Surf. Topogr.: Metrol. Prop. 9 (2021) 015031 https://doi.org/10.

1088/2051-672X/abefc2

PAPER

Analyzing the mechanical and wear behavior of age hardening

RECEIVED
4 November 2020
processed AZ31 magnesium composites
REVISED
24 February 2021
ACCEPTED FOR PUBLICATION
Seenuvasaperumal P1,2 , A Elayaperumal1 , Paskalis Sahaya Murphin Kumar3 and S Arulvel2
17 March 2021 1
Department of Mechanical Engineering, CEG Campus, Anna University, Chennai, India
2
PUBLISHED School of Mechanical Engineering, Vellore Institute of Technology, Vellore - 632014, India
3
26 March 2021 Department of Civil and Environmental Engineering, Yonsei University, Seoul, Republic of Korea
E-mail: seenumeed@gmail.com

Keywords: age hardening, wear behavior, calcium hexaboride, magnesium composite, optimization

Abstract
The usage of AZ31 magnesium alloy has been limited in tribology applications, due to low hardness and
poor wear resistance. In this connection, the age-hardening process is a promising heat treatment
process for enhancing mechanical strength and wear resistance. Hence, the present work aims to analyze
the effect of the age-hardening process on the microstructure, mechanical and wear behavior of AZ31
Magnesium-Calcium hexaboride composites (Mg composite). Here, dry sliding wear behavior was
analyzed with different loads (10, 20, and 30 N) and sliding velocity (0.4, 0.6, and 0.8 m. s−1) for a
constant sliding distance of 2000m. Age hardened composites exhibited a higher hardness and
compressive strength which was due to the increased volume of the secondary precipitates (Mg17Al12
and Al8Mn5). The morphology study revealed that there is an exhibition of shear bands and brittle
fracture for Age hardened composites. The remarkable wear rate reduction was achieved for age
hardening processed composites due to the increased load-bearing capacity induced by the presence
of a high volume of secondary precipitates. Delamination wear is the dominant wear mechanism for
the composites and the delaminated craters increases with increasing the load condition. Further, the
elemental mapping on the collected wear debris was also used to confirm the wear mechanism.

1. Introduction to understand the wear behavior of commercial AZ31 Mg

Among the different materials, Magnesium (Mg) receives
a better attraction due to low density, high specific
strength, and ease of recyclable. However, its utilization
has been limited in several industrial applications due to
poor ductility, thermal stability, creep, wear and corrosion
resistance, etc [1, 2]. Hence to improve the wear resistance
of Mg, several metals, ceramics, and solid lubricants were
added to the matrix through different processing techni-
ques [3–7]. Amongst, the introduction of soluble ele-
ments (alloy) could induce grain refinement and high
hardness due to the formation of new precipitates [2],
which results in a low wear rate. Similarly, the presence of
insoluble elements (ceramics) could also reduce the initial
grain size and increases the load-bearing capacity of
composites during surface damage.
Magnesium-Aluminum and zinc-based alloy (AZ31
Mg alloy) are commercialized and used in several auto-
mobiles application compared to the other system of Mg
alloys. Also, several research works were reported recently
alloy and their composites [8–14]. However, there are
limited reports to date on the wear behavior of Calcium
hexaboride (CaB6) reinforced Mg composites. CaB6 is a
promising reinforcement candidate for use in the compo-
sites due to the low coefficient of thermal expansion
(6.2× 10−6 °C−1) and density (2.45 g. cm−3), high hard-
ness (27 GPa), and melting point (2235 °C). Especially, in
terms of good wear resistance and chemical stability in the
corrosive environment. Hence in the previous articles
[15–17], the author has developed a CaB6 reinforced Mg
composite and observed that the CaB6 particles are cap-
able of enhancing the mechanical and tribological beha-
vior of the composite. To further enhance the mechanical
behavior and wear resistance, the present article imple-
ments the heat treatment process (Age hardening) for
AZ31 Magnesium-CaB6 composites.
The heat treatment process is a technique that is
used to increase (or) decrease the strength for achiev-
ing the desired property. Among the various heat
treatment process, Age hardening heat treatment

