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Materials Today: Proceedings 4 (2017) 557566 www.materialstoday.com/proceedings

5th International Conference of Materials Processing and Characterization (ICMPC 2016)

Effect of Calcium Hexaboride Particles on Predicting the Dry

Sliding Tribological Process Parameter of Magnesium Composite
Using Grey Relational Analysis
P.Seenuvasaperumala *, A. Elayaperumalb
a
Research Scholar, Department of Mechanical Engineering, Engineering Design Division, CEG Campus, Anna University, Chennai - 600025.
b
Professor, Department of Mechanical Engineering, Engineering Design Division, CEG Campus, Anna University, Chennai - 600025.

Abstract

Improving tribological performance of magnesium based composites in dry sliding condition is a crucial challenge. In
this work, fabrication of magnesium composites has been done using squeeze casting techniques. Dry sliding wear behavior of
magnesium composites were conducted on the Pin-on-Disc tribometer. Taguchi optimization technique was used to design the
tribological experiments, while the grey relational analysis was used to predict the optimal tribological process parameters using
multiple responses.From the results obtained, a 62.77% improvement in the predicted result of the tribological process parameter
was observed when compared with middle ranked grey relational grade on the L27 orthogonal array.

2017 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of Conference Committee Members of 5th International Conference of Materials
Processing and Characterization (ICMPC 2016).

Keywords:Magnesium Composite; Calcium Hexaboride; Squeeze Casting; Tribological property; Grey Relational Analysis;

1. Introduction
Increased absorption of carbon dioxide by the atmosphere results in a drastic climatic change and global
warming. Which threatens basic human survival throughout the world [1]. Among the different ways of controlling
carbon dioxide emission, the best is to reduce the fuel consumption by weight reduction of the vehicle in the
automotive domain [2]. Mg and its alloys, when compared with ferrous and aluminum metal alloys, have 430% and
45% lower density respectively. There are several advantages in magnesium and its alloy-based composite materials

* Corresponding author. Tel.: +91-9789414333

E-mail address: seenumeed@gmail.com

2214-78532017 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of Conference Committee Members of 5th International Conference of Materials Processing and
Characterization (ICMPC 2016).
558 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566

when compared with other pure metals and alloys such as high specific strength, hardness, and creep resistance [3-
4]. The only major disadvantage is that they do not withstand high temperature and get easily corroded. Several
researchers have tried to overcome these disadvantages by reinforcing various continuous, non-continuous fibers,
metals, and non-metals like ZrO2, Ca, Li, Y2O3, Ti, SiC, Al2O3, B2O3, ZnO, B4C [5-18].
Calcium Hexaboride (CaB6) is an alkaline earth boride from 2A group [19]. It has favorable properties such as
low density (2.45 g/cm3), high melting point (2508K), high hardness (27Gpa), and chemical stability [20-23]. It has
a major role to play in wear resistance applications in a corrosive environment. Experiments have proved that
addition of calcium hexaboride to metals and non-metals provides improved mechanical properties [24-26]. But
unfortunately, there has been little or no investigation on producing magnesium based composites with CaB6 as a
reinforcing particle. In the present work, pure magnesium has been reinforced with CaB6 by using Gravity casting
and squeeze casting techniques. Several techniques such as powder metallurgy, stir mixing, thixocasting and
centrifugal casting have been used for magnesium composite production. Amongst these, squeeze casting is seen as
a promising technique for reduced porosity which consequently improves strength. Porosity is the critical micro
structural feature that often occurs during the production of the composites which adversely affects the shrinkage of
the composites during their solidification [27-28].
Many researchers tried to improve the tribological performance of magnesium based composites. They studied
the effects of different reinforcement particles and fabrication techniques on the wear mechanism by SEM analysis
carried out on the worn out surfaces [29-32]. Tribological investigations require the optimization of multi-response
process parameters for improving their performance. Besides, the optimization is a crucial to improve the quality
and reduce the experimental costs on the investigations. Taguchi optimization technique is a well-balanced
experiment optimization technique for improving quality with reduced experimental costs and time [33-34]. Taguchi
technique is used to optimize the effects of an individual response. To overcome this issue, Grey relational analysis
was used in combination with Taguchi optimization technique. Some researchers have carried out their tribological
tests using this technique and have shown improvement of tribological performance using the confirmation test [35-
38]. Based on the suggestions found in literature, in this present work grey relational analysis is used to study the
tribological performance of pure magnesium and composites (pure magnesium reinforced with 2 wt. % Calcium
Hexaboride) under dry sliding condition with SAE52100 bearing steel disc.

