broadening of diffraction peaks are
featured due to the internal strain developed due to micro distortion of the lattice on
addition of ceramic reinforcement in copper matrix (Chen et al., 2018; Wang et al.,
2018). The details of peak broadening in form of full width at half maxima (FWHM) of
XRD peak of the materials is shown in Table 2. It shows that the FWHM of XRD peak of
composite and hybrid composites is higher compared to its matrix’s FWHM; it means
that the average crystallite size of composite materials decreases on addition of ceramic
particles into the copper matrix. Decrease in crystallite size of the composite and hybrid
composites plays a vital role on the strengthening of the materials. FWHM of the XRD
peak in HC-4 is highest among all the materials. Therefore, such variations in FWHM
make sure the effect of ceramic reinforcement in copper matrix. Kumar et al. (2017) have
made the similar study for X-ray diffraction pattern. In which, there was no phase
changes observed in XRD pattern but a little peak shift and broadening of Bragg
diffraction peak were observed. It was also observed that the average crystallite size
decreases as the Bragg peak broaden. Bagheri (2016) has also reported that copper with
different percentage of reinforcement shows the broader diffraction peak and their
decreased intensity of peak with increasing reinforcement in copper matrix. It is
attributed to the reduction in crystallite size and increase in internal strain of copper.

Figure 2 XRD pattern of pure copper, composite and hybrid composites (see online version
for colours)
140 M.K. Singh and R.K. Gautam

Table 2 Details of FWHM of pure copper, composite and hybrid composites including their
respective peak positions and diffraction planes

Peak FWHM FWHM FWHM FWHM FWHM FWHM


Diffraction
position (E-deg.) of (E-deg.) of (E-deg.) (E-deg.) (E-deg.) (E-deg.)
planes
(2θ-deg.) pure copper composite of HC-1 of HC-2 of HC-3 of HC-4
43.080 (111) 0.2302 0.2385 0.2492 0.2540 0.2565 0.2720
50.457 (200) 0.3373 0.3403 0.3537 0.3610 0.3643 0.3577
74.184 (220) 0.4632 0.4619 0.4558 0.4814 0.5039 0.4204
89.949 (311) 0.5965 0.6017 0.6140 0.6146 0.6697 0.7247
95.205 (222) 0.5780 0.5810 0.5877 0.6446 0.6730 0.8522

Figure 3 EDAX spectrum of, (a) pure copper (b) composite (c) HC-1 (d) HC-2 (e) HC-3
(f) HC-4 (see online version for colours)

Elements
Materials Totals
CK OK ZrL AIK CrK CuK WL
Pure copper Weight % ----- 0.12 ----- ----- ----- 99.88 ----- 100.00
Atomic % ----- 0.49 ----- ----- ----- 99.51 -----
Composite Weight % 14.56 2.49 ----- ----- 1.10 80.33 1.52
Atomic % 43.09 5.25 ----- ----- 0.17 51.09 0.40
HC-1 Weight % 3.31 1.57 1.10 ----- 1.27 88.95 3.80
Atomic % 15.06 5.37 0.56 ----- 0.78 77.10 1.13
HC-2 Weight % 1.73 1.03 ----- 1.04 1.03 94.80 0.37
Atomic % 8.04 0.12 ----- 0.28 0.33 91.11 0.12
HC-3 Weight % 4.22 1.40 2.23 ----- 1.04 90.84 0.27
Atomic % 18.29 4.55 0.33 ----- 0.24 76.41 0.18
HC-4 Weight % 4.50 2.84 ----- 3.14 2.03 86.21 1.28
Atomic % 27.06 2.21 ----- 1.21 1.52 67.44 0.56
Dry sliding friction and wear behaviour 141