© 2021 IOP Publishing Ltd

Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
Figure 1. Photographic image of box furnace with age hardening process parameters.
(Solution treatment+artificial aging) process is used
for enhancing the mechanical strength by refining and
increasing the volume of secondary precipitates
[18, 19]. Also, it was observed that the wear resistance
was improved through the age-hardening heat treat-
ment process due to the increased hardness of the
composite while compared with the as-received con-
dition. However, the age-hardening heat treatment
process depends on the reinforced ceramic particu-
lates in the magnesium composite. Also, increasing the
weight percentage of the ceramic particulates are
influencing to the aging kinetics of the metallic matrix
[20, 21]. Hence, the present work was aimed to analyze
the different weight percentage (0, 2, 3 and 4) of CaB6
particles to the age-hardening behavior of AZ31
Magnesium-CaB6 composites. Accordingly, the age-
hardening heat treatment processed samples were
used for microstructure characterization, microhard-
ness, compressive strength, and wear analysis. Wear
study is carried out at different loads (10, 20, and 30 N)
and sliding velocities (0.4, 0.6, and 0.8 m. s−1) for 2000
m of sliding distance at 28 °C (room temperature)
using the Pin-on-disc tribometer. Worn-out pin sur-
face, disc surface, and the collected wear debris are
characterized to find the wear mechanism with the
help of a field emission scanning electron microscope
(FESEM) which is attached with the energy dispersive
spectroscopy (EDS) analyzer.
2. Experimental details
2.1. Heat treatment process
CaB6 reinforced Mg composites (reinforced by 2, 3,
and 4 wt.% of CaB6) were fabricated through
the bottom pouring stir casting technique [15]. The
fabricated as-cast Mg-CaB6 composite ingots are
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Seenuvasaperumal P et al
heat-treated in the box furnace (as shown in figure 1)
following the ASTM standard B 661-06. The various
stages of the age-hardening process carried out on
Mg-CaB6 composite as follows, T4 process (solution
treatment) was performed at 415 °C for 10 h under an
argon atmosphere and quenched in water (76 °C). The
water quenched samples were then transferred into an
oil bath of temperature 196 °C for the artificial aging
process (T5) which was performed for 20 h. The heat-
treated composite samples were then used for
mechanical and tribological characterization.
2.2. Microstructure characterization
Microstructural characterization like grain bound-
aries, secondary phases and CaB6 particle distribution
are observed on the mirror-polished Mg composite
samples using Optical microscopy (OM). Before the
microscopy observation, metallographic polishing
was executed with a different grid range of sandpaper
and ended with colloidal silica using a mechanical
polisher. The polished samples were then ultrasoni-
cated in ethyl alcohol for 2 min. The ultrasonicated
samples were etched using an acetic-picral etching
solution to reveal the grain boundaries. The etched
samples were used for microstructure observation
done using an Olympus DP −10 microscope. Also, the
porosity of the composites was evaluated using the
Archimedes principle under ASTM standard
D3800 [15].
2.3. Mechanical behavior
A Micro-hardness test was conducted on age-hard-
ening processed AZ31 Mg composites at room temp-
erature with 50 g load applied for 15 s by using the
Shimadzu micro-Vickers hardness tester. Measure-
ments were taken on ten different locations in the
Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
Figure 2. Photographic image of Pin-on-disk tribometer set up with wear parameters.
Table 1. Design Parameters and Their Levels.
Levels
Design factors Units 1 2
Material (P) E F
Sliding load (Q) N 10 20
Sliding velocity (R) m. s−1 0.4 0.6
Sliding distance (S) m 500 1000
composite surface for avoiding the particles’ indenture
resting. Ten measurements were processed at 10
different locations on the mirror-polished composite
sample to avoid the effect of indenture resting on hard
reinforced particles. The universal testing machine
(UTM) was used for analyzing the compressive
behavior of the age-hardening processed Mg compo-
sites. Experiments were conducted with a crosshead
speed of 1 mm. min−1 at room temperature. Before
conducting the compressive test, age hardening pro-
cessed AZ31 Mg composites were machined as per the
ASTM: E9 standard. Three sets of experiments were
conducted in each composite for ensuring reproduci-
bility. Optical microscope and FE-SEM were used for
analyzing the macro and micro-fracture behavior
respectively.
2.4. Wear analysis
The dry sliding wear behavior of age hardening
processed AZ31 Mg composites were studied against
the SAE 52100 steel disc at room temperature with the
help of a pin-on-disc tribometer, as shown in figure 2.
The required dimension of pin (f 8 mm and height
30 mm) and disk (f 55 mm and thickness 10 mm)
samples were fabricated using ASTM: G99 standard.
Also, the pin and disk samples were polished to match
the same surface roughness (10 μm) on both sliding
surfaces. To avoid the high experimental cost, the
Seenuvasaperumal P et al
tribological process parameters are optimized using
the Taguchi technique assisted by grey relational
analysis. Four factors with four levels were taken as
3 4 tribological inputs which influenced the wear rate of
the age-hardening processed AZ31 Mg composite, as
G H shown in table 1. Accordingly, the Taguchi method L16
30 40
orthogonal array is designed to determine the process
0.8 1
1500 2000
interrelationship, as shown in table 2. The pin samples
were weighed before and after each tribological test to
find the exact mass lost. The mean coefficient of
friction for each test was recorded by the data
acquisition system connected to the Ducom pin-on-
disc tribometer. Three sets of experiments were
carried out for checking repeatability. The wear rate is
calculated hereby [15],
Mb - Ma
wear rate = g . m-1 (1)
Dt
Where, Mb - the mass of the pin before the wear test,
Ma - the mass of the pin after the wear test, and Dt -
total sliding distance.
The obtained average wear rate and CoF from the
L16 orthogonal array were taken as input for the grey
relational analysis. Various steps involved in the grey
relational analysis like normalization, grey relational
co-efficient and grey relational grades are evaluated
using equation number (2)–(4), respectively [17].
Also, the evaluated normalized value, grey relational
coefficient, grey relation grade, and rank are shown in
table 3. The evaluated grey relational grade is used for
deriving the response table for predicting optimized
tribological process parameter, rank was ordered by
the magnitude of the delta, as shown in table 4.
max yi (a) - yi (a)
GRNi = (a) (2)
max yi (a) - min yi (a)
Dmin + YDmax
GRCi (a) = (3)
Doi (a) + YDmax
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Surf. Topogr.: Metrol. Prop. 9 (2021) 015031 Seenuvasaperumal P et al

