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A statistical prediction on wear and friction behavior of ZrC nano particles

reinforced with Al - Si composites using full factorial design

Article · March 2018

DOI: 10.1016/j.surfin.2018.01.003

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 Surfaces and Interfaces 10 (2018) 149–161

Contents lists available at ScienceDirect

Surfaces and Interfaces

journal homepage: www.elsevier.com/locate/surfin

A statistical prediction on wear and friction behavior of ZrC nano particles T

reinforced with AleSi composites using full factorial design
⁎
A. Haiter Lenina, , S.C. Vettivelb, T. Rajaa, Lulseged Belaya, S. Christopher Ezhil Singhc
a
Department of Mechanical Engineering, Kombolcha Institute of Technology, Wollo University, Kombolcha 208, Ethiopia
b
Department of Mechanical Engineering, Chandigarh College of Engineering and Technology (Degree Wing), Chandigarh, 160019, India
c
Department of Mechanical Engineering, Bethlahem Institute of Engineering, Kanyakumari, Tamilnadu, India

A R T I C L E I N F O A B S T R A C T

Keywords: This paper investigates the dry sliding wear and friction behavior of pure Aluminium (Al), Ale12 Si with its
AleSi-xZrC reinforcement ZrC in various weight percentages. The samples were prepared by Powder Metallurgy method.
Wear The wear test was conducted using the pin-on-disc, with the varying the parameters of normal load (10–40 N),
Coefficient of friction sliding distance (500–2000 m) and constant sliding velocity of 2.618 m/s. The ZrC reinforced specimens showed
Full factorial design
the lower coefficient of friction and maximum wear resistance. The influence and percentage contribution of
Powder metallurgy
variable parameters were analyzed using Minitab 17.3.1 software. The wear worn surface of the hybrid com-
posites was analyzed using Scanning Electron Microscope and reveals that Ale12Si shows fracture and deformed
whereas Ale12Sie15ZrC consists of fine and coarse powders with uniform distribution and there is very less
wear debris are seen. Ale12Sie15ZrC shows reduced coefficient of friction and specific wear rate while the load
and sliding distances increases with increase in wt.% of carbide reinforcement.

1. Introduction
Today's scientific research concentrates on Aluminium (Al) alloys
due to their high specific strength and stiffness for automobile and
aerospace applications. The hybrid composite plays vital role in en-
hancing the mechanical properties and also reduction in fuel con-
sumption [1]. Large number of studies was much attentive in this Al
based composites due to its low density, wear resistance and good high
temperature properties [2].
Aluminium with Si is the major alloying element which forms a
class of material providing the most significant part of all manu-
facturing materials. It has a wide range of applications in the auto-
motive and aerospace industries due to an excellent combination of
castability and mechanical properties, as well as good corrosion re-
sistance and wear resistivity. Also Al–Si is the predominant material
due to their low weight, good wettability, low cost and favourable
mechanical properties [3]. Han et al. investigated that the finer grains
were lead to an increase in hardness and reduced wear rate [4].
AleMgeSi alloy based matrix composite materials prepared by stir
casting method have proved as comparable strength and improved
fracture toughness [5]. MichaelRajan et al. proved the Al reinforced
TiB2 particulate composites have high wear resistance behaviour at
constant temperature and at high temperature shows wear at the worn
surface [6]. The technical issues are overcome by adding carbide, an
ultra-hard material as reinforcement phase resulted in higher com-
pressive strength with increase in weight fractions [7]. Graphite hybrid
composites are investigated for wear and mechanical properties by re-
inforcing Al with various wt.% of graphite. Thus the presence of gra-
phite composites in Al2O3 ceramic particulates results in increase ten-
sile and flexural strength and governs less wear [8]. The as cast
AleZneMgeCu alloys improve the metallurgical conditions and Cr
improves toughness and tensile strength [9]. Many other researchers
worked with magnesium AZ31 composites reinforced MWCNT were
blended with various weight fractions and enhanced the tensile
strength and mechanical properties [10–12].
Zirconium carbide (ZrC) is ceramic materials which has high mod-
ulus, hardness and wear resistance behavior. ZrC is an important ma-
terial for high temperature applications due to its high melting tem-
perature and excellent corrosion resistance [13]. Using alloying
technique ZrC can be blended with matrix composites [14–17]. In this
research, pure Al, Ale12 Si is utilized as such for further study and
Ale12Si is blended with ZrC in various weight fractions (5, 10, 15 wt.
%) using P/M method. Al matrix composites are influenced by many
factors such as weight content, type of material, shape, size and spatial
dispersion of ZrC in this matrix. The as prepared composites were
subjected to the study of coefficient of friction and specific wear rate of

⁎
Corresponding author.
E-mail addresses: haiterlenina@gmail.com (A. Haiter Lenin), scvettivel@ccet.ac.in (S.C. Vettivel).

