materials

Article
Al0.5CoCrFeNi2 High Entropy Alloy Particle Reinforced AZ91
Magnesium Alloy-Based Composite Processed by Spark
Plasma Sintering
Chun Chiu * and Hsun-Hsiang Chang

Department of Mechanical Engineering, National Taiwan University of Science and Technology,

Taipei 106335, Taiwan; m10703517@mail.ntust.edu.tw
* Correspondence: cchiu@mail.ntst.edu.tw

Abstract: In this study, AZ91 magnesium-alloy-based metal matrix composites (MMCs) reinforced
with 10 wt% of Al0.5 CoCrFeNi2 high-entropy alloy (HEA) particles and SiC particles were prepared by
a spark plasma sintering (SPS) process at 300 ◦ C. The effects of reinforcements on the microstructure
and mechanical properties of AZ91-based MMCs were studied. The results showed that AZ91–HEA
composite consisted of α-Mg, Mg17 Al12 and FCC phases. No interfacial reaction layer was observed
between HEA particles and the Mg matrix. After adding HEA into AZ91, the compressive yield
strength (C.Y.S) of the AZ91–HEA composite increased by 17% without degradation of failure strain.
In addition, the increment in C.Y.S brought by HEA was comparable to that contributed by commonly
used SiC reinforcement (15%). A relatively low porosity in the composite and enhanced interfacial
bonding between the α-Mg matrix and HEA particles make HEA a potential reinforcement material





 in MMCs.

Citation: Chiu, C.; Chang, H.-H.

Keywords: AZ91 magnesium alloy; high-entropy alloy; metal matrix composite; spark plasma sintering
Al0.5 CoCrFeNi2 High Entropy Alloy
Particle Reinforced AZ91 Magnesium
Alloy-Based Composite Processed by
Spark Plasma Sintering. Materials
2021, 14, 6520. https://doi.org/
1. Introduction
10.3390/ma14216520 The goal for energy saving through improving fuel efficiency has driven the need for
lightweight materials. Magnesium alloy is one of the most important lightweight materials
Academic Editor: Sergey in the automotive, aerospace and biomaterial industries and has attracted much attention
V. Zherebtsov because of its high specific strength to weight ratio and recyclability [1–4]. However, the
strength of conventional AZ (Mg–Al–Zn) and AM (Mg–Al–Mn) series Mg alloys will not
Received: 20 September 2021 meet the expanded requirements for load-bearing components with the rapid development
Accepted: 26 October 2021
of science and technology [5]. As a result, research into high-performance Mg alloys that
Published: 29 October 2021
will satisfy the extended industrial applications is essential.
One way to strengthen Mg alloys is by adding reinforcement phase into Mg matrix
Publisher’s Note: MDPI stays neutral
and making Mg alloy-based composites. Ceramic hard particles, such as Al2 O3 , ZnO,
with regard to jurisdictional claims in
SiC, TiC and Y2 O3 , have been widely studied for application in Mg-based composites.
published maps and institutional affil-
However, the difference of thermal expansion coefficient, poor wettability and interfacial
iations.
reaction have hindered their application [6]. To solve the issues, metallic glass (MG)
phase reinforcement has been studied. MGs have superior elastic properties, strength
and most importantly, good wettability with metal matrix (due to its metallic nature) [7].
A metallic-glass-reinforced AZ91 magnesium-alloy-based composite was studied and
Copyright: © 2021 by the authors. displayed improved hardness and strength compared to the AZ91 alloy [8].
Licensee MDPI, Basel, Switzerland.
Recently, an emerging category of alloys, high-entropy alloys (HEAs), has attracted lots
This article is an open access article
of attention. Unlike conventional alloys, HEAs consist of five or more principal elements,
distributed under the terms and
and each element’s concentration is from 5 to 35 at% [9]. Because of the four essential
conditions of the Creative Commons
effects, such as high-entropy effect, sluggish diffusion effect, severe lattice distortion
Attribution (CC BY) license (https://
and cocktail effect, HEAs possess high strength, excellent corrosion resistance and wear
creativecommons.org/licenses/by/
4.0/).
resistance. In addition to traditional structural applications, potential applications of HEAs

