Available online at www.sciencedirect.

com

Journal of Magnesium and Alloys 8 (2020) 780–792

www.elsevier.com/locate/jma

Full Length Article

Study on effect of TiB2 reinforcement on the microstructural and
mechanical properties of magnesium RZ5 alloy based metal matrix
composites
Arabinda Meher∗, Manas Mohan Mahapatra, Priyaranjan Samal, Pandu R. Vundavilli
School of Mechanical Sciences, Indian Institute of Technology Bhubaneswar, Odisha 752050, India
Received 8 November 2019; received in revised form 3 March 2020; accepted 23 April 2020
Available online 6 June 2020

Abstract
A self-propagating high-temperature synthesis route is adopted for the fabrication of TiB2 -reinforced magnesium RZ5 alloy-based in-situ
metal matrix composites. Ti-B is used according to the appropriate stoichiometry to obtain 4, 6 and 8 wt.% TiB2 reinforcements. The base
alloy and cast composites are solutionised to enhance the mechanical properties of the materials. A microstructural study of the composites
is carried out using optical microscopy and field emission scanning electron microscopy (FESEM) and revealed near-uniform distribution of
TiB2 particles in the magnesium RZ5 alloy matrix. X-ray diffraction revealed the formation of the TiB2 reinforcement along with the transient
phase TiB and MgB7 . The hardness of the RZ5 alloy-based composites increases by 7.12%, 17.06% and 32.07% with the addition of 4, 6
and 8 wt.% TiB2 reinforcements, respectively. The ultimate tensile strength of the as-cast composite increases by 30.47% with the addition
of 8 wt.% TiB2 . The tensile strength and ductility of the materials is improved by using the solutionising heat treatment. The heat-treated
composite containing 8 wt.% TiB2 results in an ultimate tensile strength of 178.7 MPa. The tensile fracture surfaces are analysed using
FESEM. The wear loss of the materials decreased from 25.826 mm3 to 22.949 mm3 by the adding 8 wt.% TiB2 for the sliding distance of
2000 m. Micrographs of the worn surfaces obtained from FESEM of both the base alloy and composites are also studied which indicate
delamination, wear groove and oxide formation.
© 2020 Published by Elsevier B.V. on behalf of Chongqing University.
This is an open access article under the CC BY-NC-ND license. (http://creativecommons.org/licenses/by-nc-nd/4.0/)
Peer review under responsibility of Chongqing University

Keywords: In-situ composites; Magnesium RZ5 alloy; Heat-treatment; Tensile strength; Wear resistance.

1. Introduction strength for structural applications and high strength-to-weight

Metal matrix composites (MMCs) are being increasingly
used in industry because of their higher strength, stiffness
and wear resistance compared to other conventional mate-
rials [1]. The desired properties of the composites can be
achieved through the proper combination of the matrix and
the reinforcement by different fabrication processes. Different
matrix materials used for the fabrication of MMCs include
aluminium, magnesium, copper, titanium, iron and their al-
loys [2,3]. Cast magnesium alloy-based MMCs are used in
the automobile and aerospace industries due to their high-
∗ side a liquid melt by an exothermic chemical reaction, which
Corresponding author.
E-mail address: am39@iitbbs.ac.in (A. Meher).
ratio. A literature study reveals that replacing the aluminium
parts with magnesium can increase fuel efficiency by 20–
30% in automobiles [4]. Particulate-reinforced MMCs can
be processed by various processing routes, such as stir cast-
ing [5,6], squeeze casting [7], preform infiltration [8], pow-
der metallurgy [9,10] and self-propagating high-temperature
synthesis (SHS) reactions [11,12]. Composites developed by
ex-situ methods are generally characterised by low interfa-
cial bonding strength and poor wettability, which may result
in interfacial defect propagation. Hence, ex-situ composites
are not preferred for fluctuating or cyclic loading conditions.
In the in-situ process, the reinforcement is synthesised in-
is thermodynamically stable and less degradable at elevated