https://doi.org/10.1016/j.surfin.2018.01.003
Received 6 February 2017; Received in revised form 3 December 2017; Accepted 18 January 2018
2468-0230/ © 2018 Elsevier B.V. All rights reserved.
A. Haiter Lenin et al.
the composites. MINITAB software used here to correlate the responses
between the variables and equations were generated [18,19]. ANOVA
helps to analyze the result and provides the performance character-
istics, employed for determining the error variance and percentage of
contribution.
2. Experimental setup and procedures
2.1. Materials
Al, silicon and ZrC powders were used in this research. Al with
99.7% purity was purchased from Spectrum reagents and Chemicals
Pvt. Ltd, Ealayar, Cochin. Si, 98.5% purity brought from Lab a chemie
which was used as matrix and ZrC with 99.9% purity as reinforcement
purchased from US Research Nanomaterials, Inc.
2.2. Specimen preparation
The nanocomposites were fabricated using P/M Method. Ale12 Si is
blended with ZrC in various weight percentages of 5, 10, 15 respec-
tively, were grained with Ale12Si in a high energy planetary ball mill
for 1 h with the reduction ratio of 10:1. During ball milling, process
control agent (PCA) toluene was used, to reduce contamination and
oxidation, argon gas flow was maintained all over the process. The
composite powders were collected and characterized with SEM and
particles confirmed through XRD. The milled powders were taken to
compact and compressed in a punch and die set assembly.
Cylindrical compacts of 20 mm diameter were prepared. The com-
pacts were prepared using ball milled powders. The composite powders
were compacted by using suitable punch and die set assembly on a
Universal Testing machine having 1 MN capacity Compacting pressure
was applied gradually and it was 1.2 GPa for all specimens. Graphite
was used to lubricate the punch and die set assembly.
2.3. Powder characteristics
The as prepared powder mixtures were characterized using SEM and
XRD. SEM micrograph of Al particles reveals that spherical and cy-
lindrical shapes whereas ZrC incorporated micrographs shown that
slight agglomeration with good distribution of particles in the mixture.
2.4. X-ray diffraction analysis
The X-ray diffraction (XRD) for the prepared composites Ale12Si
and Ale12 Si with various weight percentage of ZrC was determined
and major peaks shown that presence of Al, minor peaks indicates Si.
The peaks inferred for ZrC is higher for increased weight percentage
which is shown in Fig. 2(a–d). Also there is no oxygen reaction during
sintering of the composite material.
2.5. Sintering
After the compaction, the compacts were immediately taken out
from die set assembly and loaded into the furnace for sintering. To
prevent oxidization, the green compacts were initially covered with
inert argon atmosphere in the furnace. The sintering was carried out in
an inert gas circulated electric muffle furnace at 550 °C for a holding
period of 1 h. As soon as the sintering schedule was over, the sintered
preforms were cooled inside the furnace itself to the room temperature.
After the completion of sintering, the preforms were cleaned by using a
fine wire brush. Powder metallurgy components are always having
pores and it is varying depends on compaction load. The porosity of the
sample is less than 8%. It is confirmed through the Archimedes prin-
ciple [20,21].
150
Surfaces and Interfaces 10 (2018) 149–161
Table 1
Procedure limits and number of levels used in experiment.
Factor Levels Values
Composites (A) 5 Pure Al, Ale12Si, Ale12Sie5ZrC,
Ale12Sie10ZrC, Ale12Sie15ZrC
Sliding distance (B) 4 500, 1000, 1500, 2000
Load (C) 4 10, 20, 30, 40
2.6. Wear test
The wear tests were carried out using pin-on-disc apparatus with the
ASTM G99 test standard. The counter disc steel was EN 31. The disc and
pins were cleaned with acetone before testing the composite. The track
radius or track diameter and sliding velocity was varied for every trial
by varying the machine parameters such as sliding distance and load.
The wear is generated and load pushes the arm to remain in contact.
The signal was generated during the movement of arm and the friction
coefficient was monitored. The smooth wear track surface was estab-
lished during wear testing and also ploughing away the surface aspe-
rities results in wear. The specimens were weighed prior to and after the
wear test using digital electronic weighing balance having an accuracy
of 0.01 mg to determine the weight loss.
2.7. Plan of experiments
The experiments were conducted as per the ANOVA shown
inTable 2. The analysis of variance is helpful in estimating the error
variance and also for determining the percentage of contribution of
parameters such as wt.% of ZrC, applied load and sliding distance.
ANOVA is mainly designed for statistical analysis and optimum para-
meter settings on the output responses. The plots were obtained by
MINITAB software, which correlates the relation between the responses
of each variables contributed in the machining parameters and also
varying the composites wt.%.
3. Results and discussion
3.1. Scanning electron microscopy analysis
The SEM micrograph used to determine the morphology of the
particles and evaluate the size of the particles in the composites. The
particles after mixing can be shown in Fig. 1 and clearly inferred that
ZrC is present in the mixed composites. The particles are uniformly
distributed and slight agglomeration can be visualized. Fig. 1(a–b)
shows spherical shaped Al (30 μm) and particulates like ZrC particles
(less than 100 nm) present. Inference from Fig. 1(c and d) predicated
that carbide particles are well bonded with AleSi composites. The ZrC
particles are in nanometer range and so finely drenched with the
composites. Fig. 1(e) demonstrated that 15 wt.% of ZrC is incorporated
and large number of carbide grains are impregnated with AleSi com-
posites.
3.2. X-ray diffraction analysis
The presence of Al, silicon and ZrC in the composites was confirmed
through X-ray diffraction. The XRD pattern reveals that peak for Al is
dominant whereas Si is reduced minor peaks. Fig. 2(a–b) shows that
absence of volume fraction of ZrC and lower weight fraction of ZrC
respectively. From Fig. 2(c and d) inferred that ZrC is present in
somewhat little higher because of its higher wt.% and reinforced in the
Ale12Si matrix. So, from the peak intensities of ZrC increased with the
increase in wt.% of carbide materials in the composites. The X-ray
diffraction (XRD) results for the prepared composites are shown in
Fig. 2. These results indicate the presence of Al (in the largest peaks),
A. Haiter Lenin et al. Surfaces and Interfaces 10 (2018) 149–161