2. Experimental details

2.1. Materials

Pure magnesium ingots with 99% purity were purchased from Vaishnavi Castings Ltd, Chennai, India. This is the
matrix material, it was cut into 50mm x 50mm x 20mm billets using a band saw. The reinforcement material, CaB6
with a mean particle size of 20mesh and purity of 99.5%, was supplied by Alfa Aeser, USA.

2.2. Processing

A bottom pouring stir casting furnace (made by Swam Equipment Ltd, Chennai, India) was used for the
composite fabrication process. The magnesium billets were melted in a steel crucible at 700C in an electrical
resistance furnace. A productive gas atmosphere of argon and sulfur hexafluoride in the ratio of 5:1 was used. The
matrix molten slurry was stirred at 450rpm for 2 minutes using a twin blade impeller inclined at 45. The blade was
coated by zirtex and made of mild steel. After stirring, the slag was removed from the matrix molten slurry.
Simultaneously, the reinforced particle(CaB6) 2% by weight was preheated and held at 400C for 2 hours in the box
furnace. This is to remove the moisture content and increase wettability. The preheated reinforcement particles was
then mixed with the matrix molten slurry and stirred for uniform distribution at 450rpm for 15 minutes. The molten
composite was then poured into a mold of 50mm diameter and 250mm height by the bottom pouring technique
under the influence of gravity. Before pouring, the mold was preheated to 250C. Squeeze casting is similar except
for the fact that a squeeze pressure of 120 MPa is applied for 2 minutes at 300C [27]. This is carried out at the end
of the above process on the magnesium composite using a hydraulic press with a capacity of 50 tons.
 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566 559

2.3. Density and Porosity

The density of pure magnesium and its composites were determined by using the Archimedes principle under
ASTM standard D3800. The weights of the sample were obtained using an analytical balance machine (with an
accuracy of 0. 00001g) made by Wensar Weighing Scale Limited, India. The theoretical density of the composites
was calculated based on the assumption of full density. All the calculations were done using the rule of mixture.
2.4. Hardness Test
The hardness of the composite material was obtained to estimate of the effect of the reinforcement particle at
room temperature. A Vickers hardness tester made by Chennai Metco Pvt. Ltd, India was used at a load of 30kg.
Ten measurements were taken at ten different locations on a single sample to avoid the effect of indenture resting on
hard reinforcement particles.

3. Tribological Test

The tribological test was carried out at room temperature, by using ASTM: G99 standard in a DUCOM pin-on-
disc tribometer. Each pin sample has a diameter of 8mm and is 50mm in length. The pin sample slides against the
SAE52100 bearing steel (63HRC) disc of 55mm diameter and 10mm thickness. The same surface roughness is
maintained on the disc and pin samples. The tribological experiments were optimized by using Taguchi technique.
Each pin sample was weighed before and after the test by the same analytical balancing machine for calculating the
exact weight lost. The worn out surfaces were cleaned with acetone before weighing.

3.1. Taguchi Method

Optimization of tribological experiment process parameters is a difficult task and it is not easy to control. To
overcome this problem, the Taguchi method has a peculiar design called Orthogonal Array (OA) which contains
well balanced experiments to improve the quality with reduced experimental cost and time. This method is used to
measure the statistical performance of experiments and is called the signal-to-noise (S/N) ratio. The S/N ratio has
three categories namely, the Smaller the better (SB), Medium is the best (MB) and the higher the better (HB). In
tribological applications, the statistical performance of the smaller the better is used for achieving reduced wear rate.
Followed by the statistical analysis of each performance of each experiment, an analysis of variance (ANOVA) is
performed to predict the process parameters that are statistically significant. Finally, a validation test is performed to
confirm the accuracy of the analysis.

Table 1. Design parameters and their levels

Levels
Design Factors Units
1 2 3
Materials (A) P (Pure Mg. as cast) Q (Mg-2 wt.% of CaB6 as R (Mg-2 wt% of CaB6
cast) Squeeze cast)
Load (B) N 10 20 30
Sliding Velocity (C) m/Sec 0.4 0.6 0.8
Sliding Distance (D) m 1000 1500 2000

Four major factors at three levels influenced wear rate of the magnesium composite as shown in Table 1. The
Taguchi method L27 orthogonal array is designed with the interaction effect of factors to determine the process
interrelationship by using Minitab-16 Software as shown in Table 2.
560 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566