Table 2. Responses to the L16 Orthogonal array.

Design Factors Experiment Results of Responses

−1
S. no. P Q R S Wear rate (μg. m ) S.D CoF S.D ST (°C)

1 E 10 0.4 500 19.80 2.01 0.23 0.023 31.3

2 E 20 0.6 1000 29.10 3.15 0.31 0.019 32.0
3 E 30 0.8 1500 49.40 4.20 0.34 0.028 34.6
4 E 40 1 2000 58.75 1.80 0.33 0.097 38.0
5 F 10 0.6 1500 18.13 2.22 0.22 0.056 32.3
6 F 20 0.4 2000 32.70 1.55 0.18 0.068 34.3
7 F 30 1 500 38.40 3.42 0.13 0.081 35.3
8 F 40 0.8 1000 50.50 3.41 0.17 0.034 38.3
9 G 10 0.8 2000 18.95 1.41 0.16 0.096 34.6
10 G 20 1 1500 33.87 2.21 0.05 0.086 35.6
11 G 30 0.4 1000 44.90 3.49 0.29 0.039 34.6
12 G 40 0.6 500 46.80 2.28 0.28 0.037 36.3
13 H 10 1 1000 19.00 2.22 0.19 0.042 34.6
14 H 20 0.8 500 26.40 5.43 0.16 0.072 34.3
15 H 30 0.6 2000 49.55 2.81 0.28 0.036 35.0
16 H 40 0.4 1500 52.20 6.10 0.18 0.051 33.6

S.D—Standard Deviation, CoF—Coefficient of Friction, ST - Sliding contact surface temperature at the end of wear
test.