https://doi.org/10.1016/j.jma.2020.04.003
2213-9567/© 2020 Published by Elsevier B.V. on behalf of Chongqing University. This is an open access article under the CC BY-NC-ND license.
(http://creativecommons.org/licenses/by-nc-nd/4.0/) Peer review under responsibility of Chongqing University
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
temperatures [13]. Researchers have endeavoured to develop
TiC-, TiB2 -, SiCNO-, ZrB2 - and carbon nanotube-reinforced
magnesium-based in-situ MMCs using different techniques
for many aerospace and automobile applications [14,15].
Very few investigators have worked on self-propagating
high temperature synthesis route for in-situ fabrication of TiB2
reinforced magnesium matrix composites. TiB2 is considered
as one of the most potential reinforcement due to properties
like high melting point, high hardness, good thermal stabil-
ity and excellent wear resistance [16]. Matin et al. fabricated
the TiB2 reinforced magnesium-based MMCs using potassium
boron tetrafluoride (KBF4 ) and potassium titanium hexafluo-
ride (K2 TiF6 ) salt. When the salt was mixed and stirred at
450 rpm after melting the magnesium (above 1023 K), re-
sulted in formation of TiB2 by a series of reactions [17].
Peng et al. also conducted the chemical reaction between
KBF4 and K2 TiF6 salt along with aluminium to fabricate Al-
20 wt.% TiB2 master alloy. The master alloy and alloying
elements were added to molten magnesium at 750°C to fab-
ricate TiB2 reinforced magnesium AZ91 based composite. It
was observed that, TiB2 extracted from the master alloy were
uniformly distributed in magnesium AZ91 alloy matrix with
the particulate size of 50-300 nm. Also, the grain refinement
of composites occured due to the presence of TiB2 particle as
it acts as a grain refiner. Ductility of the material along with
other mechanical properties were observed to have improved
[18]. Wang et al. synthesized TiB2 /Mg composite by SHS
route taking Al, Ti and B powders. Preform was prepared by
blending the powders using ball mill for 8 hours followed by
the compaction at 70 MPa and drying of the compact. Preform
was added to the magnesium melt at a temperature of 860°C
which is slightly above the exothermic reaction temperature.
The uniform distribution of TiB2 in magnesium matrix was
observed [19]. Fang et al. fabricated AZ31/TiB2 composite by
SHS reaction using coupled field treatment and noticed that
addition of TiB2 in the magnesium AZ31 alloy matrix acts as
a grain refiner. It was also observed that due to the coupled
field treatment strength as well as ductility of the composite
improved [20].
Studies describing the synthesis of TiB2 -reinforced rare-
earth-based in-situ magnesium matrix composites are rare.
The purpose of the present investigation is to develop in-
situ magnesium RZ5 alloy (Mg-Zn-Zr-RE) based MMCs with
TiB2 reinforcements using SHS reaction. The effect of the
TiB2 reinforcement on the mechanical properties, including
hardness, strength and wear resistance of the magnesium ma-
trix composites is studied. The effect of heat treatment on the
mechanical properties of both the base alloy and cast com-
posites is also investigated.
2. Experimental procedure
2.1. Synthesis of in-situ RZ5-TiB2 composites
In this study commercial grade magnesium RZ5 alloy cast
plate was used as the base material, which was procured from
Foundry and Forge Division, Hindustan Aeronautics Limited
781
Table 1
Elemental composition of magnesium RZ5 alloy
Element Zn Zr Rare earth Mn, Fe, Mg
(Ce) Cu, Ni, Si
Composition (%) 4.25 0.54 1.20 < 0.005 Remaining
Bangalore, India. The elemental composition of the cast mag-
nesium alloy is depicted in Table 1.
To develop the magnesium RZ5 alloy based metal matrix
composites, a coal-fired pit furnace was used and a stirrer ar-
rangement was made with a speed controller. Infra-red tem-
perature reader (Extech - VIR50) was used to measure the
temperature of the molten metal. The schematic representa-
tion of the casting setup is shown in Fig. 1. In this study,
high purity Ti mesh (99 % pure) and boron powder (99.5 %
pure) were used with a molar ratio of Ti: B = 1:2 to develop
the TiB2 reinforced metal matrix composites. The amount of
Ti and B was added according to the stoichiometry of the
required amount of reinforcement (i.e. 4, 6 and 8 wt.%) with
the magnesium RZ5 alloy matrix [21]. The SHS reaction be-
tween Ti mesh and boron powder led to the formation of
TiB2 reinforcement. In order to prevent oxidation, proper ar-
gon shielding was provided throughout the casting process.
The Gibbs free energy for the formation of a solid solution
phase can be determined by the following relations given in
Eq. (1)–(3).
 
◦ J
Ti + B = TiB G = −163176 + 5.85T (1)
mol
 
◦ J
Ti + B = TiB2 G = −284512 + 20.50T (2)
mol
 
◦ J
Mg + 2B = MgB2 G = −92048 + 10.46T (3)
mol
As per the thermodynamics data, the value of Gibbs free en-
ergy (G◦ ) is more negative for TiB2 as compared to that
of TiB and MgB2 . So the probability of TiB2 formation is
more as compared to other phases during the synthesis of
magnesium matrix composites [17].
For casting, the titanium mesh was heated to 1400°C in a
high temperature ceramic crucible at which the mesh structure
gets converted into the powder form. The preheated boron
powder was wrapped in an aluminium foil and was added into
the crucible in an argon protective atmosphere. The mixture
of titanium and boron was stirred continuously for 15 min
to get a uniform distribution. After holding the mixture at
1400°C for about 10 min Ti-B mixture turns into a semi-solid
slurry. Magnesium RZ5 alloy was melted in another crucible
at 750°C. The Ti-B mixture was added to molten magnesium
and stirred continuously for 20 min at 350 rpm. The diffusion
between titanium and boron was initiated at this temperature
[22]. During this period in-situ reaction between titanium and
boron took place inside the magnesium melt which resulted
in the formation of TiB2 . Then the liquid molten composite
was poured into the pre-heated (500°C) steel mould.
782 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792

Fig. 1. Schematic representation of casting setup.

Fig. 2. Schematic representation of the heat treatment process.