3.3 EDAX and HR-SEM analysis


Figures 3(a) to 3(f) show the EDAX spectrum of the pure copper, composite, HC-1,
HC-2, HC-3 and HC-4, respectively. EDAX spectrum of the pure copper shows major
intensity peak of copper and very small intensity peak of oxygen with their weight and
atomic percentage as shown in table just below the spectrum. Presence of oxygen peak
intensity is relatively very small and that can be neglected with respect to copper intensity
peak. However, the EDAX spectrum of composite and hybrid composites shows the
intensity peak of entire reinforcing materials including copper matrix with their weight
and atomic percentage. The intensity peak of oxygen is also observed in EDAX spectrum
of composite and hybrid composites. This intensity peak of oxygen in EDAX spectrum is
attributed to the possible oxidation of materials at such higher temperature due to residual
oxygen in the furnace and addition of some oxygen element in form of ZrO2 and Al2O3.
The increasing weight and atomic percent of zirconium and aluminium element can be
observed in the EDAX spectrum of HC-3 and HC-4 from HC-1 and HC-2, respectively,
as the weight percentage of ZrO2 and Al2O3 increases from 1 wt % to 2 wt % in the
copper matrix.

Figure 4 HR-SEM micrograph with selected area for colour-mapping of, (a) pure copper
(b) composite (c) HC-3 (d) HC-4 and respective colour-mapping (a’)–(d’) with their
elemental colour-coding (see online version for colours)
142 M.K. Singh and R.K. Gautam

Figures 4(a) to 4(d) show the HR-SEM micrograph with selected area for its
colour-mapping of pure copper, composite, HC-3, and HC-4, respectively. The respective
colour-mapping of selected area with its elemental colour-coding of materials are
depicted in Figures 4(a’) to 4(d’). Colour-coding is reported in terms of percentage
according to the element volume percentage present in the respective colour mapping of
materials. The respective elemental colour-mapping is also shown in the Figure 4 just by
sides the respective colour-mapping of materials. This analysis indicates that the
developed composite and hybrid composites materials contain their reinforcing materials.

3.4 Relative density and porosity


Table 3 shows the variation of relative density and porosity of pure copper, composite,
and hybrid composites. It has been observed that relative density of the composite and
hybrid composite materials is lower than that of the pure copper. It is attributed to the
reinforcement of lower density ceramics and their different crystal geometry into the
copper matrix (Fathy et al., 2012). In addition to this, the variation in crystal geometry of
reinforcement particles from the matrix possibly hindered the crystal arrangement of
composite and hybrid composite materials during solidification and develops some
possible defects such as micro voids, internal strain and porosity. In case of HC-2 and
HC-4, the addition of hexagonal structure of WC and trigonal structure of Al2O3
reinforcements in face-centred cubic structure of copper matrix, due to this dissimilar
crystal geometry, atoms will not be arrange in a systematic manner during solidification,
so it will always be settled with the above mention defects (Callister, 2007). The similar
phenomenon is also possible in case of HC-1 and HC-3 in which monoclinic structure of
ZrO2 and hexagonal structure of WC are reinforced in face-centred cubic structure of
copper matrix. However, there is some increment in relative density observed in case of
HC-2 and HC-4 compared with HC-3 and HC-4. It is attributed to the quite homogeneity
in the crystal geometry of the WC and Al2O3 which makes a better arrangement of atoms
in the matrix while solidification, and develop less voids and porosity in the materials.
Table 3 Variation of relative density, porosity and Vickers hardness of the pure copper,
composite and hybrid composites

S. no. Developed materials Relative density (%) Porosity (%) Vickers hardness (HV)
1 Pure copper 95 ± 0.25 5.0 82 ± 4
2 Composite 93 ± 0.15 7.0 112 ± 6
3 HC-1 87 ± 0.2 13.0 122 ± 5
4 HC-2 88 ± 0.15 12.0 135 ± 8
5 HC-3 86 ± 0.3 14.0 127 ± 5
6 HC-4 91 ± 0.25 9.0 155 ± 8