Table 3. Grey Relational analysis. Table 4. Response table for grey relational grade.

ND GRC Level P Q R S

Wear rate Wear rate 1 0.472 0.731 0.523 0.575

S. no. (μg. m−1) CoF (μg. m−1) CoF GRG RANK 2 0.583 0.622 0.505 0.527
3 0.588 0.431 0.581 0.581
1 0.959 0.379 0.924 0.446 0.685 5 4 0.554 0.412 0.514 0.514
2 0.730 0.091 0.649 0.355 0.502 9 Delta 0.116 0.319 0.102 0.060
3 0.230 0.000 0.394 0.333 0.364 15 Rank 2 1 3 4
4 0 0.039 0.333 0.342 0.338 16 Total mean grey relational
5 1.000 0.425 1.000 0.465 0.732 4 grade=0.554
6 0.641 0.568 0.582 0.537 0.560 8
7 0.501 0.726 0.501 0.646 0.573 7
8 0.203 0.582 0.386 0.545 0.465 10
Table 5. Results of ANOVA.
9 1 0.639 1 0.580 0.771 2
10 0.613 1 0.563 1 0.782 1 Degrees Sum
11 0.341 0 0.431 0.373 0.402 12 of of Mean % of
12 0.294 0.196 0.415 0.384 0.399 13 Source freedom square square F-test Contribution
13 0.979 0.530 0.959 0.515 0.737 3
14 0.796 0.632 0.711 0.576 0.643 6 P 3 0.034 0.110 02.76 09.3
15 0.227 0.189 0.393 0.382 0.387 14 Q 3 0.284 0.095 22.80 76.9
16 0.161 0.540 0.373 0.521 0.447 11 R 3 0.025 0.008 01.96 06.6
S 3 0.014 0.005 01.12 03.3
Error 3 0.012 0.004 03.3
Total 15 0.369 100
1 n
GRGi = å GRCi (a)
n a=1
(4)

mechanisms were confirmed by analyzing the corresp-

The analysis of variance [ANOVA] is a statistical
analysis for providing insight into the influence of the
individual factors. Hence, ANOVA was derived using
the grey relational grade, the calculated values are in
table 5. The detailed tribological analysis of AZ31 Mg
composites was conducted with different parameters,
the maximum level of the predicted insignificant fac-
tor is taken as a constant. After the wear test, the sur-
face of the worn-out pin was cleaned using ethanol
and analyzed using FESEM to predict/identify the
wear mechanisms. Also, the predicted/identified wear
onding wear debris microstructure and elemental
mapping was observed using FESEM-EDX.
3. Results and discussion
3.1. Microstructure analysis
The microstructure of age hardening processed AZ31
Mg composite with a different weight percentage of
CaB6 particle is depicted in figures 3(a)–(d). Image J
software was used to measure the average grain size of