3.2. Grey Relational Analysis

Table 2.Grey Relational analysis

Experiment
Design Factors ND GRC GRG Rank
Results
S.
No. Wear Wear Wear
A B C D rate COF rate COF rate COF
(g/m) (g/m) (g/m)
1 P 10 0.4 1000 17.2 0.079 0.7424 0.8805 0.6600 0.8072 0.7336 3
2 P 10 0.6 1500 19.8 0.106 0.6815 0.7884 0.6109 0.7026 0.6568 6
3 P 10 0.8 2000 22.5 0.156 0.6183 0.6177 0.5671 0.5667 0.5669 12
4 P 20 0.4 1500 34.5 0.326 0.3372 0.0375 0.4300 0.3419 0.3860 22
5 P 20 0.6 2000 25.6 0.044 0.5457 1.0000 0.5239 1.0000 0.7620 1
6 P 20 0.8 1000 22.3 0.106 0.6230 0.7884 0.5701 0.7026 0.6364 8
7 P 30 0.4 2000 45.5 0.297 0.0796 0.1365 0.3520 0.3667 0.3594 24
8 P 30 0.6 1000 46.3 0.302 0.0609 0.1195 0.3474 0.3622 0.3548 25
9 P 30 0.8 1500 48.9 0.311 0.0000 0.0887 0.3333 0.3543 0.3438 27
10 Q 10 0.4 1000 15.1 0.186 0.7916 0.5154 0.7058 0.5078 0.6068 10
11 Q 10 0.6 1500 14.5 0.107 0.8056 0.7850 0.7201 0.6993 0.7097 4
12 Q 10 0.8 2000 14.1 0.335 0.8150 0.0068 0.7299 0.3349 0.5324 13
13 Q 20 0.4 1500 28.7 0.322 0.4731 0.0512 0.4869 0.3451 0.4160 21
14 Q 20 0.6 2000 31.5 0.249 0.4075 0.3003 0.4577 0.4168 0.4372 17
15 Q 20 0.8 1000 33.6 0.234 0.3583 0.3515 0.4379 0.4354 0.4367 18
16 Q 30 0.4 2000 44.8 0.337 0.0960 0.0000 0.3561 0.3333 0.3447 26
17 Q 30 0.6 1000 36.6 0.32 0.2881 0.0580 0.4126 0.3467 0.3797 23
18 Q 30 0.8 1500 30.2 0.291 0.4379 0.1570 0.4708 0.3723 0.4215 19
19 R 10 0.4 1000 15.5 0.316 0.7822 0.0717 0.6966 0.3501 0.5233 14
20 R 10 0.6 1500 8.6 0.26 0.9438 0.2628 0.8989 0.4041 0.6515 7
21 R 10 0.8 2000 9.7 0.28 0.9180 0.1945 0.8592 0.3830 0.6211 9
22 R 20 0.4 1500 7.5 0.15 0.9696 0.6382 0.9426 0.5802 0.7614 3
23 R 20 0.6 2000 20.8 0.231 0.6581 0.3618 0.5939 0.4393 0.5166 15
24 R 20 0.8 1000 28.9 0.311 0.4684 0.0887 0.4847 0.3543 0.4195 20
25 R 30 0.4 2000 6.2 0.293 1.0000 0.1502 1.0000 0.3704 0.6852 5
26 R 30 0.6 1000 15.2 0.27 0.7892 0.2287 0.7035 0.3933 0.5484 12
27 R 30 0.8 1500 30 0.25 0.4426 0.2969 0.4729 0.4156 0.4442 16

The Grey relational analysis was first proposed by Deng in 1989. It is an effective statistical tool for analyzing
multiple response characteristics in tribological applications. This analysis is used for finding both the independent
and interrelated data in the series. The grey relational analysis is combined with the Taguchi technique to find the
parameters that influence the wear rate of magnesium, gravity and squeeze magnesium composite under multiple
responses.
In this investigation, wear rate and co-efficient of friction are taken as the multiple responses. These were taken
and discussed as shown in Table 2.
 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566 561

(i) Grey Relational Normalization

The first step in the grey relational analysis is normalizing the experimental results. The values are converted in
the range of 0 to 1. For the condition of"the smaller the better", the following equation is used.

Max Yi ( a ) Yi ( a )
GRN i ( a ) = (1)
Max Yi ( a ) Min Yi ( a )

Where, GRNi(a) is grey relational normalization, while Max Yi(a) and Min Yi(a) are the largest, and smallest
values of Yi(a) for the ath response. Here, 'a' is the notation for wear rate. Similarly, 'b' can be substituted for 'a'
derives the normalized value of co-efficient of friction. The best possible normalized result is indicated by 1 as
shown in Table 2.