3.5 Vickers hardness


Table 3 shows the variation of the Vickers hardness of pure copper, composite and hybrid
composites. Composite and hybrid composites exhibit the higher hardness compared with
pure copper. It is also observed that hardness of the developed copper hybrid materials
increases with increase in wt % of reinforcement. This increased hardness is attributed to
Dry sliding friction and wear behaviour 143

the addition of harder ceramic materials in copper matrix, their presence leads to a higher
hardness of the composites (Samal et al., 2013). By increasing of the Al2O3 reinforcement
from 0 to 2 wt % with same amount of WC and Cr the hardness increased from 112 to
~155 HV. However, with increasing of ZrO2 from 0 to 2 wt % with same amount of WC
and Cr the hardness increased from 112 to ~127 HV (Rajmohan et al., 2013). Such
improvement in hardness of the developed hybrid composites may be attributed to the
high interfacial bonding strength at matrix and reinforcement and homogeneous
distribution of reinforcement within matrix which restrict the grain growth (Rahimian
et al., 2011; Singh and Gautam, 2017). The advancement in hardness of composite and
hybrid composites may also be possible by dislocations locking mechanism due to the
significant atomic size mismatch of reinforcing particles and copper, possible segregation
of reinforcing atom in stacking faults of copper may be another reason of hardness
improvement (Bagheri, 2016).

Figure 5 Variation of the cumulative volume loss with sliding distance of materials at constant
sliding speed of 2.43 m/s at, (a) 9.81 N (b) 19.62 N (c) 29.43 N (d) 39.24 N
(see online version for colours)

(a) (b)

(c) (b)

3.6 Dry sliding wear


Figures 5(a) to 5(d) show the variation of the cumulative volume loss with sliding
distance of materials at constant sliding speed of 2.43 m/s and normal loads of 9.81,
144 M.K. Singh and R.K. Gautam

19.62, 29.43, and 39.24 N. Cumulative volume loss increases as the sliding distance
increases in all cases of materials investigated (Janbozorgi et al., 2017). This is attributed
to the increase in contact area between wear pin and counter EN31 steel disc due to the
combination of different wear mechanism involved. Therefore, the temperature of the
contacting surfaces increases as the sliding distance increases due to increasing asperity
contacts (Anil et al., 2017). An increase in temperature of the wear pin surface can also
be a factor of more volume loss. Due to this increase in temperature the surface of wear
pin gets soften which leads to high surface and subsurface damage leading to high
volume loss (Rajkumar and Arvindan, 2011). From the Figure 5, it is observed that the
cumulative volume loss with sliding distance of the composite and hybrid composites is
comparatively lower than pure copper, which is attributed to the reinforcement of harder
ceramic materials; these hard ceramics particles resist the further wear of the composite
materials due to its strengthening effects (Silva et al., 2016). Al2O3 reinforced copper
hybrid composite, i.e., HC-2 and HC-4 have low cumulative volume loss with sliding
distance. It is attributed to the high hardness of the materials that obey the Archard’s law
of wear. Figure 5 also shows the decrease in cumulative volume loss with increasing
content of reinforcement from 1 wt % to 2 wt % of ZrO2/Al2O3 for the same sliding
distance and they follow the almost linear relation with the sliding distance (Kanagaraj
et al., 2010).

Figure 6 Variation of the wear rate with normal load of materials at constant sliding speed of
2.43 m/s for sliding distance of ~9,000 m (see online version for colours)

Figure 6 shows the variation of the wear rate with normal load of materials at constant
sliding speed of 2.43 m/s and for sliding distance of ~9,000 m. It is observed that the
wear rate increases as the normal load increases from 9.81 to 39.24 N for all materials
investigated (Walid et al., 2009; Zhan and Zhou, 2005; Zhan et al., 2004). The extent of
plastic deformation is high at higher normal loads which promotes higher wear rates in all
samples. The pure copper shows the fastest increase in wear rate as compared with
composite and hybrid composites. There are possible reasons for high wear rate in pure
Dry sliding friction and wear behaviour 145