Table 2 Table 2 (continued)

ANOVA values of SWR and COF.
Composites Sliding Load SWR COF Rank Rank
Composites Sliding Load SWR COF Rank Rank distance (SWR) (COF)
distance (SWR) (COF)
Ale12Sie15ZrC 1500 20 1.801166 0.62 14 21
Pure Al 500 10 7.162963 0.62 80 21 Ale12Sie15ZrC 1500 30 1.462616 0.64 5 33
Pure Al 500 20 4.944444 0.63 75 28 Ale12Sie15ZrC 1500 40 1.371075 0.65 4 37.5
Pure Al 500 30 4.577778 0.66 72 44 Ale12Sie15ZrC 2000 10 2.520436 0.63 31 28
Pure Al 500 40 4.392593 0.68 71 58 Ale12Sie15ZrC 2000 20 1.601166 0.66 8 44
Pure Al 1000 10 5.429756 0.65 78 37.5 Alee12Siee15ZrC 2000 30 1.211987 0.67 3 51
Pure Al 1000 20 3.725926 0.67 63 51 Ale12Sie15ZrC 2000 40 1.210141 0.69 2 63
Pure Al 1000 30 3.446914 0.68 59 58
Pure Al 1000 40 3.215741 0.71 54 69
Pure Al 1500 10 4.967901 0.67 76 51 and the presence of silicon carbide particles and ZrC is indicated by
Pure Al 1500 20 3.417284 0.70 58 65.5
minor peaks. A clearly visible carbon peak can be observed in the hy-
Pure Al 1500 30 3.164609 0.72 51 73
Pure Al 1500 40 2.911111 0.74 45 77 brid composites. The rise in the intensity of the carbon peaks with the
Pure Al 2000 10 4.592593 0.71 73 69 collective graphite content of the composite is evident. A gradual
Pure Al 2000 20 3.218519 0.73 55 75.5 marginal shift of the Al peaks to higher angles with an increase in the
Pure Al 2000 30 3.064815 0.75 50 78.5
wt.% of the graphite relaxed is also evident. Fig. 2(a–d) shows that
Pure Al 2000 40 2.618056 0.76 37 80
Ale12Si 500 10 6.133997 0.60 79 11.5
there is no oxygen reaction in the samples during the sintering process.
Ale12Si 500 20 4.234171 0.62 69 21
Ale12Si 500 30 3.920176 0.63 66 28 3.3. Statistical analysis of variance (ANOVA)
Ale12Si 500 40 3.778759 0.66 65 44
Ale12Si 1000 10 4.624285 0.63 74 28
Ale12Si 1000 20 3.190694 0.65 53 37.5 ANOVA is a numerical design procedure used to break up the spe-
Ale12Si 1000 30 2.951762 0.67 49 51 cific effects from all control factors. The percentage influence of each
Ale12Si 1000 40 2.882341 0.68 44 58 control factor is involved to extent the corresponding effect on the
Ale12Si 1500 10 4.254258 0.66 70 44
brilliance characteristic [11]. Tables 3 and 4 relate the ANOVA tables
Ale12Si 1500 20 2.926388 0.68 47 55
Ale12Si 1500 30 2.71001 0.69 40 63
for the SWR and COF of the wear test specimens. In this table, the
Ale12Si 1500 40 2.558597 0.72 33 73 values given in the column 2 are “Sum of squares” which the variability
Ale12Si 2000 10 4.06113 0.68 67 58 fraction in the dependent variable which is lightened by changes in the
Ale12Si 2000 20 2.727445 0.71 41 69 amount of independent variables. To find out if the test is significant,
Ale12Si 2000 30 2.584438 0.73 34 75.5
some statistic test in the ANOVA case, such as an F-statistic is essential
Ale12Si 2000 40 2.338142 0.75 27 78.5
Ale12Sie5ZrC 500 10 4.985331 0.57 77 5 in which the statistic test holds an F-distribution under the null hy-
Ale12Sie5ZrC 500 20 3.691177 0.60 62 11.5 pothesis [12]. Hence, “F0 value” can be defined as the ratio of mean
Ale12Sie5ZrC 500 30 3.486075 0.62 61 21 square variance of factor divided by the mean square variance of error.
Ale12Sie5ZrC 500 40 3.314962 0.64 56 33
The P-value is the possibility test statistics takes on a value that is
Ale12Sie5ZrC 1000 10 3.758331 0.61 64 16
Ale12Sie5ZrC 1000 20 2.543104 0.62 32 21