(ii) Grey Relational Co-efficient

The Grey relational co-efficient express the relationship between the actual experiment and the normalized
experimental results. The grey relational co-efficient is calculated by using the following equation,

Min + Max
GRCi ( a ) = (2)
oi ( a ) Max

Where, GRCi(a) is the Grey relational co-efficient, Max, Min are the maximum and minimum normalized values.
oi is the difference between the maximum and the actual normalized value. is the distinguishing co-efficient and
it is used to adjust the difference due to the relational co-efficient. In this analysis, value of 0.5 is taken for good
stability of outcomes with moderate effects. The grey relational co-efficient is shown in Table 2.

(iii) Grey Relational Grade

The multiple response characteristics are obtained by using the grey relational grade. The equation used here is,

1 n
GRGi = GRCi ( a ) (3)
n a =1

Where 'n' is the number of performance characteristics.

(iv) Grey Relational Ranking

The grey relational rank is based on the grey relational grade and is shown in Table 2. The experimental
parameters of the top ranked experiments are closer to the optimal parameters.

4. Result and Discussion

4.1. Density and Porosity

The outcome of changes in density and porosity of the developed composite are shown in Table 3. The
experimentally obtained density of the composites is higher than that of pure magnesium. This is because the density
of reinforcing particle is higher than that of matrix material. The results Results obtained from pure magnesium, gravity and
562 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566

squeeze magnesium composites shown in table 3, the squeezed composite has reduced porosity and higher density than the
gravity composite. This may be attributed to the squeeze pressure applied on the former.

Table 3.Results obtained from pure magnesium, gravity and squeeze magnesium composites
Materials Theoretical density Experimental density Porosity Hardness (30Kgf)
(g/cm3) (g/cm3) (%) HV
P 1.74 1.725 0.86 322
Q 1.758 1.72 2.16 392
R 1.758 1.745 0.74 452

4.2. Hardness

The composite samples show hardness values higher than that of pure magnesium shown in Table 3. This is due
to the reduced grain size and also due to presence of hard reinforcement particles (CaB6) in the matrix material
which constrains local deformation during indentation. In a comparison between gravity and squeeze casting, the
latter offers higher hardness due to reduced porosity and grain size [28].

4.3. Tribological Analysis

Tribological tests were conducted based on optimized tribological process parameters of pure magnesium,
gravity and squeeze magnesium composites. The pin samples were weighed before and after each tribological test to
find the exact weight lost. The mean co-efficient of friction for each test was recorded by the data acquisition system
connected to the Duccom pin-on-disc tribometer. Three sets of experiments were carried out for checking
repeatability. The mean value of the wear rate and co-efficient of friction were used as inputs for grey relational
analysis.

4.3.1. Factor and interaction effects

Where the load increases wear rate increased on composites due to the abrasive micro cutting. The tribological
process parameters are separated at different levels by taking the average of the grey relational grades for each
individual level in an orthogonal array. The mean grey relational grade of each level(1,2 and 3) for factor A are
calculated by taking the average of the experiments 1 to 9, 10 to 18 and 19 to 27 respectively. The mean grey
relational grade of the composite is calculated in the same manner from the remaining experimental results. Details
are shown in Table 4.

Table 4. Response table for grey relational grade

Level A B C D
1 0.5333 0.6224 0.5351 0.5154
2 0.4761 0.5302 0.5574 0.5323
3 0.5746 0.4313 0.4914 0.5362
Delta 0.0985 0.1911 0.0660 0.0207
Rank 2 1 3 4
Total mean grey relational grade = 0.5332

The response table is derived and the rank is ordered by the magnitude of delta. Delta is calculated by subtracting
the minimum from the maximum for each level. The top ranked factor exerts maximum on influence the wear rate
of the composite.Table 4.reveals that factor B has the highest influence in controlling the wear rate of the composite.
The individual effects and interaction effects of mean grey relational grades are plotted by using Minitab-16 and are
shown in Figs. 1(a) and (b).
 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566 563

Fig. 1. Mean Grey Relational Grades for multi response characteristics (a) Individual effects; (b) Interaction effects.
From the response table, A3B1C2D3 is found to be the optimal process parameter offering a minimal wear rate and
co-efficient of friction. The squeezed composites offer higher density and lower porosity compared to the gravity
cast composite and the matrix material. From the response table, load is seen as a biggest influencing factor on wear
rate and co-efficient of friction. Decrease in sliding velocity is also noticed. Due to the concentration of the load
impact at a certain sliding area, the wear rate and co-efficient of friction increases. An increase in the sliding
velocity occurs irrespective of load on the sliding surface which leads to an increase in the wear rate. When the
sliding distance increases, the decrease in wear rate can be attributed to oxide formation on the surface due to
temperature rise [29].

