Tribology International 111 (2017) 1825

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Inuence of calcium hexaboride reinforced magnesium composite for the MARK

mechanical and tribological behviour

P. Seenuvasaperumala, , A. Elayaperumala, R. Jayavelb
a
Department of Mechanical Engineering, Engineering Design Division, CEG Campus, Anna University, Chennai 600025, India
b
Center for Nanoscience and Technology, Anna University, Chennai 600025, India

A R T I C L E I N F O A BS T RAC T

Keywords: The eect of calcium hexaboride (CaB6) reinforced magnesium metal matrix composite (Mg-MMC) for
Magnesium composite mechanical and tribological behavior have been investigated. Fabrication of the Mg-MMC was done by the
Calcium hexaboride squeeze casting process using the bottom pouring stir casting furnace. Mechanical properties such as tensile
Mechanical property strength and hardness of the composites were analyzed. The dry sliding wear behavior of the pure Mg and the
Tribological property
composites was evaluated in the pin-on-disk tribo-meter using SAE52100 bearing steel disk at room
temperature. Improvement in the mechanical property was found in CaB6 reinforced Mg-MMC as compared
with pure Mg. A signicant fact was that, addition of CaB6 enhanced the wear resistance of Mg-MMC, revealing
the delamination wear mechanism is dominant from other wear mechanisms.

1. Introduction
In recent years, extensive investigations have been done on light-
weight materials in the automobile domain for increasing fuel economy
[1,2]. In general, Magnesium, Aluminum and Titanium are considered
as lightweight materials for structural applications. Among them, Mg is
considered as an essential candidate because of its high specic
strength and easy recyclability [3]. But, the utilization of pure Mg has
certain limitations such as poor ductility, thermal stability, wear
resistance, creep and corrosion resistance etc. Such limitations can
be overcome through use of various methods such as alloying and
composite processes, which form new precipitates and the benecial
eect on hard reinforced particle [410]. However, studies in the Mg
based alloys and composites for development of tribological behavior
have not been much to be talked. In recent years, many reports have
been published to explain the tribological behavior of Mg based alloys
and composites. Particularly, the hard particles present in Mg-based
composite provide improved wear resistance compared to pure Mg
[1118].
CaB6 belongs to the 2 A group alkaline earth boride [19]. It has
favorable properties such as low density (2.45 g cm3), high melting
point (2235 C), low coecient of thermal expansion (6.2106 C1),
high hardness (27 GPa), chemical stability and good wear resistance in
a corrosive environment [2022]. Previous studies have proved that
the addition of CaB6 to metals and non-metals provides improved
mechanical properties [23,24]. However, there are not many reports as
the subject of the CaB6 reinforced composites for mechanical and
tribological behavior.
On the other hand, the fabrication processes also inuence the
mechanical and tribological behavior. Squeeze casting is one of the
fabrication technique to promote the solidication under the high
pressure. The application of squeeze pressure has the possibility of
recrystallization, grain renement and porosity reduction, resulting
in improvement of mechanical and tribological behavior [2527].
Here, an attempt has been made to prepare Mg based composites
by reinforcing 2 wt% of CaB6 using squeeze casting process. The
prepared samples were mechanically polished and tribological tests
were conducted under dierent loads (10, 20 and 30 N) and
velocities (0.4, 0.6 and 0.8 m s1) for a constant sliding distance of
2000 m. Optical microscope (OM) was used for revealing the grain
structure of the etched surface. Mechanical tests were conducted and
enhancement of mechanical property was estimated as a function of
hardness and tensile strength. Essentially, the wear mechanisms
were investigated as a function of wear rate and co-ecient of
friction using worn-out surface morphology. Fractography and sur-
face morphology of the worn out surfaces were observed using
Scanning electron microscope (SEM) analysis. Energy dispersive
X-ray (EDX) analysis was used for analyzing the worn out debris to
conrm wear mechanism.