smallest as exciting as the apparent value of the statistic when the null
Ale12Sie5ZrC 1000 30 2.365612 0.65 29 37.5 hypothesis H0 is true. Degrees of freedom “DF” indicate the contribu-
Ale12Sie5ZrC 1000 40 2.233318 0.67 25 51 tion of controllable factors.
Ale12Sie5ZrC 1500 10 3.457596 0.63 60 28 ANOVA tables shows that the error sum of squares remains zero,
Ale12Sie5ZrC 1500 20 2.128293 0.66 24 44
that is only one replication was considered to study the design of ex-
Ale12Sie5ZrC 1500 30 1.969132 0.68 21 58
Ale12Sie5ZrC 1500 40 1.817078 0.70 15 65.5 periment for three factors (composition, sliding distance and load) and
Ale12Sie5ZrC 2000 10 3.363181 0.67 57 51 two responses (SWR, COF). Since only one replication was considered
Ale12Sie5ZrC 2000 20 2.016675 0.69 22 61 for SWR and COF, therefore the degree of freedom remains zero.
Ale12Sie5ZrC 2000 30 1.910926 0.71 18 69 Thereby the error sum of squares and the error mean sum of squares
Ale12Sie5ZrC 2000 40 1.758407 0.72 13 73
Ale12Sie10ZrC 500 10 4.229508 0.56 68 2.5
remains zero. So, F0 value column remains zero. Since the test for sig-
Ale12Sie10ZrC 500 20 2.921311 0.57 46 5 nificance is not possible that the F value column remains zero. The R-
Ale12Sie10ZrC 500 30 2.701639 0.60 39 11.5 squared statistic designates that the model as close-fitting describes
Ale12Sie10ZrC 500 40 2.647541 0.62 38 21 100% of the variability in SWR and COF. The adjusted R-squared sta-
Ale12Sie10ZrC 1000 10 3.186885 0.58 52 7
tistic and the predicted R-squared remains zero. Therefore the % con-
Ale12Sie10ZrC 1000 20 2.243698 0.61 26 16
Ale12Sie10ZrC 1000 30 1.925683 0.63 19 28 tributions (P) were tabulated in the last column to determine the in-
Ale12Sie10ZrC 1000 40 1.871311 0.65 17 37.5 fluence of main effects and interaction effects. From the % contribution
Ale12Sie10ZrC 1500 10 2.933333 0.62 48 21 (P) column the main effects such as compositions (A), sliding distance
Ale12Sie10ZrC 1500 20 2.017486 0.64 23 33 (B) and load (C); therefore the predominant factor that influence the
Ale12Sie10ZrC 1500 30 1.722404 0.66 12 44
Ale12Sie10ZrC 1500 40 1.718579 0.67 11 51
SWR and COF was compositions (A) and the remaining two factors
Ale12Sie10ZrC 2000 10 2.837705 0.65 42 37.5 sliding distance (B) and load (C) are very small and the interaction
Ale12Sie10ZrC 2000 20 1.854098 0.66 16 44 effects are negligible. Consequently the test of 5% significance level was
Ale12Sie10ZrC 2000 30 1.540437 0.69 6 63 not conceivable. To test the 95% confidence level on the input para-
Ale12Sie10ZrC 2000 40 1.568443 0.71 7 69
meter the 3-way interaction effect was rejected and hence it is con-
Ale12Sie15ZrC 500 10 1.20186 0.54 1 1
Ale12Sie15ZrC 500 20 2.605094 0.56 35 2.5 sidered as a residual error.
Ale12Sie15ZrC 500 30 2.411783 0.59 30 8
Ale12Sie15ZrC 500 40 2.355017 0.60 28 11.5 3.4. Coefficient of friction as a function of sliding distance
Ale12Sie15ZrC 1000 10 2.844431 0.57 43 5
Ale12Sie15ZrC 1000 20 1.962258 0.60 20 11.5
Ale12Sie15ZrC 1000 30 1.713204 0.61 10 16 The coefficient of friction was explored during the wear test. The
Ale12Sie15ZrC 1000 40 1.659251 0.63 9 28 metal on metal contact takes place at the initial stage and surfaces were
Ale12Sie15ZrC 1500 10 2.616344 0.60 36 11.5 heated to achieve higher coefficient of friction in low steady state. The
generation of loose debris results in increased coefficient of friction at