Table. 2
Notation of different materials
Sl. No. Materials conditions
1 As-cast base alloy
2 As-cast composite
3 Heat-treated cast base alloy
4 Heat-treated cast composite
As the cast magnesium RZ5 alloy is brittle in nature so
the heat treatment of the base alloy and the cast composites
was carried out as per ASTM B661 – 12 [23]. The schematic
representation of the heat-treatment process of the material is
shown in Fig. 2. The mechanical properties of the materials
were characterized in the following four categories as given
in Table 2.
2.2. Material characterization
For the metallographic study, a standard procedure was fol-
lowed to prepare the samples [24]. Etching of the samples was
done by the etchant acetic picral (10 ml acetic acid + 4.2 g
picric acid + 10 ml distilled water + 70 ml ethanol). To know
Notation the different phase formations during the in-situ synthesis of
ACB the materials, phase analysis of the materials was performed
ACC by using BRUKER D8 Advance x-ray diffractometer with Cu
HTCB Kα (λ = 1.542 Å) radiation. X-ray diffraction was measured
HTCC within the scan range of 10° to 90° with a scan speed of
0.5°/min. Micro-structural characterization of the composites
was done using LEICA DMI3000 M optical microscope and
ZEISS MERLIN Compact field emission scanning electron
microscope (FESEM).
The mechanical behaviour of the base alloy and 4, 6 and
8 wt.% TiB2 -reinforced magnesium matrix composites under
both as-cast and heat-treated conditions was studied. The mi-
crohardness test of the materials was carried out by an Om-
nitech semi-automatic micro-hardness tester applying a load
of 500 gf and a dwell time of 10 s. The indentation was
taken at five different points to obtain the average hardness
value along with the standard deviation. The tensile strength
of the composites was measured using an INSTRON 5982
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
Fig. 3. Schematic representation of wear testing setup.
universal testing machine. The tensile strength test samples
were prepared according to the ASTM E8/E8M – 13a stan-
dard [25]. The tensile test was conducted with a strain rate of
0.1 mm/min. The fracture surface of the tensile test samples
was studied using FESEM. A Charpy test was completed us-
ing a pendulum impact testing machine (Tinius Olsen model
Impact 104). ASTM E23 – 07a was followed to prepare the
samples for the test [26]. The dimensions of the impact test
specimen were 55 × 10 × 10 mm3 with a single-edge v-notch
of 45° with a root radius of 0.25 mm and a depth of 2 mm.
For each composition, four samples were taken to obtain the
average impact strength along with the standard deviation.
The wear rate of the materials was found using a Ducom
TR-20LE-PHM 400 wear testing machine. A schematic rep-
resentation of the wear testing setup is shown in Fig. 3. The
wear test samples were rectangularly shaped with dimensions
of 10 × 10 × 30 mm3 for both the base alloy and composites.
Fig. 4. XRD spectra of magnesium RZ5 alloy and RZ5-TiB2 composites.
783
A dry sliding wear test of the materials was carried out with
a rotating counter body made up of EN31 hardened steel.
The volumetric wear loss of the materials was studied as a
function of reinforcement content and sliding distance. The
volumetric wear loss (in mm3 ) of the materials was measured
from the weight loss of the materials due to the wear test, as
shown in Eq. (4) [27,28]. The microstructural variations on
the wear surfaces of both the base alloy and cast composites
were studied using FESEM.
  weight loss (g)
volumetric wear loss mm3 =   × 1000 (4)
Density mgm3
3. Results and discussions
3.1. Phase analysis
The X-ray diffraction (XRD) phase diagram shown in Fig.
4 shows the presence of the TiB2 phase in the composite. A
few peaks of the TiB2 reinforcement coincide with the peaks
of the magnesium alloy. In addition to TiB2 , a transient phase
of MgB7 and TiB (in the case of 8 wt.% TiB2 ) was also de-
tected in the cast composites. The MgB7 and TiB phase might
have formed during the in-situ reaction of the Ti and B in the
magnesium melt. There was no phase formed between Ti and
Mg, because as per the Mg-Ti phase diagram, no reaction
takes place in this temperature range. As per the thermody-
namics data available for the Gibbs free energy relation, the
probability of formation of the TiB2 phase is higher and it
is a thermodynamically stable phase, since it has the low-
est Gibbs free energy [18]. Thus, TiB2 particles are mostly
distributed in the matrix phase. Along with Mg and the TiB2
phase, other phases of the alloy, like Mg17 Ce and CeZn3 , were
noticed in the XRD spectra. All the major peaks are identi-
784 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792

Fig. 5. Optical micrograph of (a) RZ5 alloy, (b)RZ5-8 wt.% TiB2 .

Fig. 6. SEM micrograph of (a) Base RZ5 alloy, (b) 4 wt.%, (c) 6 wt.% and (8) 8 wt.% TiB2 reinforced magnesium matrix composites.

fied as per the JCPDS database. A few oxide peaks may be
present that cannot be identified by XRD due to their low
intensity.
3.2. Microstructural analysis
Fig. 5 shows the optical micrograph of the base RZ5 mag-
nesium alloy and the RZ5-8 wt.% TiB2 magnesium matrix
composites. It can be noticed that during the SHS process,
several reinforcements develop along the grain boundaries
while others form along the grain. Reinforcements are dis-
tributed near uniformly in the magnesium matrix. Wang et al.
also observed a similar trend during the development of AZ91
magnesium alloy-based TiB2 -reinforced MMCs. In addition,
it was found that the addition of TiB2 in the magnesium ma-
trix improves grain refinement [22].
Microstructural characterisation of the TiB2 -reinforced
magnesium RZ5 alloy-based MMCs was carried out using
FESEM. Fig. 6(a–d) shows FESEM micrographs of the base
RZ5 alloy and 4, 6 and 8 wt.% TiB2 -reinforced magnesium
RZ5 alloy-based MMCs. It was noticed that the reinforce-
ments formed due to the in-situ reaction of Ti-B in magne-
sium melts are of hexagonal or rectangular shape. Similar
microstructure was observed by other researchers during syn-
thesis of (TiB2 -TiC)/AZ91 [29] and TiB2 /AZ31 [30] magne-
sium matrix composite.
The FESEM micrographs reveal the near-uniform distri-
bution of TiB2 reinforcement in the magnesium RZ5 alloy
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792 785

Fig. 7. Elemental mapping of 8 wt.% TiB2 reinforced RZ5 alloy-based magnesium matrix composites.