Corresponding author.
E-mail addresses: seenumeed@gmail.com (P. Seenuvasaperumal), profelaya@gmail.com (A. Elayaperumal), rjvel@annauniv.edu (R. Jayavel).

http://dx.doi.org/10.1016/j.triboint.2017.02.042
Received 9 November 2016; Received in revised form 3 February 2017; Accepted 26 February 2017
Available online 28 February 2017
0301-679X/ 2017 Elsevier Ltd. All rights reserved.
P. Seenuvasaperumal et al. Tribology International 111 (2017) 1825

2. Experimental details 2.4. X -Ray diraction Studies

2.1. Materials and processing
A pure Mg ingot with 99% purity was purchased from Vaishnavi
castings Ltd, Chennai, India. This is the matrix material, it was cut into
50 mm x 50 mm x 20 mm billets using a band saw. The CaB6 with a
mean particle size of 50 mesh and purity of 99.5%, was supplied by Alfa
aeser, USA. A bottom pouring stir casting furnace (made by swam
equipment Ltd, Chennai, India) was used for the composite fabrication
process. The Mg billets were melted in a steel crucible at 700 C in an
electrical resistance furnace. A productive gas atmosphere of argon and
sulfur hexauoride in the ratio of 5:1 was maintained. The matrix
molten slurry was stirred at 450 rpm for 2 min using a twin blade
impeller inclined at 45. The mild steel blade was coated by zirtex to
avoid sticking. After stirring, the slags were removed from the matrix
molten slurry. In order to remove the moisture and increase wett-
ability, 2 wt% of reinforced particles (CaB6) was preheated in the box
furnace at 400 C for 2 h.
The preheated reinforced CaB6 particles were then mixed in to the
matrix molten slurry and stirred at 450 rpm for 15 min for achieving
uniform distribution. The molten composite was then poured into the
mold of 50 mm diameter and 250 mm height by the bottom pouring
technique. Before pouring, the mold was preheated to 250 C for 1 h.
Squeeze casting which is similar to the above technique together with
squeeze pressure (120 MPa) was applied at 300 C for 2 min during
solidication. The squeeze pressure was applied using a hydraulic press
with a capacity of 50 t.
The crystalline structure of pure Mg and Mg-MMCs were analyzed
by using XRD (Shimadzu, Japan). The X-ray wavelength was
=1.5405 with a scan speed of 2 min 1. The joint committee on
powder diraction standards (JCPDS) was used for analyzing the XRD
results of both pure Mg and Mg-MMC samples.
2.5. Hardness test
The hardness of pure Mg and Mg-MMCs were evaluated to
determine the eect of reinforced particles at room temperature.
Vickers micro-hardness test (Buehler) was used with a load of 50 gf
for 15 s dwell time. Ten measurements were processed at ten dierent
locations on the same sample to avoid the eect of indenture resting on
hard reinforced particles.
2.6. Tensile test
The universal testing machine (Instron UTM 50 kN, model: 3369)
was used for studying the tensile behavior of pure Mg and Mg-MMC
materials at room temperature with a minimum cross head speed of
1 mm. min1. Prior to taking the tensile test, the composite specimens
were machined as per the ASTM: E8 Standard. Three samples were
used for each composite to ensure a reproducibility. The surface
morphology of tensile fractured surface was observed by using a
Hitachi scanning electron microscope for analyzing fracture behavior.