copper first, due to its lower micro hardness compared with composite and hybrid
composites that lead to high wear rate which is motivated by the delamination
phenomenon. Second, high wear rate in pure copper can be attributed to the formation of
oxide layer when the temperature increases due to high friction at higher normal load,
and the developed oxide layer gets fractured and remove the materials in greater extent.
Whereas, in case of composite and hybrid composites the wear rate increases as the load
increases that is attributed to the load effect on the wear pin, i.e., the depth of penetration
of the harder ceramic reinforcements in the soft matrix increases as the normal load
increases, and it is also motivated by increase in the temperature of the pin surface. The
increase in temperature makes the matrix surface more ductile so penetrations are highly
envisaged. Therefore, harder ceramic like – WC, Al2O3 and ZrO2 push back into the
matrix and starts wear of matrix materials in form of plastic deformation of sub surfaces
by the hard counter disc surface. However, it is observed that the composite and hybrid
composites have low wear rate compared with pure copper, this is attributed to the
improved hardness of the composite and hybrid composites due to the harder ceramics
addition, which follows the Archard’s law of wear (Tjong and Lau, 2000a, 2000b). In
addition to this, the harder ceramic reinforcements render remarkable resistance to plastic
deformation and reduce the adhesion between the composite/hybrid composites pin and
counter steel disc. Apart from this, the ceramic reinforcements act as load bearing
components in the composite and hybrid composites which significantly reduces the
contact area between copper matrix and counter steel disc. Therefore, with the reduced
contact area, the deterioration of pin is less (Mallikarjuna et al., 2017).

3.7 Dry sliding friction


Figures 7(a) to 7(d) show the variation of the coefficient of friction with sliding distance
of pure copper, composite and hybrid composites at constant normal loads of 9.81, 19.62,
29.43, and 39.24 N, sliding speed of 2.43 m/s. The behaviour of coefficient of friction
with sliding distance is fluctuating in nature. It has been observed that at low loads such
as 9.81 and 19.62 N the fluctuating range varies from 0.4 to 0.97. The least coefficient of
friction is observed for pure copper and most for HC-4. In case of higher loads, the
fluctuating range of coefficient of friction is from 0.55 to 0.9 and it can be attributed to
the better asperity contact between surfaces of counter disc and wear pin. Overall, pure
copper shows lower coefficient of friction compared with composite and hybrid
composite materials.
Figure 8 shows the variation of average coefficient of friction with normal load of
pure copper, composite and hybrid composites for sliding distance of ~9,000 m at
constant sliding speed of 2.43 m/s. It is observed that the coefficient of friction of pure
copper, composite and hybrid composites decreases as the normal load increases.
However, it is observed that the coefficient of friction increases up to normal load of
19.62 N in all the materials investigated. In case of unreinforced copper, increase in
coefficient of friction is attributed to the formation of oxide layer of copper that is harder
than copper. This harder oxide layer offers high coefficient of friction with hard counter
surface; however as the normal load increases beyond the 19.62 N the developed oxide
layer get fractured due to high normal load and remove easily from the pin surface. In
addition to this, on application of high normal load that increases the contact area
between pin and counter disc surface which may raise the contact temperature and it
146 M.K. Singh and R.K. Gautam

soften the pin surface. Thus the pin surface tends to slip during high loads thereby
reducing the coefficient of friction in all case of materials (Rao et al., 2009;
Lakshmipathy and Kulendran, 2014). Further, in case of composite and hybrid
composites the coefficient of friction increases due to the early exposure of the harder
ceramic particles and come into contact with the counter surface resulting in increase of
coefficient of friction up to normal load of 19.62 N. However, it decreases beyond
normal load of 19.62 N. It can be attributed to the wear debris and pull out reinforced
particles from the pin surface which entrap in between the pin and counter surface and
start acting as roller or solid lubricating agent that reduces the coefficient of friction (Jha
et al., 2017).

Figure 7 Variation of the coefficient of friction with sliding distance of materials at constant
sliding speed of 2.43 m/s and at, (a) 9.81 N (b) 19.62 N (c) 29.43 N (d) 39.24 N
(see online version for colours)

(a) (b)

(c) (d)

3.8 Worn surface analysis and wear mechanism


Figures 9(a) to 9(f) show the typical SEM micrograph of the worn surface of pure copper,
composite, HC-1, HC-2, HC-3 and HC-4 at constant normal load of 39.24 N and sliding
speed of 2.43 m/s for the sliding distance of ~9,000 m. In contrast, the morphology of the
worn surface of the composite and hybrid composites is significantly different from the
worn surface of pure copper. Figure 9(a) shows the severe plastic deformation and
Dry sliding friction and wear behaviour 147