Fig. 8. (a) FESEM micrograph of 4 wt.% TiB2 reinforced RZ5 composite, (b) Grain size measurement of TiB2 reinforced composites.

matrix. From the micrographs, it is noticed that there was
no macro or microporosity in the composites, which are gen-
erally observed in the composites developed by the ex-situ
method.
To study the areal distribution of the TiB2 reinforcement,
X-ray elemental mapping of the cast 8 wt.% TiB2 -reinforced
composites was carried out. The elemental mapping shown in
Fig. 7 reveals the uniform distribution of TiB2 particles along
with magnesium and its alloying elements.
A transient phase MgB7 was detected by XRD formed
during the in-situ reaction. In the FESEM micrograph, the
MgB7 phase formed along the grain boundary, as shown by
the dark grey colour in Fig. 8(a). From the micrograph shown
in Fig. 8(b), it was found that the average particle size of
the TiB2 reinforcement formed due to the in-situ reaction is
∼4–6 μm.
3.3. Mechanical properties
3.3.1. Hardness test
Fig. 9 shows the variation of hardness with an increase
in TiB2 reinforcement content for the as-cast and heat-treated
composites. It was noticed that the hardness of the composites
increased with increasing TiB2 reinforcement content. As the
TiB2 particles are very brittle in nature, they act as resistance
to the plastic deformation. The hardness of the composites
may also increase because of the grain refinement as TiB2
acts as a grain refiner. From the Fig. 9, it can be noticed that
the hardness of the HTCC is relatively low compared to ACC
because the ductility of the material increases due to the heat
treatment. For the ACB alloy, the hardness value was found
to be 64.2 HV, whereas for the HTCB material, the hardness
was found to be 61.1 HV. A similar trend was also observed
786 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792

Fig. 9. Variation of hardness with wt.% TiB2 all ACB, ACC, HTCB and HTCC materials.

for TiB2 -reinforced composites. Fig. 9 shows a hardness of

85.0 HV at 8 wt.% TiB2 for ACC, whereas for HTCC, the
hardness value decreased to 81.3 VHN.
The hardness of the materials also depends on the strength-
ening mechanism during synthesis and further processing of
materials. The strengthening mechanism of RZ5 alloy is gov-
erned by the elemental composition (Mg-Zn-Zr-RE) and heat
treatment (solutionize at 330°C for 2h followed by aged at
180°C for 16h). In case of RZ5/TiB2 composites, it is known
that during in-situ synthesis, magnesium doesn’t form any
phase with titanium. However, it forms a phase of MgB7 ,
which indicates the better interfacial bonding. To further en-
hance the mechanical properties of the composites, solution
strengthening regime is applied. The hardness of the materials
mainly depends on the distribution of the TiB2 reinforcement
in the magnesium RZ5 alloy matrix. The hardness of the ma-
terials also depends on the holding time during heat treatment
(solutionizing and aging). The heat treatment of the material
affects the dislocation density, as the difference between the
coefficient of thermal expansion of magnesium (26.5 × 106
K−1 ) and TiB2 (7 × 106 K−1 ) is high [31]. So, VHN of the
composites depends on the presence of precipitated MgB7
phase which helps in formation of strong interfacial bond and
difference in the coefficient of thermal expansion between re-
inforcement and matrix phase.
3.3.2. Tensile strength
The stress-strain behavior of base alloy and in-situ TiB2
reinforced MMCs was studied at room temperature (27°C).
The tensile strength properties of the magnesium RZ5 alloy
based MMCs were examined by varying the TiB2 reinforce-
ment contents. The gauge length of the samples was prepared
Fig. 10. Typical image of tensile samples after the tensile test.
as per ASTM E8/E8M – 13a standard. Fig. 10 shows the typ-
ical image of the samples after the test.
The stress-strain curve for ACB and ACC is shown in Fig.
11 (a), it was noticed that with an increase in TiB2 reinforce-
ment content, both yield strength (YS) and ultimate tensile
strength (UTS) improved. For the as-cast magnesium RZ5 al-
loy, the YS and UTS was found to be 91.3 MPa and 129.05
MPa respectively. With the addition of TiB2 reinforcement
by 4, 6 and 8 wt.%, the UTS of the composites increased by
10.48 %, 15.77 % and 30.47 % respectively. For the compos-
ite containing 8 wt.% of TiB2, the UTS value was found to be
168.31 MPa. It was observed that solutionize heat treatment
enhanced the tensile strength and ductility of the material.
From the engineering stress-strain curve of HTCB and
HTCC shown in Fig. 11 (b), it was noticed that HTCB con-
dition UTS is 150.93 MPa which indicate that the UTS of
the material increased by 16.95 % via heat treatment as per
ASTM B661 – 12. As the heat treatment was conducted in
two steps, i.e. solutionizing followed by aging, the ductility of
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
Fig. 11. Engineering stress-strain curve (a) ACB and TiB2 reinforced ACC and (b) HTCB and TiB2 reinforced HTCC.
the material improved significantly. For the base RZ5 alloy,
the ductility improved by 79.85 % post heat treatment. Sahoo
et al. also observed the significant improvement in strength
and ductility due to the heat treatment of magnesium AZ91
alloy and TiB2 /TiC reinforced composites [32]. It was also
found that the UTS and ductility improved by 6.31 % and
47.24 % respectively in case of 8 wt.% TiB2 reinforced mag-
nesium matrix composites. Fig. 11 (a and b) shows the reduc-
tion in ductility as the TiB2 reinforcement content increases.
The enhancement in strength and reduction in ductility de-
pends on the distribution of the TiB2 reinforcement particle
in the magnesium matrix.
The improvement of the tensile properties of the compos-
ite by the addition of TiB2 reinforcement is based on two ap-
proaches. One is, continuum mechanics indicating the transfer
of load and bonding between TiB2 reinforcement and matrix
during loading. Another is, strengthening effect of the com-
posites based on the yield strength of the material [33,34].
Nardone et al. established a formula for estimation of the the-
oretical yield strength of discontinuously reinforced ceramic
particle in a metal matrix which is based on the modified
shear-lag model for the particulate reinforced composites [35],
as shown in Eq. (5).
  