4.3.2. Analysis of variance (ANOVA)

ANOVA is a method of statistical analysis providing insight on the influence of individual and interaction
factors. Here, it is used to analyze the contribution of factors on wear rate. Taguchi method cannot estimate the
effects of the individual and interaction factors. In this present work Minitab-16 was used to perform ANOVA.
Table 5.reveals that the factor B (load) is the highest contributing individual factor. The interaction factor A x B
(material x load) is the highest contributing interaction factor on wear rate.

Table 5. Results of ANOVA

Source Degrees of freedom Sum of square Mean square F-test % of Contribution
A 2 0.0441 0.0221 1.51 8.9
B 2 0.1645 0.0823 5.64 33.1
C 2 0.0203 0.0102 0.7 4.1
D 2 0.0022 0.0011 0.08 0.4
AXB 4 0.0819 0.0205 1.41 16.5
AXC 4 0.0397 0.0099 0.68 8
AXD 4 0.0571 0.0142 0.98 11.5
Error 6 0.0874 0.0145 1 17.5
Total 26 0.4971 0.0191 1.31 100

4.3.3. Confirmation test

A confirmation test is carried out to check the accuracy of analysis after optimizing the process parameters. The
grey relational grades ( ) for the optimal tribological process parameter can be calculated by using the following
equation,

n
= m + ( a m ) (4)
a =1
564 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566

Here, m is the total mean grey relational grade, a is the mean grey relational grade at the optimal level, n is the
number of the input process parameters that significantly affects wear rate and co-efficient of friction. The
comparison of experimental grey relational grade, predicted grey relational grade and the initial grey relational grade
is shown in Table 6. The tribological parameters of the middle ranked (14th rank) grey relational grade is assumed
as the initial condition. The improvement of the grey relational grade at optimal level is 0.3285 which is an
improvement of 62.77%.Improvement of grey relational grade = 0.3285

Table 6. Results of confirmation test

Initial Parameter Optimal Parameter
Prediction Experimental
Level A3B1C1D1 A3B1C2D3 A3B1C2D3
Wear 15.5 7.5
COF 0.316 0.09
Grade 0.5233 0.6761 0.8518

4.3.4. Microstructural study of the worn out surfaces

Worn out surfaces on the pin and disc samples (tested under predicted optimal parameters) were analyzed by
using SEM for prediction of wear mechanism.

Fig. 2. SEM images of worn out surfaces (a) Pin sample (b) Disc sample (c) Wear debris (d) EDX pattern of the wear debris.

From the SEM images [Figs. 2(a) and 2(b)], it is observed that worn out material from the pin surface was
transferred on to the disc surface due to adhesive wear which results in plastic deformation on the pin surface.
Oxidation wear also takes places on the pin samples due to thermal softening caused by the long sliding distance
[29]. Some of the horizontal grooves present on the disc surface are due to abrasive wear that takes place where the
hard reinforced particles slide on the disc [31]. The EDX analysis confirms that elements (B, Ca, Fe, Mg and O)
 P.Seenuvasaperumal/ Materials Today: Proceedings 4 (2017) 557566 565

were present in the wear debris [Figs. 2(c) and 2(d)] collected during the experiment. This is evidence that oxidation
and abrasive wear occurred on the pin and disc.

5. Conclusion

In this study, tribological tests were carried out on pure magnesium, gravity and squeeze magnesium composites.
Based on the results, the following major conclusions have been arrived at:
Fabrication of the new CaB6 reinforced magnesium composite is possible.
Improvedhardness values obtained on the composites were due to reinforcement by the hard particle. A further
improvement was noticed on the squeeze composite. The squeeze composite also offers reduced porosity, when
compared to the gravity composite. This can be attributed to the applied squeeze pressure.
Tribological tests were conducted using the Taguchi optimized process parameters. The predicted optimized
tribological parameter(A3-R, B1-10N, C2-0.6m/Sec, D3-2000m) using grey relational analysis offer reduced wear
rate and co-efficient of friction. This provides an improvement of 60% when compared with the middle ranked grey
relational grade in the L27 orthogonal array.
Load is the biggest factor influencing rate of wear and co-efficient of friction. This is confirmed by ANOVA.
Adhesive wear mechanism predominates wear on the squeeze composite pin. The reinforcing hard particles cause
abrasive wear on the disc, as seen in the SEM images.

Acknowledgement

The Authors would like to express their sincere thanks to the Anna University, Chennai-600025 for the
opportunity of availing the research fund under the scheme of Anna Centenary Research Fellowship (ACRF). Also,
thanks to Swam Equipment Ltd, Chennai for the composite fabrication work.

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