151
A. Haiter Lenin et al.
higher load. In order to reduce the friction coefficient, ZrC is reinforced
to the matrix and results were taken by varying the load levels (10, 20,
30 and 40 N) and sliding distance (500, 1000, 1500 and 2000 m) by
keeping the track radius and sliding velocity of 100 m and 2.618 m/s
respectively as constant.
In this work, pure Al, Ale12 Si and Ale12Si with ZrC in different
weight percentage is subjected to study the friction coefficient. Fig. 3(a)
illustrates that coefficient of friction is very high for pure Al, whereas Al
with Si shows little reduced friction coefficient and Ale12Sie15ZrC
shows higher reduction in coefficient of friction. From this graph,
Fig. 3(b, c and d) one can infers that, when the load increases with
increase in weight percentage of ZrC, the friction coefficient is reduced.
But pure Al and Ale12Si shows increase in coefficient of friction with
the increase in load. So, ZrC acts as a barrier and form the carbonaceous
film between the specimens and counter surface.
Testing under normal load, ZrC are pressed out from the composites
to the contact surface, thereby the coefficient of friction is reduced.
Under higher load, generation of loose wear debris on the counter-face
is due to the disintegration of copper matrix, results in increased
coefficient of friction. From Fig. 3(a–d), variations of coefficient of
friction with sliding distance were determined for change in load with
152
Surfaces and Interfaces 10 (2018) 149–161
Fig. 1. SEM micrographs of composites (a) Pure Al,
(b) Ale12Si, (c) ZrC, (d) Ale12Sie5ZrC, (e)
Ale12Sie10ZrC and (f) Ale12Sie15ZrC.
composition of carbide materials. The coefficient of friction value was
taken by keeping the track radius and sliding velocity as 100 mm and
2.61 m/s respectively and also by varying the load levels (10 N, 20 N,
30 N and 40 N) and sliding distance (500 m, 1000 m, 1500 m and
2000 m). The friction coefficient is decreasing with increased amount of
nano ZrC to the matrix.
The aluminum hybrid composite shows different friction coefficient
values for various compositions of ZrC. Al matrix is kept as such, pri-
mary reinforcement is Si and secondary reinforcement is nano ZrC
(different wt.%). Mainly, nano-ZrC plays a vital role in increasing the
hardness and wear rate and reducing the friction coefficient to achieve
better mechanical and tribological properties. The coefficient of friction
value was reduced for normal sliding distance and load. Among all
combinations of Si and nano boron carbide, the 15 wt.% ZrC shows very
less coefficient of friction value at 10 N load and 500 m sliding distance.
If the sliding distance and the load are increased gradually, friction
coefficient is also raised for reduced wt.% of samples. The result has
good agreement with [12,15].
A. Haiter Lenin et al. Surfaces and Interfaces 10 (2018) 149–161

Fig. 2. XRD images of composites (a) Ae12Si, (b) Ale12Sie5ZrC, (c) Ale12Sie10ZrC and (d) Ale12Sie15ZrC.

Table 3 3.5. Interpretation of residual graphs of COF

ANOVA for specific wear rate. (Neglecting all the interactioneffects).
The normal probability plot (NPP) of the residuals was plotted to
Source DF Adj SS Adj MS F-value P-value Contribution
(P), (%)
check the normality of the data. The residuals are the variation between
the experimental and predicted values from the linear regression [13].
A 4 42.559 10.6397 227.56 – 39.36 Fig. 4 shows the normal probability plot for Al hybrid nano-composite.
B 3 26.697 8.8990 190.33 – 24.69 These probability plots clearly designates that the detected investiga-
C 3 35.653 11.8842 254.17 – 32.97
Error 69 3.226 0.0468 – – 2.98
tional values lies very close to the normal probability line (straight line)
Total 79 108.134 – – – 100 inferring that the errors are neglected and the model is adequate [14].
S R-sq R-sq (adj) R-sq (pred) Thus, the model formulated for the prediction of both the wear loss and
0.216232 97.02% 96.58% 95.99% the friction coefficient of the Al hybrid composites, as represented by
Eqs. (1) and (2) are adequate [15].

Table 4
ANOVA for COF. (Neglecting all the interaction effects).

Source DF Adj SS Adj MS F-value P-value Contribution (P), (%)

A 4 0.059197 0.014799 673.19 – 31.20

B 3 0.088821 0.029607 1346.77 – 46.80
C 3 0.040234 0.013411 610.05 – 21.20
Error 69 0.001517 0.000022 – – 0.80
Total 79 0.189769 – – – 100
S R-sq R-sq (adj) R-sq (pred)
0.0046887 99.20% 99.08% 98.93%

153
A. Haiter Lenin et al. Surfaces and Interfaces 10 (2018) 149–161

Fig. 3. (a–d) Influence of coefficient of friction as a function of sliding distance for various composites.