S   was also noticed that some TiB2 particles were present on
σyc = σym v p 1 + + 1 − vp
2 the fracture surface. As the strength of the material increases
Where σ yc and σ ym are the yield strength of the composite
and the matrix phase respectively, vp is the volume fraction of
the particulate reinforcement and s is the aspect ratio of the
reinforcement particles. The overall strength of the MMCs
improved due to the strong interfacial bond between TiB2
particle and RZ5 alloy matrix. With the increase in TiB2 re-
inforcement content (vp ), both YS and UTS increased whereas
tensile strain of the material decreased.
787
3.3.3. Tensile fracture surface
The morphology of the tensile fracture surface of the base
RZ5 alloy and in-situ TiB2 reinforced composite is shown in
Fig. 12. From Fig. 12 (a) it was observed that in case of base
RZ5 magnesium alloy, deep equiaxed dimples throughout the
surface which indicates the ductile mode of fracture. Few mi-
cro voids were also noticed on the fracture surface where the
cracks may have initiated. Also, the dimple type of structures
remains on the surface.
In case of TiB2 reinforced composites shown in Fig. 12(b),
along with few smaller size dimples, tear ridges were also
noticed on the surface. So the mixed mode of fracture has
occurred in case of composites. Tear ridge on the fracture
surface indicates the brittle modes of fracture. Presence of
ceramic reinforcement in the composites acts as a crack ar-
rester, which helps in improving the strength of the materi-
als [36]. Due to the presence of TiB2 particles, the ductility
of the material reduces. In case of composites, few micro
cracks were noticed at higher magnification along with tear
ridge surface shown in Fig. 12 (c) and 12 (d). The tear ridge
and micro-cracks may have initiated due to the presence of
ceramic TiB2 particle agglomeration at some points. Several
smaller size dimples were noticed in RZ5 – 8 wt.% TiB2 com-
posites shown in Fig. 12 (e) and 12(f) indicate that composite
follows a mixed mode of fracture. From the micrograph, it
(5)
with a minimal reduction of ductility indicates the good wet-
tability effect and strong bonding present due to the in-situ
formation of TiB2 particle.
3.3.4. Impact strength
The impact strength of the materials was measured by the
Charpy test. A typical image of the Charpy test samples along
with the V notch is shown in Fig. 13. The variation of the
impact strength of the Charpy sample is shown in Fig. 14
788 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792

Fig. 12. FESEM micrograph of tensile fracture surface (a) Magnesium RZ5 alloy, (b) Mg-8 wt.% TiB2 composite, (c) and (d) Micro-cracks and tear ridges
on the surface at the different magnifications of Mg-6 wt.% TiB2 composite, (e) and (f) Mg-8 wt.% TiB2 composite showing micro dimple and TiB2 particle
.
for the ACB, ACC, HTCB and HTCC materials. The impact
strength of the materials was recorded from the energy deliv-
ered by the pendulum during the impact test. For ACB and
HTCB alloys, the impact strength was found to be 1.62 and
1.41 J, respectively. Similarly, for the 8 wt.% TiB2 -reinforced
ACC and HTCC materials, the impact strength was found to
be 6.32 and 4.73 J, respectively. It was also noticed that for
all compositions of reinforcement content, the impact strength
of the ACC is more than for the HTCC materials. This may
have occurred as the materials were solutionize at 330°C for
2h followed by aged at 180°C for 16h. The impact strength
of the materials decreases with prolong aging time as the eu-
tectic phase of the materials get dissolved [37]. The impact
strength of the materials depends on the type of matrix and
reinforcement, as well as on the presence of any intermetallic
phase. In addition, the impact strength depends on the con-
dition of the heat treatment of the materials because of the
Fig. 13. Typical image of Impact test sample.
possibility of the formation of the precipitated phase [38].
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792 789

Fig. 14. Variation of impact strength with wt.% TiB2 ACB, ACC, HTCB Fig. 15. Variation of volumetric wear loss (mm3 ) with sliding distance (m)
and HTCC materials. of HTCB alloy and HTCC materials with a load of 20 N.