3. Tribological test
2.2. Density and porosity
The tribological test was carried out at room temperature by using a
The densities of pure Mg and its composites were determined using DUCOM pin-on-disk tribo-meter, as schematically shown in Fig. 1.
the Archimedes principle under ASTM standard D3800. Eq. (1) was Each pin sample has a diameter of 12 mm and length of 50 mm. The
used for calculating the density of the materials. pin sample slides on the SAE 52100 bearing steel (63 HRC) disk with a
WaX Dw diameter of 55 mm and a thickness of 10 mm. The same surface
Da = roughness was maintained on the disk and the pin samples. The
Wa Ww (1)
tribological experiments were conducted at room atmospheric condi-
where, Da - Actual density of the specimen, Wa - weight of the specimen tion with various loads (10, 20 and 30 N) and sliding velocities (0.4, 0.6
in air, Dw - water density, Ww - weight of the specimen in water. and 0.8 m. s1) for a constant sliding distance of 2000 m. The wear rate
Eq. (2) was used to calculate the porosity of the composite material, was calculated by mass loss method (Eq. (3)), and coecient of friction
was measured by the software which is congured with DUCOM pin-
Dt Da on-disk tribo-meter.
Percentage of porosity = X 100%
Dt (2)
mass of the pin before the wear test mass of the pin
where, Dt - Density of pure Mg.
after the wear test
The weight of the samples was obtained using an analytical wear rate = g m 1
total sliding distance
weighing balance (wensar, India, accuracy of 0.00001 g). The
theoretical density of the composites was calculated on the basis of (3)
the assumption of full density. All the calculations were done using the
rule of mixture.

2.3. Microstructure observation

Microstructural observations such as grain structure and interfacial

integrity between Mg and CaB6 were analyzed by using the metallo-
graphic polished samples. The polishing was carried out with various
grid ranges (240, 600 grid SiC sand paper, 6 m, 1 m diamond
suspension and nally colloidal silica) by using mechanical polisher.
For every grid range, the samples were initially washed with water and
ultra-sonication was then performed in ethanol for 2 min. The polished
samples were immersed in acetic - picral etchant (6 g picric acid, 10 ml
acetic acid, 70 ml ethanol and 20 ml water) for etching until the
formation of brown lm on the surface. It was subsequently washed
with ethanol to get clear grain structures. Olympus DP 10 microscope
was used for analyzing the grain structure. Fig. 1. Schematic representation of pin- on-disk tribometer.

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P. Seenuvasaperumal et al. Tribology International 111 (2017) 1825

Fig. 3. XRD diractograms of pure Mg, Mg composite and Mg squeeze composite.

initially grown Mg grains, which restrict further grain growth.

Reduction in the grain size was also observed in the Mg squeeze
composite as compared to the as-cast Mg composite. It is due to the
applied squeeze pressure [29]. The as-cast Mg composite shows both
visible porosity and a void between matrix and reinforced particles.
However, in the squeeze composite the occurrence of porosity and
visible void are minimal because of the applied squeeze pressure.
The interfacial reaction between matrix and reinforced particles is
conrmed through XRD analysis, the XRD patterns obtained are
shown in Fig. 3. It reveals the absence of reactive phases between the
matrix and the reinforced material. This is evidenced by a comparison
with the JCPDS card number for Mg and CaB6, the JCPDS card
numbers are 35-0821 and 03-0662 respectively. There are three main
peaks of 2 =32, 34 and 36 corresponding to the prism (10-10),
basal (0002) and pyramidal (1011) planes of pure Mg crystal
respectively [7]. Addition of reinforced particles to Mg reduces peak
intensity and it also causes shifts in the peak position (indicated by
arrow in Fig. 3) as compared to the pure Mg. However, the random
orientation was changed in squeeze composite by the squeeze pressure
[25].