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Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
Figure 3. Observed OM images for age hardening processed AZ31 Mg composites (a). 0 wt. % of CaB6, (b). 2 wt. % of CaB6, (c). 3 wt. %
of CaB6, (d). 4 wt. % of CaB6.
over 50 grains. The evaluated grain size of heat-treated
monolithic AZ31B Mg alloy with 0, 2, 3, and 4 wt.% of
CaB6 reinforced AZ31B Mg composite are 263 μm,
102 μm, 82 μm and 65 μm respectively. There was a
reduction in the grain size after the reinforcement of
the CaB6 particle in the Mg matrix. Also, the refine-
ment increases considerably with the increase in the
weight percentage of CaB6 particles. Among the
different weight percentages, AZ31 Mg composite
with 4 wt.% of CaB6 has shown a greater reduction in
the grain size due to the higher pinning effect. Also, it
is observed that the secondary precipitates (Mg17 Al12)
were well refined and their volume increases for the
heat treatment process. The Image J software was used
for evaluating the amount of Mg17Al12 presents in the
composites. The evaluated amount of Mg17Al12 in
heat-treated monolithic AZ31B Mg alloy with 0, 2, 3,
and 4 wt.% of CaB6 reinforced AZ31B Mg composite
is 2.3%, 3%, 3.1% and 3.1% respectively. In addition
to this, the refined secondary precipitates are located
in the junction of triple grain boundaries of age
hardening processed AZ31B Mg composites, indicated
by the arrow in figure 1(a). The distribution of these
precipitates was also found increasing with the weight
percentage of the CaB6 particle.
The high precipitates distribution was reported for
the AZ31 Mg composite with 4 wt.% of CaB6 particles.
The porosity of the composites was evaluated using the
5
Seenuvasaperumal P et al
Archimedes principle under ASTM standard D3800.
The evaluated values have been inserted into the
microstructure. It was observed that higher porosity in
the composite while compared with the monolithic
alloy. It was due to the micropores and microvoids
between matrix and reinforced particles which were
attributed to the gas entrapment and the solidification
shrinkages.
3.2. Mechanical behaviour
The microhardness evaluation was conducted on
mirror polished age-hardening processed AZ31 Mg
composite samples using Vickers microhardness tester
with 50 g load for 15 s of dwell time. The evaluated
microhardness is shown in figure 4, and it is observed
that the microhardness of the age-hardening pro-
cessed AZ31 Mg composites are enhanced compared
to the age-hardening processed AZ31 Mg alloy due to
the refined microstructure. This could be related to the
three phenomena as follows, (i) Homogenous distri-
bution of hard CaB6 particulates in the AZ31 Mg alloy,
(ii) An increased volume of the secondary precipitates
and (iii) The presence of refined secondary precipitates
in the junction of triple grain boundaries. The induc-
tion of these three phenomena has constrained the
local deformation during indentation and thereby
improving the hardness despite the porosity. Among
the different composites, the higher hardness was
Surf. Topogr.: Metrol. Prop. 9 (2021) 015031 Seenuvasaperumal P et al

Figure 4. Evaluated microhardness, compressive strength, and strain for age hardening processed AZ31 Mg composites.

Figure 5. FESEM observation on compressive fractured surface of age hardening processed AZ31 Mg composites, (a). 0 wt. % of CaB6,
(b). 2 wt. % of CaB6, (c). 3 wt. % of CaB6, (d). 4 wt. % of CaB6. The macro view of fractured samples was inserted in the corresponding
FESEM images.

reported for the age hardening processes AZ31 Mg
composite with 4 wt.% of CaB6 particles.
The ultimate compressive strength of age hard-
ening processed AZ31 Mg composites are compara-
tively higher than the age-hardening processed AZ31B
Mg alloy. Compressive strength increases considerably
with the addition of CaB6 particles. In comparison, the
ultimate compressive strength of age hardening pro-
cessed AZ31 Mg composite with 4 wt.% is compara-
tively higher (Values) than the 3 and 2 wt.% of CaB6
particle reinforcement age-hardening processed AZ31
Mg composites. Primarily, this was arising as a result
of grain boundary strengthening of an increased
volume of CaB6 particles. Also, the refined secondary
precipitates with increased volume are contributing to
an increased barrier to the dislocation motion. Also,
few secondary precipitates are dispersed in the Guinier
Preston zones which facilitates cross-slip, and the Gui-
nier Preston zones do not work as crack initiation and
propagation site. Hence, it is favouring strength