Fig. 16. FESEM micrograph of (a) RZ5 alloy, (b) 4 wt.%, (c) 6 wt.% and (d) 8 wt.% TiB2 , (e) and (f) delamination of 6 wt.% TiB2 reinforced RZ5 alloy
based magnesium matrix composites with a load of 20 N.
790 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
Fig. 17. EDX analysis of wear surface of magnesium RZ5 alloy.
3.3.5. Wear test
Tribological behavior of RZ5 magnesium alloy and 4, 6
and 8 wt.% TiB2 reinforced MMCs was measured using pin-
on-disk wear testing setup. Fig. 15 shows the volumetric wear
loss (in mm3 ) for both HTCB and HTCC by applying a load
of 20 N. For each sample, three sets of tests were performed
to evaluate the actual wear loss by varying both the sliding
distance and reinforcement content. From Fig. 15, it can be
observed that the volumetric wear loss of the materials in-
creased with increase in sliding distance. It was also noticed
that with the increase in TiB2 reinforcement content wear
loss decreased. Which indicates that the presence of ceramics
phase TiB2 is acting as the resistance to wear at the contact
surface. Volumetric wear loss of 25.826 mm3 was observed in
case of HTCB alloy whereas that of 22.949 mm3 was found
in case of HTCC when reinforced with 8 wt.% TiB2 for a
sliding distance of 2000 m. For different sliding distances,
the volumetric wear loss for TiB2 particles reinforced com-
posites observed to be lesser when compared to RZ5 base
alloy due to the absence of TiB2 particles on the contact sur-
face in the softer matrix phase. For the RZ5 alloy wear loss
was 6.424, 12.929, 19.462 and 26.019 mm3 whereas in case
of 8 wt.% TiB2 composite wear loss was found to be 5.371,
11.327, 16.970 and 22.656 mm3 for the sliding distance of
500, 1000, 1500 and 2000 m respectively.
The FESEM microstructural examination of the wear sur-
face includes delamination, wear groove, micro-crack, wear
debris and oxides. During the wear process, materials re-
moved in the form of wear debris and wear grooves were
formed due to the plastic deformation of the material at the
contact surface. Due to friction, the temperature at the contact
surface increases and some of the wear debris became oxides.
Fig. 16 (a–d) shows the FESEM micrograph of RZ5 base al-
loy and 4, 6 and 8 wt.% TiB2 reinforced composites with
a test condition of 20 N load and for a sliding distance of
2000 m. The morphology of the worn surface showed some
wear groove formation and delamination along with wear de-
bris and oxides. In case of composites, the presence of hard
ceramic TiB2 particle acts as a protective layer at the contact
surface and these ceramic particles lead to the formation of
heavy delamination and deep groove. In case of composites,
some cracked ceramic particles were noticed on the worn sur-
face. The wear behavior of the composite materials depends
on the interfacial bond formation between the matrix and the
reinforcement [39]. Fig. 16 (e and f) shows the initiation of
delamination on the worn surface of 6 wt.% TiB2 reinforced
composite due to the presence of hard ceramic particles at
different magnifications. Wear groove, delamination and ox-
ide particles were observed clearly on the wear surface at
higher magnification of the materials. EDX analysis of the
wear surface of the material was conducted to study the for-
mation of the oxide during the dry sliding wear. The EDX
analysis of magnesium shown in Fig. 17 confirms the forma-
tion of oxide during the dry sliding of the materials with the
hardened EN31 rotating disc. The oxide on the contact surface
formed due to the rubbing action at the contact surface.
4. Conclusion
In the present research work, TiB2 -reinforced magnesium
RZ5 alloy-based in-situ MMCs were successfully synthesised
by an SHS route. During the synthesis of composite, temper-
ature, holding time and casting environment were the major
variables. The following conclusions can be made from the
present work:
1. Optical and FESEM micrograph indicated the near-uniform
distribution of the TiB2 reinforcement in the magnesium
RZ5 alloy matrix. XRD phase analysis confirmed the for-
mation of a stable TiB2 phase along with the TiB and
MgB7 transient phase.
2. The hardness value of the composite increased from 64.2
to 85.0 VHN by reinforcing with 8 wt.% TiB2 . The impact
 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
strength of the material also increases with increasing TiB2
content. The solutionising heat treatment of ACB and ACC
improved the ductility of the materials, which led to a
minor reduction in hardness and impact strength.
3. A maximum increase of 30.47% was observed in the UTS
by the addition of 8 wt.% TiB2 in the magnesium RZ5