Materials 2021, 14, 6520. https://doi.org/10.3390/ma14216520 https://www.mdpi.com/journal/materials

Materials 2021, 14, 6520 2 of 15

can be found in surface coating, environmental protection, gas sensing, energy storage
and waste heat recovery [10,11]. HEAs also have good wettability with metal and thermal
expansion coefficients similar to those of metals. Thus, it has potential for the application as
a reinforcement in Mg-alloy-based metal matrix composites and can solve the compatibility
issue between metal matrices and ceramic reinforcements. HEAs can be classified into 3D
transition metal HEAs, 4f transition metal HEAs, refractory metal HEAs and light metal
HEAs [10]. Among different series of HEAs, the one based on principle elements of Al,
Co, Cr, Fe and Ni has been extensively studied for its microstructure, phase stability and
mechanical properties [9–16]. Equiatomic AlCoCrFeNi HEA is a dual-phase (FCC and
BCC) material, and it undergoes a phase transformation at high temperature [17]. On the
other hand, Al0.5 CoCrFeNi2 [18,19], which has an FCC structure, exists a high thermal
stability and is more suitable for application as a reinforcement in MMCs.
The fabrication of Mg-based metal matrix composites (MMCs) has been carried out
by stir casting or by the powder metallurgy (P/M) method, which combines powder
preparation and consolidation of powders. Unlike the agglomeration of reinforced particles
in the ingot prepared by stir casting, uniform distribution of reinforcements is obtained in
the samples prepared by the P/M method. Recently, spark plasma sintering (SPS) has been
applied in P/M. Compared to traditional hot pressing method, samples processed by SPS
have high density and less grain or microconstituent growth due to the short holding time.
Studies of Mg and its alloys prepared by SPS have been reported, and the results indicated
that the strength of the Mg alloy prepared by SPS is superior to that of the cast one [20–22].
In the present work, we explored a new way of strengthening of Mg alloy by addition
of HEA particles. The Al0.5 CoCrFeNi2 HEA was chosen as the reinforcement due to its
high strength and its well-known properties, which make it suitable for the early-stage
development of HEA-reinforced MMCs. Al0.5 CoCrFeNi2 -reinforced AZ91 composites
were fabricated by SPS, and their microstructures and mechanical properties were studied.
SiC-reinforced AZ91 composites were also prepared for comparison of their mechanical
properties.

2. Materials and Methods

Atomized AZ91 powder with an average particle size of 45 µm was purchased from
Weihao Magnesium Powder Co., Ltd. (Tangshan, China). Al0.5 CoCrFeNi2 (at%) high
entropy alloy (HEA) powder fabricated by gas-atomization process was supplied by Nano
Manufacturing and Surface Treatment Lab, NTUST, Taipei, Taiwan (R.O.C.). Details of the
HEA powder preparation can be found in reference [23]. The average particle size of HEA
powder was 28 µm. SiC powder with an average particle size of 38 µm was acquired from
Taicheng Metallic Materials Co. Ltd. (Wuxi, China).
Powder mixtures of AZ91 with 10 wt% of HEA and SiC powder were blended in a
twin arm shaker for 5 min. All of the powder handling was implemented in a glove box
filled with purified argon to prevent oxidation. Subsequently, AZ91–HEA and AZ91–SiC
powder mixtures were consolidated by spark plasma sintering (SPS). The SPS was carried
out under vacuum in a SPS-515S system (SPS SYNTEX INC, Tokyo, Japan,) with a sintering
temperature of 300 ◦ C, a pressure of 50 MPa and a holding time of 5 min. The nomenclature
and processing of the alloys and composites in the present study are summarized in Table 1.
The porosity (φ) of the sample was calculated from the difference between the theoretical
(ρT ) and experimental density (ρE ):

φ = 1 − ρE /ρT (1)

Microstructural characterization was conducted with a scanning electron microscope