Fig. 4. Residual plot for COF.

154
A. Haiter Lenin et al.
Fig. 5. Interaction plot for COF.
The distribution of residuals for all the interpretation of runs is
shown in the histogram. Almost bell shaped proportioned histogram
can be incidental from Fig. 4. The residuals versus the fitted values
(predicted response) for COF and specific wear rate are plotted. The
scattering of the residuals are randomly about zero which implies that
the errors are negligible having constant variance. The responses are
inclined by the order of the runs that share a place when the line se-
quence is used to collect the data. This plot is especially helpful to a
developed design in which the runs are regular.
3.6. Interaction plot for COF
This plot provides detailed information about the factors influencing
the hybrid composite and its friction coefficient was determined by
varying the parameters like wt.%, sliding distance and load applied on
it. COF versus wt.% of ZrC indicates that 15 wt.% of ZrC reduce the
friction coefficient. COF versus load (N) applied shows that reduced
friction coefficient obtained only when there is 10 N (low) load applied.
COF versus sliding distance represents, at 500 m (less) sliding distance
dropping down of friction coefficient was observed. This plot places an
interest that, only when the load and sliding distance is less with in-
creased wt.% of ZrC resulted in reduced friction coefficient as shown in
Fig. 5.
3.7. Specific wear rate as a function of sliding distance
The wear rate of the hybrid composites were determined by keeping
track radius and sliding velocity of 100 m and 2.618 m/s respectively
with varying load (10, 20, 30 and 40 N) and sliding distance (500,
1000, 1500 and 2000 m). When the load and sliding distance increases,
wear of the material also increases. By reinforcing the ZrC material in to
the matrix, specific wear rate gradually reduces with increase in weight
percentage of the reinforcement material. From these graphs,
Fig. 6(a–d) confirms that when the load and sliding distance increases,
wear also increases for pure Al and AleSi matrix. While incorporating
the reinforcement in higher weight percentage reverse nature of results
155
Surfaces and Interfaces 10 (2018) 149–161
as reduced wear rate was obtained.
The deviations of the wear rate of the Ale12SieZrC hybrid com-
posite with normal load at different sliding distance. The specific wear
rate is resolute by keeping the sliding velocity and track radius at
2.61 m/s and 100 mm respectively. The steady increase in wear rate of
the unreinforced Al is recognized to the deformation of microstructure
and steady formation of thin oxide layer which covered the contact
surface. The direct contact of Al with the counter surface is prohibited
at lower load. So the Al deformation and transfer of Al is detected at the
improved normal load. The specimen surface increases with the addi-
tion of ZrC particles, so there may be decline in the contact between the
pin and disc. Basically, the hardness of the composite specimen and
wear rate of the material is contrariwise proportional to each other.
When the sintering temperature and sliding velocity are kept constant,
there must be decrease in wear rate.
From Fig. 6(a–d), it was perceived that specific wear rate of the Al
hybrid composite attained by varying the composition of the material
with sliding distance and load. Al matrix with Si shows steady and
slight increase in specific wear rate for the applied load of 10 N to 40 N
at the sliding distance of 500 m, also when the sliding distance is in-
creased to 1500 m, specific wear rate is raised at 40 N applied load
shown in Fig. 6(d). After the addition of nano ZrC 5 wt.% with the Al
matrix and primary reinforcement enhances the hardness and reduces
the wear of the material even when it was heated to a high temperature
of about 550 °C. Inference from Fig. 6(d) confirms that reduction in
wear rate at 2000 m sliding distance with the 40 N load is applied on
the material. The alternative composite material is enriched with ad-
dition of 10 wt.% ZrC to reduce the wear rate at the low range of sliding
distance and load by keeping the sliding velocity as 2.61 m/s and
temperature as 550 °C at constant. The increase in load and sliding
distance affects the wear rate to rise gradually from 3.9 × 10−6 mm3/
Nm to 4.7 × 10−6 mm3/Nm roughly. So to reduce the wear rate by the
addition of 15 wt.% ZrC with that 12 wt.% Si and Al matrix as revealed
which entails that steady and slight upsurge in curve indicates the
specific wear rate about 3.97 × 10−6 mm3/N-m for 40 N load and
4.25 × 10−6 mm3/Nm for 10 N load applied with a sliding distance of
A. Haiter Lenin et al.
Fig. 6. (a–d) Influence of specific wear rate as a function of sliding distance for various composites.
2000 m.
3.8. Interpretation of residual graphs of SWR
The normal probability plot (NPP) of the residuals was plotted to
check the normality of the data. The residuals are the variation between
the experimental and predicted values from the linear regression. Fig. 7
shows the normal probability plot for Al hybrid nano-composite. These
probability plots clearly designates that the detected investigational
values lies very close to the normal probability line (straight line) in-
ferring that the errors are neglected and the model is adequate. Thus,
the model formulated for the prediction of both the wear loss and the
friction coefficient of the Al hybrid composites, as represented by
equations.
The distribution of residuals for all the interpretation of runs is
shown in the histogram. Almost bell shaped proportioned histogram
can be incidental from Fig. 7. The residuals versus the fitted values
(predicted response) for COF and specific wear rate are plotted. The
scattering of the residuals are randomly about zero which implies that
the errors are negligible having constant variance. The responses are
inclined by the order of the runs that share a place when the line se-
quence is used to collect the data. This plot is especially helpful to a
developed design in which the runs are regular. The distribution of
residuals for all the interpretations is shown in Fig. 7.
3.9. Interaction plot for SWR
The interaction plot shows the specific wear rate of the Al hybrid
composite by varying its influential parameters. SWR versus wt.% of
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Surfaces and Interfaces 10 (2018) 149–161
ZrC infers that reduced wear observed when 15 wt.% ZrC is further.
Then considering the SWR versus load, the 40 N load is applied on the
composite the wear rate reaches extreme point. So, when the load is
10 N, SWR is nearly to 0.05. Also comparing the wear rate with sliding
distance, 2000 m sliding distance affects the material and enhance the
wear rate. The wear rate was reduced only when the sliding distance is
less (say 500 m). So, one can justified from the plot that however ag-
gregate the addition of ZrC (wt.%) to reduce the wear of the composite,
sliding distance and load applied on the material must be less as shown
in Fig. 8. The result has good agreement with [12,15].
3.10. Data checking and model adequacy
The effect of independent variables such as sliding distance, applied
load and wt.% of ZrC were dependent on wear mass loss shown in
Fig. 9. Implies that the mean of COF and SWR. The graphical re-
presentation of the response for the variables like wt.% of ZrC, applied
load and sliding distance are shown in Fig. 10. The presence of green
region evidences that the weight loss of the wear specimen is reduced
for lower load and compare to base alloy and matrix material [16,17].
The following mentioned representation shows that COF and SWR are
contributed with various machining parameters and wt.% of the hard
ceramics. From these pictorial representation inferred that wear re-
sistance is high in dark (green and blue) region which was offered by
the hybrid composites (Ale12Sie15ZrC) under the sliding conditions
and applied load. Thereby, mass loss is also reduced for higher wear
resistance composites as shown in Fig. 11.
A. Haiter Lenin et al. Surfaces and Interfaces 10 (2018) 149–161