alloy matrix. The solutionising heat treatment further en-
hanced the UTS by 16.95%. The micrograph of the ten-
sile fracture surface for the RZ5 alloy revealed the ductile
mode of fracture, whereas for the composites, a mixed
mode of fracture was observed.
4. Volumetric wear loss for the RZ5 base alloy was found
to be 25.826 mm3 for the sliding distance of 2000 m,
whereas the wear loss reduced to 22.655 mm3 in the case
of the composite with 8 wt.% TiB2 . FESEM micrographs
revealed the delamination, wear groove and oxide particle
formation on the contact surface.
The addition of up to 8 wt.% TiB2 reinforcement in the
magnesium RZ5 alloy matrix improved the mechanical prop-
erties, including tensile strength, impact strength and wear
resistance, making the material more suitable for use in var-
ious components of the automobile and aerospace industries.
The further addition of TiB2 may lead to excessive brittleness,
which may not be suitable for practical applications.
Acknowledgment
The author(s) would like to express their gratitude to
Foundry and Forge Division, Hindustan Aeronautics Limited
Bangalore, India for providing the magnesium alloy.
References
[1] K.K. Chawla, N. Chawla, Metal Matrix Composites, Academic Press,
Inc., 1991 doi:10.1002/0471238961.1305200103080123.a01.pub3.
[2] G.T. Kridli, P.A. Friedman, J.M. Boileau, Manufacturing Processes
for Light Alloys, Woodhead Publishing Limited, 2010, doi:10.1533/
9781845697822.2.235.
[3] N. Natarajan, V. Krishnaraj, J.P. Davim, Metal Matrix Composites
Synthesis, Wear Characteristics, Machinability Study of MMC Brake
Drum, Springer Cham Heidelberg New York Dordrecht London, 2015,
doi:10.1016/j.mpdhp.2014.03.001.
[4] L. Ceschini, A. Dahle, M. Gupta, A.E.W. Jarfors, S. Jayalakshmi,
A. Morri, F. Rotundo, S. Toschi, R.A. Singh, Aluminum and Mag-
nesium Metal Matrix Nanocomposites, Springer Nature Singapore Pte
Ltd., 2017, doi:10.1007/978- 981- 10- 2681- 2.
[5] P.R. Samal, P.R. Vundavilli, A. Meher, M.M. Mahapatra, Influence of
TiC on dry sliding wear and mechanical properties of in situ synthesized
AA5052 metal matrix composites, J. Compos. Mater. 53 (2019) 4323–
4336, doi:10.1177/0021998319857124.
[6] Q. Chen, G. Chen, F. Han, X. Xia, Y. Wu, Microstructures, mechanical
properties, and wear resistances of thixoextruded SiCp/WE43 magne-
sium matrix composites, Metall. Mater. Trans. A Phys. Metall. Mater.
Sci. 48 (2017) 3497–3513, doi:10.1007/s11661- 017- 4104- z.
[7] A.A. Luo, Magnesium casting technology for structural applications, J.
Magnes. Alloy. 1 (2013) 2–22, doi:10.1016/j.jma.2013.02.002.
[8] D.J. Towle, C.M. Friend, Effect of reinforcement architecture on me-
chanical properties of a short fibre/magnesium RZ5 MMC manufac-
tured by preform infiltration, Mater. Sci. Eng. A 188 (1994) 153–158,
doi:10.1016/0921- 5093(94)90367- 0.
791
[9] A. Meher, D. Chaira, Effect of graphite and SiC addition into Cu
and SiC particle size effect on fabrication of Cu–graphite–SiC MMC
by powder metallurgy, Trans. Indian Inst. Met. 70 (2017) 2047–2057,
doi:10.1007/s12666- 016- 1026- 1.
[10] H.Y. Wang, Q.C. Jiang, Y. Wang, B.X. Ma, F. Zhao, Fabrication of
TiB2participate reinforced magnesium matrix composites by powder
metallurgy, Mater. Lett. 58 (2004) 3509–3513, doi:10.1016/j.matlet.
2004.04.038.
[11] Q.C. Jiang, X.L. Li, H.Y. Wang, Fabrication of TiC particulate rein-
forced magnesium matrix composites, Scr. Mater. 48 (2003) 713–717,
doi:10.1016/S1359- 6462(02)00551- 1.
[12] D. Vallauri, I.C. Atías Adrián, A. Chrysanthou, TiC-TiB2composites: a
review of phase relationships, processing and properties, J. Eur. Ceram.
Soc. 28 (2008) 1697–1713, doi:10.1016/j.jeurceramsoc.2007.11.011.
[13] S.C. Tjong, Z.Y. Ma, Microstructural and mechanical characteristics of
in situ metal matrix composites, Mater. Sci. Eng. R Reports 29 (2000)
49–113, doi:10.1016/S0927- 796X(00)00024- 3.
[14] D. Mehra, M.M. Mahapatra, S.P. Harsha, Processing of RZ5-10wt%TiC
in-situ magnesium matrix composite, J. Magnes. Alloy. 6 (2018) 100–
105, doi:10.1016/j.jma.2018.01.002.
[15] H. Li, X. Dai, L. Zhao, B. Li, H. Wang, C. Liang, J. Fan, Microstructure
and properties of carbon nanotubes-reinforced magnesium matrix com-
posites fabricated via novel in situ synthesis process, J. Alloy. Compd.
785 (2019) 146–155, doi:10.1016/j.jallcom.2019.01.144.
[16] M. Shamekh, M. Pugh, M. Medraj, Understanding the reaction mech-
anism of in-situ synthesized (TiC-TiB 2)/AZ91 magnesium matrix
composites, Mater. Chem. Phys. 135 (2012) 193–205, doi:10.1016/j.
matchemphys.2012.04.054.
[17] M.A. Matin, L. Lu, M. Gupta, Investigation of the reactions between