(SEM) (JEOL JSM-6500F, Tokyo, Japan) equipped with Energy Dispersive Spectroscopy
(EDS). Phase analysis was performed by X-ray diffraction (XRD) (Bruker D2, Billerica,
MA, USA) using Cu Kα radiation. The diffraction data were collected with a step size
of 0.02◦ and time of 0.5 s in the scan range of 20 to 80◦ . Dislocation densities of AZ91,
Materials 2021, 14, 6520 3 of 15

AZ91–HEA and AZ91–SiC composites were calculated by analyzing XRD patterns using
the Williamson–Hall equation [24] and Williamson–Smallman equation [25]:
 
β cos θ 1 2sin θ
= + 2ε (2)
λ Dv λ

where Dv is the average crystallite size, ε is the microstrain, b is the integral breadth, λ is
the wave-length and θ is the position of the analyzed peak maximum. Dislocation density
(ρ) is related to microstrain and can be calculated using the following equation:

kε
ρ= (3)
b2
where k is the material constant (considered as 1 for Mg alloy), and b is the magnitude of
Burger’s vector.
Mechanical properties of the composites were evaluated by using compression test,
microhardness test and nanoindentation test. Compression test was performed at room
temperature using a universal material testing machine MTS810 (MTS, Eden Prairie, OR,
USA). Samples with a diameter of 10 mm and a height of 10 mm were tested under a strain
rate of 10−3 /s following ASTM standard E9-89a. Three tests were performed for each alloy
and composite to obtain average value and standard deviation. The strain hardening rate
(θ) was calculated using the following equation:

θ = dσt /dεt (4)

where σt and εt are true stress and true strain, respectively.

Vickers microhardness tests were performed using Akashi MVK-H1 (Mitutoyo, Kawasaki,
Japan) microhardness tester. The load and the dwell time were 200 g and 15 s, respectively.
The spacing between indents was at least three times the diagonal. Nanoindentation tests
were performed by using TI-900 Nanoindentator (TriboIndenter, Hysitron, Billerica, MA,
USA). The maximum load was set as 1000 µN. The load function for nanoindentation is of
5 × 5 × 5 mode, which means taking 5 s to increase the load to 1000 µN, holding for 5 s
and then reducing to zero in another 5 s. Ten measurements were carried out for hardness
tests, and an average value was presented.

Table 1. Nomenclature and processing of the alloys and composites studied in the present study.

Sample ID Processing
AZ91 AZ91 powder compacted by SPS
AZ91–HEA AZ91-10 wt% Al0.5 CoCrFeNi2 compacted by SPS
AZ91–SiC AZ91-10 wt% SiC compacted by SPS

3. Results
3.1. Microstructural Characterization
3.1.1. Characterization of AZ91, HEA and SiC Powders
SEM micrographs of the cross section of AZ91, HEA (Al0.5 CoCrFeNi2 ) and SiC pow-
ders are shown in Figure 1, and the corresponding XRD patterns are given in Figure 2. The
gas-atomized AZ91 and HEA powders had a circular cross section and the SiC powder
had an irregular shape. AZ91 powder contained α-Mg and Mg17 Al12 precipitates along the
grain boundary. Diffraction peaks at 43.5, 51.2 and 75.0◦ were observed in the XRD pattern
of HEA powder, indicating that HEA has an FCC structure. No precipitates were observed
in HEA powder. Only the SiC phase was observed in as-received SiC powders.
Materials 2021, 14, 6520 4 of 15
Materials 2021, 14, x 4 of 16
Materials 2021, 14, x 4 of 16

Figure 1. SEM micrographs showing the cross section of (a) AZ91, (b) HEA and (c) SiC powders.
Figure
Figure1.1.SEM
SEMmicrographs
micrographsshowing
showingthe
thecross
crosssection
sectionofof(a)
(a)AZ91,
AZ91,(b)
(b)HEA
HEAand
and(c)
(c)SiC
SiCpowders.
powders.