Fig. 7. Residual plot for SWR.

3.11. Linear regression models
The correlations between the factors (wt.% of nano carbides, sliding
distance, sliding velocity and load) and the measured parameters (wear
rate and coefficient of friction) were obtained by multiple linear re-
gressions. MINITAB software helps in generating the linear regression
equation which determines the COF and SWR. The friction coefficient
and specific wear rate was calculated by substituting the values in the
regression equation by correlate the relation between the variables such
as load, sliding distance and wt.% of ZrC. Finally, the following re-
gression equations were fitted to the wear and the coefficient of friction
is exemplified below.

Fig. 8. Interaction plot for SWR.

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A. Haiter Lenin et al. Surfaces and Interfaces 10 (2018) 149–161

Fig. 9. Main effect plot (a) SWR and (b) COF.

3.12. Regression equation SWR = 4.288 + 0.1258 wt. % ZrC + 0.08622 Sliding distance
+ 0.08803 Load + 0.02924 wt. % ZrC * Sliding distance

COF = 0.6433 + 0.02891 wt. % ZrC + 0.04453 Sliding distance + 0.02096 wt. % ZrC * Load + 0.02308 Sliding distance * Load

+ 0.03078 Load + 0.000156 wt. % ZrC * Sliding distance + 0.02765 wt. % ZrC * Sliding distance * Load.

+ 0.001094 wt. % ZrC * Load + 0.000469 Sliding distance * Load (2)

+ 0.002656 wt. % ZrC * Sliding distance * Load.

(1) 3.13. Worn surface analysis

The worn surface morphology of the Al hybrid composites were

obtained by the SEM micrographs. Fig. 12 shows Al and Ale12Si are
having high abrasive wear. After the addition of ZrC to the matrix, the

Fig. 10. Effect of sliding distance, composition and load on COF.