boron and titanium compounds with magnesium, Scr. Mater. 45 (2001)
479–486, doi:10.1016/S1359- 6462(01)01059- 4.
[18] P. Xiao, Y. Gao, C. Yang, Z. Liu, Y. Li, F. Xu, Microstructure, mechan-
ical properties and strengthening mechanisms of Mg matrix composites
reinforced with in situ nanosized TiB 2 particles, Mater. Sci. Eng. A.
710 (2018) 251–259, doi:10.1016/j.msea.2017.10.107.
[19] H.Y. Wang, Q.C. Jiang, Y.G. Zhao, F. Zhao, In situ synthesis of
TiB2/Mg composite by self-propagating high-temperature synthesis re-
action of the Al-Ti-B system in molten magnesium, J. Alloys Compd.
379 (2004) 4–7, doi:10.1016/j.jallcom.2004.02.036.
[20] C. Fang, G. Liu, H. Hao, X. Zhang, Effects of particle distribution
on microstructural evolution and mechanical properties of TiB2/AZ31
composite sheets, Mater. Sci. Eng. A 684 (2017) 592–597, doi:10.1016/
j.msea.2016.12.072.
[21] K.V. Narayanan, B. Lakshmikutty, Stoichiometry and Process Calcula-
tions, 2nd editio, PHI, 2006.
[22] Y. Wang, H.Y. Wang, Y.F. Yang, Q.C. Jiang, Solidification behavior of
cast TiB2 particulate reinforced Mg composites, Mater. Sci. Eng. A 478
(2008) 9–15, doi:10.1016/j.msea.2007.05.055.
[23] ASTM, B661 - 12, Standard practice for heat treatment of magnesium
alloys (2000) 1–7, doi:10.1520/B0661-12.2.
[24] R.C. Adams, ASM hand book -metallography and microstructure, Tech-
nology 9 (2) (2001) 3470, doi:10.1016/S0026- 0576(03)90166- 8.
[25] ASTM, in: E8/E8M - 13a, Standard test methods for tension testing of
metallic materials, 2012, pp. 133–140, doi:10.1520/E0008.
[26] ASTM, E23 − 16b, Standard test methods for notched bar impact testing
of metallic materials (2009) 1–26, doi:10.1520/E0023-07AE01.
[27] ASTM, G99-17, Standard test method for wear testing with a pin-on-
disk apparatus (2017) 1–6, doi:10.1520/G0099-17.
[28] R.V.P. Kaviti, D. Jeyasimman, G. Parande, M. Gupta,
R. Narayanasamy, Investigation on dry sliding wear behavior of Mg/BN
nanocomposites, J. Magnes. Alloy. 6 (2018) 263–276, doi:10.1016/j.
jma.2018.05.005.
[29] B.X. Ma, H.Y. Wang, Y. Wang, Q.C. Jiang, Fabrication of (TiB2-
TiC)p/AZ91 magnesium matrix hybrid composite, J. Mater. Sci. 40
(2005) 4501–4504, doi:10.1007/s10853- 005- 0886- 2.
[30] Q. Guohong, F. Canfeng, B. Yun, H. Hai, Z. Xingguo, Effect of hot
extrusion on microstructures and properties of TiB2/AZ31 magnesium
792 A. Meher, M.M. Mahapatra and P. Samal et al. / Journal of Magnesium and Alloys 8 (2020) 780–792
based composites, Rare Met. Mater. Eng. 40 (2011) 1339–1343, doi:10.
1016/S1875- 5372(11)60053- 2.
[31] S. Mozammil, J. Karloopia, R. Verma, P.K. Jha, Effect of varying TiB2
reinforcement and its ageing behaviour on tensile and hardness prop-
erties of in-situ Al-4.5%Cu-xTiB2 composite, J. Alloy. Compd. 793
(2019) 454–466, doi:10.1016/j.jallcom.2019.04.137.
[32] B.N. Sahoo, S.K. Panigrahi, Synthesis, characterization and mechanical
properties of in-situ (TiC-TiB2) reinforced magnesium matrix compos-
ite, Mater. Des. 109 (2016) 300–313, doi:10.1016/j.matdes.2016.07.024.
[33] F. Chen, Z. Chen, F. Mao, T. Wang, Z. Cao, TiB2 reinforced aluminum
based in situ composites fabricated by stir casting, Mater. Sci. Eng. A
625 (2015) 357–368, doi:10.1016/j.msea.2014.12.033.
[34] S. Jayalakshmi, S. Gupta, S. Sankaranarayanan, S. Sahu, M. Gupta,
Structural and mechanical properties of Ni60Nb40 amorphous alloy par-
ticle reinforced Al-based composites produced by microwave-assisted
rapid sintering, Mater. Sci. Eng. A 581 (2013) 119–127, doi:10.1016/j.
msea.2013.05.072.
[35] V.C. Nardone, K.M. Prewo, On the strength of discontinuous silicon
carbide reinforced aluminum composites, Scr. Metall. 20 (1986) 43–48,
doi:10.1016/0036- 9748(86)90210- 3.
[36] S.V. Sujith, M.M. Mahapatra, R.S. Mulik, An investigation into fabrica-
tion and characterization of direct reaction synthesized Al-7079-TiC in
situ metal matrix composites, Arch. Civ. Mech. Eng. 19 (2019) 63–78,
doi:10.1016/j.acme.2018.09.002.
[37] Q. Wang, L. Xiao, W. Liu, H. Zhang, W. Cui, Z. Li, G. Wu, Effect
of heat treatment on tensile properties, impact toughness and plane-
strain fracture toughness of sand-cast Mg-6Gd-3Y-0.5Zr magnesium al-
loy, Mater. Sci. Eng. A 705 (2017) 402–410, doi:10.1016/j.msea.2017.
08.100.
[38] M.F. Ibrahim, H.R. Ammar, A.M. Samuel, M.S. Soliman, F.H. Samuel,
On the impact toughness of Al-15 vol.% B4C metal matrix composites,
Compos. Part B Eng. 79 (2015) 83–94, doi:10.1016/j.compositesb.2015.
04.018.
[39] A. Kumar, P.K. Jha, M.M. Mahapatra, Abrasive wear behavior of in
situ tic reinforced with Al-4.5%Cu matrix, J. Mater. Eng. Perform. 23
(2014) 743–752, doi:10.1007/s11665- 013- 0836- 0.