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Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
enhancement [22–24]. Also, the reinforced CaB6 par-
ticles could have the ability to enhance the strain hard-
ening rate by hindering the dislocation motion [11].
To further study the failure mechanism, the frac-
tured surfaces of age hardening processed AZ31 Mg
composites were analyzed using FESEM and shown in
figures 5(a)–(d). Also, the corresponding macroscopic
images were inserted as an inlay image of figures 5(a)–(d).
It is well evident that from the macroscopic image
that the composites failed via crack (inclined with 45° to
the compressive axis) and shattered into 2 parts. Also, the
microscopic images revealed the shear bands arising
as a result of the twinning shear [18]. Moreover, the
fracture was initiated along the twin boundaries or inter-
face between the reinforced particles/secondary pre-
cipitates and the matrix. As the twin boundaries are
favouring the crack nucleation and propagation path
[19], the cracks and voids are seen on the fractured sur-
face. Particularly, the fractured surface of age hardening
processed AZ31 Mg composites showed a mixed-mode
of fractures such as shear bands and brittle fracture
[figures 5(b)–(d)].
3.3. Wear analysis
The tribological tests were conducted with the help of
a pin-on-disc tribometer using age-hardening pro-
cessed AZ31 Mg composites. The obtained average
wear rate and CoF from the L16 orthogonal array were
taken as input for the grey relational analysis using
equations (2), (3), and (4). The evaluated normalized
value (equation (2)), grey relational coefficient
(equation (3)), grey relation grade (equation (4)), and
rank are shown in table 3.
The grey relational grade is used for deriving the
response table, rank was ordered by the magnitude of
the delta, as shown in table 4. Delta is calculated by
subtracting the min from the max for each level. The
1st ranked factor exerts max influence on the wear rate
of age hardening processed AZ31 Mg composite.
Table 4 reveals that factor Q has the highest influence
to control the wear rate of age hardening processed
AZ31 Mg composite. It was observed that (from the
response table) the load is the major contribution to
control the wear rate. Also, contact surface temper-
ature was measured with the help of an IR thermo-
meter, measured values are in table 2.
It was noticed that the contact surface temperature
was increased by increasing load. It was arising as a
result of the increased contact surface. It was found
that (From the response table), P3Q1R3S3 to be an
optimal tribological process parameter to offer the
minimal wear rate. The analysis of variance [ANOVA]
is a statistical analysis for providing insight into the
influence of the individual factors. Hence, ANOVA
was derived and shown in table 5. It was observed that
the sliding distance is insignificant (3.3%) to tribologi-
cal behavior. Also, it was observed by the author’s pre-
vious report, the sliding distance is not more
7
Seenuvasaperumal P et al
Table 6. Results of the confirmation test.
Optimal Parameter
Initial
Parameter Prediction Experimental
Level P3Q2R4S3 P3Q1R3S3 P3Q1R3S3
Wear 33.86 13.86
COF 0.052 0.125
Grade 0.782 0.861 0.831
Improvement of grey
relational grade=0.062
significant than the dry sliding behavior above 500 m
[17]. Hence, a confirmation test is carried out to check
the accuracy of the analysis after optimizing the pro-
cess parameters. The comparison of experimental grey
relational grade predicted grey relational grade and the
initial grey relational grade is shown in table 6. It is
observed that the predicted tribological parameter of
P3Q1R3S3 shows an improvement of 6% than the 1st
ranked grey relational grade on the L16 orthogonal
array.
According to the grey relational analysis, it was
noted that the sliding distance is insignificant to the
tribological behavior. Hence, the detailed tribological
analysis was conducted with different loads (10, 20,
and 30 N) and sliding velocities (0.4, 0.6, and
0.8 m. s−1) for a constant sliding distance of 2000 m.
Three sets of experiments of Tribological tests were
conducted on the age hardening processed AZ31B Mg
composites, the evaluated average wear rates with
standard deviations were plotted concerning the var-