4.2. Eect of CaB6 on density and porosity

Variations in density and porosity of the fabricated composite are

Fig. 2. OM image of grain structures (a). Pure Mg, (b). Mg as-cast composite, (c). Mg shown in Table 1. The experimentally obtained density values of the
squeeze composite.
composites are higher than that of the pure Mg. This is due to the high
density of reinforced particles relative to that of the matrix material.
Every pin sample was weighed before and after the test using the
The results indicate reduction in porosity and increased density in the
same analytical weighing balance for calculating the exact mass loss.
squeeze composite compared to as-cast composite. This can be
Three sets of experiment conducted and the obtained results have been
attributed to the squeeze pressure applied on the as-cast composite
plotted with standard deviation. The worn out surface of the samples
[29].
was cleaned with ethanol before weighing. The worn out pin and disk
surface morphology were observed by using SEM for nding the wear
Table 1
mechanisms. Also, SEM attached EDX was used for analyzing the Results obtained from pure Mg, Mg as-cast and squeeze composites.
chemical composition present on the worn out wear debris to conrm
the wear mechanisms. Samples Theoretical Experimental Porosity Hardness UTS Strain
density density (50 gf)
(g cm3) (g cm3) (%) Hv (MPa) (%)
4. Result and discussions
Pure Mg 1.740 1.725 0.86 32 1.0 94 2.10
4.1. Eect of CaB6 on microstructure Mg as- 1.758 1.720 2.16 39 2.5 106 1.75
cast
com-
The mechanically polished surface of the composite specimens posite
visually reveal uniform distribution of reinforced particles in the matrix Mg 1.758 1.745 0.74 45 1.0 143 4.50
material. The observed OM images [Fig. 2(a)(c)], Mg composite squee-
ze
samples show reduced grain size compared to pure Mg, due to the
com-
presence of CaB6 particles. During solid state cooling, the hard posite
reinforced particles were pushed in to the intergranular region of

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P. Seenuvasaperumal et al. Tribology International 111 (2017) 1825

4.3. Eect of CaB6 on mechanical property

Hardness test was conducted on the pure Mg, as-cast and squeeze
Mg composite in Vickers micro-hardness tester for studying the eect
of CaB6 in Magnesium matrix. Hardness values evaluated from the
pure Mg, as-cast and squeeze composite, are presented in Table1. Both
as-cast and squeeze Mg composites show higher hardness than pure
Mg due to the reinforced particles. The reinforced particles restrict the
local deformation of the matrix materials during indentation, and also
rened matrix microstructure [10]. However, Mg squeeze composite
oers higher hardness due to reduced porosity and grain size than Mg
as-cast composite [26].
The tensile test was conducted using a UTM machine and the
results obtained are presented in Table1. The tensile strength of the as-
cast and squeeze composites shows improved behavior compared to
pure Mg. The presence of hard reinforced particles can increase the
dislocation density in the matrix, which is due to the mismatch of co-
ecient of thermal expansion (Mg 27106 C1, CaB6
6.2106 C1). When the tensile loading is applied the CaB6 acts as
an obstacle to the dislocation motion. Therefore, the additional load is
needed to continue the motion of dislocation to destroy these obstacles,
showing improved strength. The Mg squeeze composites show im-
proved ductility compared to the pure Mg. This is attributed to the
presence of CaB6 and it may activate the non-basal slip systems in the
matrix [3034]. The reduced ductility in the Mg as-cast composite is
due to the presence of porosity and voids between the reinforced CaB6
particles and Mg matrix. These pores and voids act as load concentra-
tion sites followed by nucleation of crack that propagates to failure.
The fractured surfaces were analyzed for nding the fracture
behavior by using SEM. The observed images are shown in Fig. 4(a)
(c). It was clearly observed that the presence of brittle cleavage fracture
on the pure Mg tensile fractured sample [Fig. 4(a)]. Straight lines on
the fractured surface morphology indicate the evidence of basal plane
slip [28]. Similarly, for both the composites, the fractured surface
shows mixed mode of fracture [Fig. 4(b) and (c)]. Due to the activated
non-basal slip systems in the matrix, many micro-dimples were present
on the fractured surface. However, the size of the observed dimples in
the squeeze composite is smaller than the as-cast Mg composite. This
can be attributed to the squeeze pressure.