Figure
Figure2.2. XRD patterns
XRDpatterns
2.XRD of
patternsof (a)
of(a) AZ91,
(a)AZ91, (b)
AZ91,(b) HEA
(b)HEA and
HEAand (c)
and(c) SiC
(c)SiC powders.
SiCpowders.
powders.
Figure
Materials 2021, 14, 6520 5 of 15

3.1.2. Characterization of SPS Samples

Figure 3a shows the SEM micrograph of the sintered AZ91 sample. Pores could be
seen along the particle boundary and the porosity measured by image analysis was ~1.0%.
A higher magnification micrograph (Figure 3b) illustrates the microstructure of the sintered
AZ91 consisting of brighter precipitates (area B) located along the boundary of gray grains
(area A). By combing results from EDS and XRD analysis (Table 2 and Figure 4), the brighter
precipitate was identified as the Mg17 Al12 phase, and the gray grain was α-Mg. The results
Materials 2021, 14, x indicated that no phase transformation occurred in the AZ91 sample after the SPS6 of process,
16
and the precipitates still distributed along the grain boundary.

Figure 3. SEM micrograph showing (a) particle boundaries in AZ91, (b) precipitates in Mg matrix in AZ91, (c) distribution
SEMinmicrograph
Figureof3.HEA AZ91–HEA showing
composite,(a)
(d)particle
boundaryboundaries in AZ91,
of HEA particle (b) precipitates
in AZ91 in Mg matrix
matrix, (e) distribution in AZ91,
of SiC (c) distribution
in AZ91–SiC com- of
HEA inposite
AZ91–HEA composite,
and (f) boundary of (d)
SiCboundary
particle inof HEAmatrix
AZ91 particle
(EDSin AZ91 matrix,
analysis results(e)
ofdistribution of SiC
area A (matrix) andinBAZ91–SiC composite
(reinforcement) are and
given inofTable
(f) boundary 2).
SiC particle in AZ91 matrix (EDS analysis results of area A (matrix) and B (reinforcement) are given in Table 2).
Materials 2021, 14, 6520 6 of 15

Figure 3c shows the microstructure of the sintered AZ91–HEA composite. HEA

particles distributed uniformly in the AZ91 matrix. A clear boundary between HEA
particle and matrix could be seen and no interfacial reaction layer was observed (Figure 3d).
The porosity in the sintered composite was 0.8%. EDS analysis results indicated that
compositions of α-Mg grain (area A) and HEA (area B) were almost identical to that
of α-Mg in sintered AZ91 and the composition of as-received HEA, respectively. The
observation that no phase transformation occurred in the AZ91–HEA composite after SPS
process was also confirmed by XRD analysis (Figure 4). HEA had a single FCC phase after
SPS, and α-Mg with Mg17 Al12 was still detected. Moreover, no interfacial reaction layer
was observed implying there was no interdiffusion between reinforcement and matrix.
The microstructure of sintered AZ91–SiC composite showed uniformly distributed SiC
particles in the AZ91 matrix (Figure 3e). No interface reaction layer was formed between
reinforcement and the matrix after SPS. Combined with the results from the EDS and XRD
analyses, α-Mg, Mg17 Al12 and SiC were the only phases presented in the composite. No
phase transformation occurred after SPS. However, the porosity of the sintered sample was
3.8%, which was four times higher than those from the sintered AZ91 and the AZ91–HEA
composite.
From the SEM images in Figure 3, a clear interface between the matrix and the
reinforced phase HEA and SiC was observed. The compositions of the α-Mg matrix in
the composites were similar to that in the AZ91 (Table 2). The composition of HEA in the
sintered composite had no obvious change, compared to composition of as-received HEA
powder. Moreover, from the results of the EDS line scans of HEA and SiC particles in the
composites (Figure 5), no interfacial reaction layer was formed between the HEA, SiC and
Mg matrix. The above results confirmed that no diffusion between the reinforced particle
Materials 2021, 14, x 7 of 16
and the matrix occurred during the SPS process. No aggregations of reinforced particles
were observed in the AZ91–HEA and AZ91–SiC composites.

Figure
Figure4. XRD patterns
4. XRD of AZ91,
patterns AZ91–HEA
of AZ91, and AZ91–SiC
AZ91–HEA samples.samples.
and AZ91–SiC

Table 2. Composition of as-received HEA and different areas marked in AZ91–HEA and AZ91–SiC (at%).