ploughing in worn surface of pure copper. The formation of grooves on the worn surface
of pure copper may be attributed to formation of copper oxide. EDAX investigation on
worn surface of copper displays the oxygen peak which confirms the formation of copper
oxide as shown in Figure 10(a). During the dry sliding test, the temperature rise due to
frictional heating between pin and counter disc may led to reaction between copper and
atmospheric oxygen developing copper oxides. The developed copper oxides are hard in
nature get embedded in the debris and account for ploughing of pin surface in the form of
grooves (Mallikarjuna et al., 2017). It is observed that the morphology of worn surface of
composite and hybrid composites is smoother as compared with worn surface of pure
copper. It is attributed to the harder ceramics reinforcement which improves the wear
resistance against dry sliding by restricting the deformation of the copper matrix. It is due
to the improved hardness of composite and hybrid composites results in significant
reduction in the localised plastic deformation of the pin surfaces (Rajkumar and
Arvindan, 2011) that can be observed in the SEM micrographs of worn surface of
composite and hybrid composites. The delamination, mechanical mixed layer (MML),
narrow grooves, wear debris and micro cracks are observed in the worn surfaces of the
materials, due to different wear mechanism involved during dry sliding as shown in
Figure 9. The grooves are found on the worn surfaces that are attributed to the ploughing
through hard asperities of counter steel surface or ploughing through detached harder
ceramic particles from pin surface (Li et al., 2015).

Figure 8 Variation of average coefficient of friction with normal load at constant sliding speed of
2.43 m/s for sliding distance of ~9,000 m (see online version for colours)

Figures 10(a) to 10(f) show the EDAX spectrum of the worn surface of the pure copper,
composite, HC-1, HC-2, HC-3, and HC-4, respectively. This investigation is conducted
on worn surfaces of the materials to understand the wear mechanisms which govern the
tribological behaviours of pure copper and other developed materials. It is observed that
the presence of small intensity peak of the oxygen in the entire EDAX spectrum, its
weight and atomic percentage are given in the table just below the spectrums. It indicates
148 M.K. Singh and R.K. Gautam

that the oxide layer has been developed on the worn surfaces of developed materials
during the dry sliding. It may be attributed to the increase in the temperature of the
surfaces during sliding against the hard steel counter surface; such increase in
temperature is prone to oxidation (Rajkumar and Arvindan, 2011). The small intensity
peak of iron is also observed in all the EDAX spectrum of composite and hybrid
composites, their weight and atomic percentage are reported in the table just below the
spectrum. It can be attributed to the harder ceramic reinforcements in composite and
hybrid composites, which abrade some amount of materials from the hard steel counter
surface after long sliding distance and get stick with the pin surface of composite and
hybrid composites. The presence of iron and oxygen intensity peak in the spectrum also
indicates that the mechanically mixed layer has been developed on the worn surface of
the materials (Janbozorgi et al., 2017). Therefore, the investigation of worn surface of all
materials suggest the wear mechanism involved in pure copper is quite seizing and
oxidative wear proceeded by the delamination of subsurface layers develop the severe
worn surface. However, the oxidative and abrasive wear is mainly involved in case of
composite and hybrid composites without any seizing wear.

Figure 9 SEM morphology of the worn surface at constant sliding speed of 2.43 m/s and normal
load of 39.24 N for sliding distance of ~9,000 m (see online version for colours)

(a) (b)

(c) (d)
Dry sliding friction and wear behaviour 149

Figure 9 SEM morphology of the worn surface at constant sliding speed of 2.43 m/s and normal
load of 39.24 N for sliding distance of ~9,000 m (continued) (see online version
for colours)

(e) (f)

Figure 10 EDAX spectrum of the worn surface of developed materials at constant sliding speed
of 2.43 m/s and normal load of 39.24 N for sliding distance of ~9,000 m
(see online version for colours)
150 M.K. Singh and R.K. Gautam

Figure 10 EDAX spectrum of the worn surface of developed materials at constant sliding speed
of 2.43 m/s and normal load of 39.24 N for sliding distance of ~9,000 m (continued)
(see online version for colours)