4.4. Eect of CaB6 on tribological behavior

Three set of experiments of Tribological tests were conducted on

the pure Mg, as-cast and squeeze Mg-MMCs, and the average wear
rates with standard deviations obtained were plotted with respect to
the various sliding speed with dierent loading condition, as shown in
Fig. 5(a)(c). The wear graphs show the Mg-MMCs oering a lower
wear rate compared to pure Mg. This may be due to the following
reasons, (a) The presence of hard reinforced CaB6 particles can
enhance the higher load bearing capacity and protect the sliding
surface from damage, (b) Reduced grain size and improved mechanical
properties could improve wear resistance, (c) Reduced pores, voids in
the squeeze composite may be the additional reasons for the reduced
wear rate compared to the as-cast composite. In contrast, 20 N loading Fig. 4. SEM images of the Fractured surfaces for the magnesium composites (a). Pure
under 0.6 and 0.8 m. s1 sliding velocity condition, pure Mg oers Mg, (b). Mg as-cast composite, (c). Mg squeeze composite.
reduced wear rate compared to the Mg-MMCs. This may be due to the
formation of oxide layer on the pure Mg pin surface. This oxide layer conditions. With increase in the sliding load and speed, the coecient
can avoid the true metallic contact between the sliding surfaces, which of friction and wear rate also increased. In contrast, for the sliding load
controls the wear rate [11]. When the load and velocity were increased 20 N, the coecient of friction decreased with an increase in sliding
to 30 N and 0.8 m. s1, the wear rate increases due to the oxide layer speed. It could be also related to the oxide layer formation and growth
breakage. The broken oxide layers (hard MgO particles) act as a third on the pin surface. This oxide layer could also to grow with further
body abrasion, which damages both pin and steel counterface surfaces. increase in the load. This oxide layer cannot resist the cyclic load and
The average co-ecient of friction in the tribological tests obtained breaks the oxide layer by the action of friction [35]. Once the oxide
were plotted with respect to the various sliding speed and dierent layer breaks, true metallic contact occurs between the sliding bodies
loading conditions, as shown in Fig. 6(a)(c). The coecient of friction and raise the wear rate. This is likely a quasi-periodic process [35]. In
was found directly related to the wear rate of the pure Mg in all sliding Mg-MMC, there was a non-linear consequence between wear rate and