ious sliding speeds with different loading condition, as
shown in figures 6(a)–(c). It was ascertained that the
wear rate of age hardening processed AZ31 Mg com-
posites were lower than the wear rate of monolithic
age-hardening processed AZ31 Mg alloy. Also, the
wear rate of heat-treated (T6) samples offered a
reduced wear rate compared to the as-cast condition
[18]. This may be due to the following reason, (a)
enhancement of load-bearing capacity through the
presence of hard CaB6 particles in the matrix, as it can
protect the composites from surface damages, (b)
Improved mechanical properties by the refined pre-
cipitates, and (c) An increased volume of the second-
ary precipitates is providing the additional load-
bearing capacity against the sliding wear. However, the
wear rate of monolithic alloy offered a reduced wear
rate than the composites at 10 N load with 0.6 m. s-1
sliding velocity (figure 6(b)). This may be owing to the
development of an oxide layer on the pin surface. The
presence of this oxide layer has restricted the true
metallic contact between the two sliding surfaces and
thereby improving the wear resistance. However, the
formation of the oxide layer is delayed while compared
with the monolithic alloy due to the presence of CaB6
(oxide resistant) particles.
Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
Figure 6. The evaluated wear rate of T6 processed Mg composites for different sliding velocities (a). 0.4 m. s-1, (b). 0.6 m. s−1, (c).
0.8 m. s−1.
On further increasing the load and sliding velocity
to 30 N and 0.8 m. s−1, the wear rate gradually
increased for age hardening processed AZ31 Mg com-
posites due to the breakage of the oxide layer. The bro-
ken oxide layers (grainy) acted as third body particles,
which severely damaged both pin and disk surfaces.
Among different weight percentages, the wear rate of
age hardening processed AZ31 Mg composite with
3 wt.% of CaB6 particles showed a higher wear resist-
ance than the other composites. This higher wear
resistance is attributed due to the better mechanical
locking effect on the reinforced particle and
matrix [13].
To further discuss the wear mechanism of age
hardening processed AZ31 Mg composite (0 and
3 wt.% of CaB6), the obtained SEM image of the wear
track is depicted in figures 7–8. It was observed that
there were five different wear mechanisms (abrasion,
adhesion, delamination, plastic deformation, and oxi-
dation) exhibited for age hardening processed AZ31
Mg composite, indicating the mixed-mode (more
than one) wear mechanisms. Amongst, the delamina-
tion wear mechanism was the dominant wear mech-
anism than the other composites. Several narrow
grooves and scratch marks were observed parallel to
the sliding direction on the pin surfaces under low
load sliding, shown in figures 7(a)–(b). This feature
8
Seenuvasaperumal P et al
can be often linked with the abrasive wear mechanism,
which is caused by the plough and micro-cutting of
hard asperities on the counter-face, or the detached
particles that are removed from the disk or pin surface
and then retain at the surface contact [13]. However,
the depth of grooves was smaller in age hardening pro-
cessed AZ31 Mg composite compared to the age-hard-
ening processed AZ31 Mg alloy.
This indicates that the increased surface hardness
due to the age-hardening process could restrict the
deep penetration of hard asperities. Also, the uniform
distributions of the finer precipitates have increased
the load-bearing capacity and prevent surface damage
significantly. These results were frequently recognized
as a predominant wear mechanism of magnesium
alloys at low load sliding wear. As the load was
increased to 20 N, a shallow delaminated crater was
appeared on the worn-out pin surface indicating the
delamination wear mechanism (figures 8(a)–(b)).
This was attributed to the higher surface and subsur-
face deformation in age hardening processed AZ31 Mg
alloy at a higher load. Also, in composites, the load
concentration has occurred around the particle and
cluster zone which facilitates the nucleation of voids/
cracks. The nucleation and propagation of cracks
beneath the surface were triggered by provoking plas-
tic strain which was attributed to the normal and the
Surf. Topogr.: Metrol. Prop. 9 (2021) 015031 Seenuvasaperumal P et al