Elements
Materials Totals
CK OK ZrL AIK FeK CrK CuK WL
Pure Weight % ----- 10.67 ----- ----- ----- ----- 89.33 ----- 100.00
copper Atomic % ----- 32.18 ----- ----- ----- ----- 67.82 -----
Composite Weight % 18.20 7.98 ----- ----- 1.56 0.14 71.71 0.42
Atomic % 47.72 15.70 ----- ----- 0.88 0.08 35.54 0.07
HC-1 Weight % ----- 10.02 0.12 ----- 0.97 ----- 86.77 2.12
Atomic % ----- 30.97 0.06 ----- 0.86 ----- 67.54 0.57
HC-2 Weight % 19.48 16.09 ----- 0.54 47.66 0.67 15.17 0.40
Atomic % 43.20 26.78 ----- 0.53 22.73 0.34 6.36 0.06
HC-3 Weight % ----- 16.87 ----- ----- 45.32 0.90 36.75 0.16
Atomic % ----- 42.82 ----- ----- 32.95 0.70 23.49 0.04
HC-4 Weight % 17.70 9.42 ----- 0.47 0.90 0.01 71.07 0.43
Atomic % 45.81 18.30 ----- 0.54 0.50 0.01 34.7 0.07

Figure 11 3D profile and surface roughness profile of the worn surface of developed materials
for sliding distance of ~9,000 m at constant normal load of 39.24 N
(see online version for colours)
Dry sliding friction and wear behaviour 151

Figure 11 3D profile and surface roughness profile of the worn surface of developed materials
for sliding distance of ~9,000 m at constant normal load of 39.24 N (continued)
(see online version for colours)

3.9 Worn surface analysis using profilometer


Figures 11(a) to 11(f) and 11(a’) to 11(f’) show the 3D profile of the worn surface of the
pure copper, composite, HC-1, HC-2, HC-3, and HC-4 with their respective surface
roughness profiles for sliding distance of ~9,000 m at constant sliding speed of 2.43 m/s
and normal load of 39.24 N. 3D profiles of worn surfaces show the peak height and depth
of valley with different colours. Here, it is observed that roughness peak heights shown
with blue and valley depth with dark yellow, respectively. The roughness values (Ra and
Rq) of worn surfaces are reported in the roughness profile of the respective materials. The
surface roughness of pure copper is highest among all materials investigated. This is
attributed to the high delamination of subsurface of copper pin on high normal load and
the plastic flow of subsurface are also taking place due to increase in temperature.
Moreover, due to increase in temperature oxidative layer forms and fracture occurs
unevenly at high normal load, which left some severe surface morphology behind it as
shown in Figure 11(a). However, the HC-4 shows the least surface roughness (Ra and Rq)
among all the materials. It is attributed to the least wear of pin surface due to its highest
hardness so its worn surface is much smoother comparative to others as shown in
Figure 11(f) (Gautam et al., 2016; Petrica et al., 2017).
152 M.K. Singh and R.K. Gautam

4 Conclusions

From the present investigation, the following conclusions can be drawn:


1 The copper-based metal matrix composite and hybrid composites can be successfully
developed by conventional and cost effective liquid stir-casting technique.
2 The composite and hybrid composites show the lower relative density compared with
pure copper due to the reinforcement of lower dense ceramic materials into the
matrix and presence of some voids and porosity.
3 Vickers hardness of the composite and hybrid composites is higher than pure copper.
It increases as the weight percentage of reinforcement increases. HC-4 shows
optimum result among all investigated materials.
4 The dry sliding wear resistance of the composite and hybrid composites is much
better than pure copper. HC-4 shows optimum wear resistance among all materials
investigated.
5 The behaviour of coefficient of friction with sliding distance and normal load show
the fluctuating nature in all the cases. Nevertheless, the hybrid composite materials
show the higher coefficient of friction and low wear compared with pure copper that
is demanding property of a good friction material.
6 Quite seizing, abrasive and delamination wear mechanisms are mainly involved
during dry sliding of pure copper. However, the oxidative and abrasive wear is
mainly involved during dry sliding of composite and hybrid composites without any
seizing wear.
7 Worn surface of pure copper shows higher roughness (Rq = 2.6 µm) compared with
worn surfaces of composite and hybrid composites. Worn surface of HC-4 shows the
least roughness (Rq = 0.12 µm) that is expected due to its low wear.

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