21
P. Seenuvasaperumal et al.
Fig. 5. Wear rate of dierent load with dierent velocities (a). Pure Mg, (b). Mg as-cast
composite, (c). Mg squeeze composite.
coecient of friction. It may be due to the presence of hard reinforced
particles, non-uniformity of thermal equilibrium between the sliding
surfaces.
4.5. Microstructural study of the worn-out surfaces
The SEM images of worn-out pin and disk surface in dierent
sliding condition and the corresponding wear debrises were analyzed
for evaluating the wear mechanism. The squeeze composite worn out
pin and disk surfaces are shown in Fig. 7(a) and (b). Which show many
scratches and grooves on the surface, which are parallel to the sliding
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Tribology International 111 (2017) 1825
Fig. 6. Co-ecient of friction of dierent load with dierent velocities (a). Pure Mg, (b).
Mg as-cast composite, (c). Mg squeeze composite.
direction. It is due to the abrasive wear [36,37], resulting from the hard
asperities of the steel counterface or the hard CaB6 of the composite.
The fractured hard CaB6 particles are stuck on the steel counterface
grooves and scratches are made on the pin surface. Similarly, the
fractured hard asperities from the steel counterface caused by hard
reinforced CaB6 particles that stuck between pin and counterface act as
a third body and cause third body abrasive wear on both pin and
counterface surface. The collected worn-out wear debris shows ribbon
like fragments of Mg material, as shown in Fig. 7(c). It is due to the
occurrence of abrasive wear.
P. Seenuvasaperumal et al.
Fig. 7. Squeeze composite under the sliding condition of 10 N load, 0.8 m. s1 speed (a).
worn out pin surface, (b). worn out disk surface, (c). Elemental mapping of collected wear
debrises.
The same sliding condition of worn out pin and disk surface of pure
Mg are shown in Fig. 8(a) and (b). It shows mixed wear as grooves and
prows as the indication of abrasive and adhesive wear, respectively. The
presence of prows is attributed to the sliding speed along with the
frictional heating that causes the pin surface becomes softer. Then, the
soft pin materials were transferred from the pure Mg pin surface to the
steel counterface surface. As a result, the grooves on the counterface
surface were lled by pure Mg material and gained weight, greater than
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Tribology International 111 (2017) 1825
Fig. 8. Pure Mg under the sliding condition of 10 N load, 0.8 m. s1 speed (a). worn out
pin surface, (b). worn out disk surface.
seen before the test. The surface roughness of the disk rubbed the
materials from the softer side and lled in their grooves. Also, pure Mg
pin sample show smaller patches of white color on the surfaces under
higher sliding speed, suggesting the formation of oxide wear. When the
load increases from 10 N to 20 N, pure Mg pin surface fully covered
with white color, as shown in Fig. 9(a). For repeated sliding, the
threshold sliding speed concurrent with the frictional heating causes
oxidation after the asperities reach ash temperature for oxidation. A
thin oxide layer is formed on the pin surface and it prevents the true
metallic contact, oering lower wear rate [38,39]. When the load
increases, these oxide layer is fractured causing a true metallic contact,
which results in the increased wear rate. The EDX analysis of collected
wear debrises shows the presence of both Mg and oxygen. This suggests
the formation of magnesium oxide [11]. In composite samples,
oxidative wear occurs at higher sliding load and speed condition. It is
due to the thermal equilibrium between the reinforced CaB6 particles
and the Mg matrix which delays the oxidation.
Higher sliding load and speed of the materials were delaminated
from the pin surface resulting in micro cracks and cavitation on the Mg
squeeze composite pin surface. It is due to the delamination wear [40],
as well as fatigue related wear mechanism. The subsurface deformation
occurred on the pin surface followed by crack initiation, propagation
and detachment of bulk material due to the cyclic load. Details of the
cavitation on the pin surface, are shown in Fig. 10(a). These detached
pin materials (wear debris) are akes or thin sheets, as shown in
Fig. 10(b). This type of wear mechanism aects the pin surface more
severely than other wear mechanisms. Nevertheless, the wear rate of
P. Seenuvasaperumal et al.
Fig. 9. Pure Mg under the sliding condition of 20 N load, 0.8 m. s1 speed (a). worn out
pin surface, (b). Elemental mapping of collected wear debrises.
composite was lower than pure Mg due to the presence of hard
reinforced particles.
5. Summary
The CaB6 reinforced Mg-MMCs were demonstrated for the rst
time on the mechanical and tribological behaviours in which the four
major characteristics have been summarised, as follows:
1. The prescence of CaB6 in Mg-MMC, eects the reduced grain size in
the composites compared to pure Mg. The grain size of the squeeze
Mg-MMC is smaller than the as-cast Mg-MMC, because of the
applied squeeze pressure.
2. Improved mechanical properties were obtained in the composites
because of the eect of hard reinforced CaB6 particles. Hardness was
enhanced by the reinforced CaB6 particles, which constrained the
local deformation during indentation. The mechanical strength
improved due to the reinforced CaB6 particles, which interrupted
the dislocation motion during straining. Also, the ductility improved
by additional slip system activated by the incorparation of particles.
However, the ductility of the as-cast Mg-MMC was lowered due to
the presence of porosity and voids.
3. Lower wear rates were obtained for the composites compared to
pure Mg for all sliding conditions except 20 N of load under 0.6 and
0.8 m. s1. The hard CaB6 particles could absorb high load bearing
capacity under dynamic loading, preventing the sliding pin surface
from damage.
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Tribology International 111 (2017) 1825
Fig. 10. Squeeze composite under the sliding condition of 30 N load, 0.8 m. s1 speed
(a). worn out pin surface, (b). Elemental mapping of corresponding wear debrises.
4. The worn out pin surface, steel counterface and collected wear
debrises analysis corm the wear mechanisms such as abrasive,
adhesive, oxidative and delamination wear. In the present study, the
delamination wear mechanism was the dominant wear mechanism
from the other wear mechanisms in the Mg-MMC.
Acknowledgement
The Authors would like to express their sincere thanks to the Anna
University, Chennai-600025 (Grant no. CR/ACRF/2014/6) 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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