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A. Haiter Lenin et al.
Fig. 11. Effect of sliding distance, composition and load on SWR.
wear is somewhat reduced. The increase in wt.% of ZrC with Ale12Si
shows much reduced wear in all the tracks [18,19]. The wear debris is
indicated amount of ZrC particles present in the composite. It is clearly
inferred from Fig. 12(b-e) that wear debris of hybrid composites
Ale12Sie15ZrC is lesser than the wear from Ale12Si composites. The
ZrC particles are much harder than the Al matrix, so higher wear re-
sistance can be obtained.
SEM observations were employed to scan the morphology of worn
surface and the presence of composition of all samples. As expected, the
worn surface of Ale12SieZrC composites show a wrinkled wear surface
morphology and some of the particles protruding from the surface.
From the SEM micrographs, one can perceive the wear debris layer,
smooth grooves, ploughing and roughening of surfaces. When the
specimen was treated in a pin-on-disc apparatus, the hard asperities on
the steel counterpart penetrated and there might be a pull out of re-
inforcement from the composites. The micrographs were taken for Al, Si
and ZrC individually and seen that severe deformation and wear oc-
curred for matrix alloy compared to ZrC. After addition of reinforce-
ment with the matrix element one can grasp the enhancement in re-
duced wear by noticing the smoother surface of the specimen. When the
specimen material was subjected to various load and sliding velocity, it
undergoes wear and different features and morphologies were seen
from the SEM images by using Scanning Electron Microscopy equip-
ment. As the wear debris is totally scattered, higher matrix debris for-
mation occurs by increasing load and sliding distance. Also sliding
velocity, an important factor which was kept constant and supports in
wear behavior reveals that spreading of debris and also forms the oxide
layer. The result has good agreement with [12,22,23].
The worn surface of the composites is shown in Fig. 12(a-e) typi-
cally. The SEM pattern indicates the formation of debris, grooves and
oxide layer. The wear debris formation is mainly generated from the pin
surface. The wear appeared for the composite was significantly differs
from the unreinforced matrix. The specimen was tested under various
loads and observed that reinforced composites were smoother and also
the presence of some grooves at the worn surface. There must be a
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Surfaces and Interfaces 10 (2018) 149–161
considerable reduction in the plastic deformation due to increased
hardness of the composites and increased plastic deformation with in-
creasing the load. The formation of large wear at the pin surface results
in fracture of reinforcements. The result has good agreement with [24].
Fig. 12(c–e) shows characteristic SEM micrographs of worn surfaces
and wear debris of Ale12Si-5 wt.% ZrC and Ale12Si-10 wt.% ZrC and
Ale12Si-15 wt.% ZrC. The worn surface of the composites tested at the
sliding distance of 500 m and at the applied load of 40 N infers that
wear debris and delamination of the composites increases and
ploughing depth is shallower for reduced wt.% of reinforced nano
carbide materials whereas ploughing depth is reduced for higher wt.%
of reinforced material. Also temperature plays a role in worn surface of
the composite material, i.e., at room temperature grooves and ridges
reduces considerably whereas the light material heated to a sintering
temperature shows increased wear and higher depth of grooves was
seen.
The wear test result of pure Al showed in Fig. 12(a) have more
abrasion, wear tracks and delamination. Fig. 12(b) illustrated that un-
even surface formation but slight reduction in wear due to addition of Si
in to Al. The high hard carbide material is incorporated into the matrix
composites resulted in reduced wear. The weight percentage of ZrC
varies wear mechanism also changed. The hybrid composites are sub-
jected to sintering at 550 °C and abrasion wear was deliberated. The
composites after impregnated with 5 wt.% ZrC prevents the dominant
wear as shown in Fig. 12(c). The carbon particles are smeared from the
contact surface of the composites helps in the formation of carbon rich
layer at the interface region. Thereby the contact between the specimen
and disc was barred. The harder nano carbide materials are rich in
hybrid composites as elucidated in Fig. 12(e), the higher wear re-
sistance is obtained by formation of tribo layer that benefits the carbon
rich layer formation at the interface region.
4. Conclusion
In this work, characterizations, mechanical behavior of composite
A. Haiter Lenin et al.
Fig. 12. Worn surface analysis of composites (a) Pure Al, (b) Ale12Si, (c) Ale12Sie5ZrC, (d) Ae12Sie10ZrC and (e) Ale12Sie15ZrC.
specimens were carried out on pure Al, Ale12Si and Ale12SieZrC
hybrid composites. From this experimental work the conclusions can be
drawn.
The composites were prepared by P/M technique. The hybrid
composites were heated to sintering temperature of 550 °C for further
study. The specimens demonstrated that lower coefficient of friction
and specific wear rate. Also maximum wear resistance was achieved for
increase in weight percentage of hard ceramic ZrC. Even when the load
and sliding distance increases, reduced wear obtained for hybrid com-
posites. The influence and percentage contribution of variable para-
meters were analyzed by ANOVA. The variables interacting the wear
rate are sliding distance (28.14%), wt.% of ZrC (39.06) and applied
load (27.9). The higher contribution of ZrC reinforcement improves all
the properties of hybrid composites. The contribution of variables for
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Surfaces and Interfaces 10 (2018) 149–161
friction coefficient are wt.% of ZrC (21.28), sliding distance (53.47 and
applied load (24.34)). In both the cases, contribution of load is lower
and sliding distance is comparatively high. There is no error and neg-
ligible constant variance. By concluding this work, Al hybrid compo-
sites shows significant improvement which mostly attributed to en-
hanced wear resistance and reduced friction coefficient compared to Al
matrix composite.
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