Figure 7. FESEM observation on the age hardening processed AZ31 Mg composite worn-out pin surface under 10 N load with 0.4 m. s−1
(a). 0 wt. % of CaB6, (b). 3 wt. % of CaB6. (c and d ) Corresponding wear debris with elemental mapping.

Figure 8. FESEM image of age hardening processed AZ31 Mg composite worn-out pin surface under 20 N load with 0.6 m. s−1 (a) 0 wt. %
of CaB6 and (b) 3 wt. % of CaB6. (c) and (d) Corresponding wear debris with elemental mapping.

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Figure 9. FESEM image of the collected wear debris under 30 N load with 0.8 m. s−1 (a) 0 wt.% of CaB6 and (b) 4 wt.% of CaB6.
tangential forces. As a result, the growth of cracks grow
was extend to the pin surface and leading to the
detachment of wear layers (plate-like sheets), as shown
in figures 8(c)–(d). Das et al. described that the earlier
existence of subsurface cracks can also contribute to
this delamination. Consequently, such a type of wear
mechanism (delamination) has been restricted for the
age-hardening processed AZ31 Mg composite with 2
and 3 wt.%.
When the applied load is increased to 30 N, the
delaminated craters become wider and deeper, denot-
ing the severity of the delamination, as shown in
figures 9(a)–(b). It also suggests the transition of wear
from mild to severe. It is attributed to a reduction in
the ductility of the composites in age hardening pro-
cessed condition. This attainment of subsurface plastic
strain condition has led to the surface softening [19]
and hence, the wear rate is higher for the age-hard-
ening processed AZ31 Mg composite at 30 N. How-
ever, the transition regime was varying between the
monolithic AZ31 Mg alloy and the composites which
are attributed to the reinforced particulates. The sur-
face of the age-hardening processed AZ31 Mg alloy is
much smoother than that of the age-hardening pro-
cessed AZ31 Mg composite, as shown in figure 8(a). As
a result, the formerly damaged locations on the surface
can be easily replenished by the plastic deformation,
which would diminish the probability of sequential
surface destruction. Also, it was believed that the sec-
ondary phase (Mg17Al12) has a low melting point
(∼250 ºC), which can readily soften and coarsen as
temperature increases [19]. So this could have
also caused the strength reduction and an inability to
resist sliding wear for the Mg-CaB6 composites.
From the wear debris analysis (figures 8(c)–(d) and
figures 9(a)–(b)), it is also concluded that the size
of the removed wear particles was increasing with the
load condition. The majority of wear debris resembles
chips (continuous and discontinuous) and grainy
indicating the existence of abrasive wear. In addition
to this, sheet-like debris was also reported for the
age-hardening processed AZ31 Mg composite at
high load conditions due to the severe delamination.
10
Seenuvasaperumal P et al
From the wear characterization, it reveals that T6 trea-
ted alloy exhibited could generate sheet-like debris
and improves the wear transition from severe to mod-
erate wear.
4. Conclusion
Age hardening process was conducted in the as-cast
AZ31 Mg composites using ASTM standard B 661-06
and following major conclusions were drawn,
• The age hardening process has induced the formation
of secondary precipitates (Mg17Al12 and Al8Mn5) in
AZ31B Mg alloy and composites. Also, the grain sizes
were refined considerably and located in the junction
of triple grain boundaries with the addition of CaB6
particle and age hardening process.
• Age hardening processed Magnesium composite
(4 wt.%) microhardness was increased by 15% as
compared to the age-hardening processed mono-
lithic alloy due to the refined microstructure. Also,
the ultimate tensile strength was increased by 65%
as compared with monolithic alloy. The fractured
surfaces revealed the shear bands in a monolithic
alloy and shear bands and brittle fracture for age
hardening processed AZ31 Mg composite.
• A remarkable wear rate reduction was obtained for
the age-hardening processed AZ31 Mg composite
compared to the age-hardening processed AZ31 Mg
alloy. The enhancement of load-bearing capacity,
improved mechanical properties and increased
volume of the secondary precipitates has consider-
ably improved the wear resistance of age hardening
processed AZ31 Mg composite.
• The presence of sheet-like debris has evidenced the
wear transition from severe to moderate wear.
However, still above 30 N, the delaminated craters
to become wider as well as deeper, indicating the
rigorousness of delamination wear and hence this
can be controlled in the future by optimizing the
suitable parameter of the heat treatment process.
Surf. Topogr.: Metrol. Prop. 9 (2021) 015031
Acknowledgments
The Authors would like to express their sincere thanks
to the Engineering design division, Department
of Mechanical Engineering, CEG Campus, Anna
University, Chennai-600025 for providing the research
facility to complete this research work successfully.
Data availability statement
All data that support the findings of this study are
included within the article (and any supplemen-
tary files).
ORCID iDs
Seenuvasaperumal P https://orcid.org/0000-0002-
4071-0168
A Elayaperumal https://orcid.org/0000-0003-
4182-1473
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