Element
Sample Area
Mg Al Mn Zn Co Cr Fe Ni Si C
HEA - - 8.64 - - 18.15 18.34 18.72 36.15 - -
Materials 2021, 14, 6520 7 of 15

Table 2. Composition of as-received HEA and different areas marked in AZ91–HEA and AZ91–SiC (at%).

Element
Sample Area
Mg Al Mn Zn Co Cr Fe Ni Si C
HEA - - 8.64 - - 18.15 18.34 18.72 36.15 - -
AZ91 A 90.91 8.76 0.13 0.21 - - - - - -
AZ91 B 80.11 19.56 0.10 0.13 - - - - - -
AZ91–HEA A 91.45 8.13 0.10 0.31 - - - - - -
AZ91–HEA B - 8.87 - - 18.16 18.11 18.99 35.87 - -
AZ91–SiC A 91.36 8.21 0.13 0.30 - - - - - -
Materials 2021, 14, x 8 of 16
AZ91–SiC B - - - - - - - - 47.09 52.91

Figure 5. EDS line scan of (a) HEA and (b) SiC in the AZ91-based composites.
Figure 5. EDS line scan of (a) HEA and (b) SiC in the AZ91-based composites.
3.2. Mechanical Properties of SPS Samples
The results of engineering compressive stress-strain curves of the AZ91 alloy and the
AZ91–HEA and AZ91–SiC composites are shown in Figure 6 (Enlarged sections of curves
of the composites are shown in Figures S1 and S2 in Supplementary Material). The en-
Materials 2021, 14, 6520 8 of 15

3.2. Mechanical Properties of SPS Samples

The results of engineering compressive stress-strain curves of the AZ91 alloy and
the AZ91–HEA and AZ91–SiC composites are shown in Figure 6 (Enlarged sections of
curves of the composites are shown in Figures S1 and S2 in Supplementary Material).
The enhancement of compressive yield strength (C.Y.S), ultimate compressive strength
Materials
Materials2021,
2021,14,
14,xx 99 ofof 16
16
(U.C.S.) of the AZ91 composites can be observed when compared to those of the AZ91
alloy. Figure 7 shows the strain hardening rate versus the true strain for various samples.
Higher strain hardening rates were found in the AZ91 alloys reinforced with SiC and HEA.
all
allof
For ofthe
all of samples,
the samples,
the the
thehardening
samples, hardening
the occurred
hardeningoccurredatatthe
occurred atinitial
the initial
the stage
stage
initial of
ofthe
stage ofdeformation.
the deformation. All
Allsam-
the deformation. sam-
All
ples displayed
ples displayed
samples similar
displayedsimilar decreasing
similardecreasing of work
decreasingofofworkhardening
workhardening tendency,
hardening tendency, indicating that behavior
indicating thatbehavior
tendency, indicating behavior
of plastic
ofplastic
of deformation
plasticdeformation
deformationofof the
ofthe alloy
thealloy and
alloyand composites
andcomposites
compositesisisisalmost
almost the
almostthe same.
thesame.
same.

Figure
Figure 6.6.Engineering
Figure6. Engineering
Engineeringcompressive
compressivestress-strain
stress-straincurves AZ91
curvesofofAZ91 alloy,
AZ91alloy, AZ91–HEA
alloy,AZ91–HEA and
AZ91–HEAand AZ91–SiC
andAZ91–SiC
AZ91–SiC
composites.
composites.
composites.

Figure
Figure 7.7.Curves
Figure7. Curves ofofstrain
Curvesof strain
strainhardening
hardening
hardening rate
rate
rate against
against
against true
true
true strain
forfor
strain
strain forAZ91
AZ91AZ91 alloy,
alloy,
alloy, AZ91–HEA
andand
AZ91–HEA
AZ91–HEA andAZ91–
AZ91–
AZ91–SiC
SiC
SiCcomposites.
composites.
composites.

Mechanical
Mechanicalproperties
propertiesof
ofthe
thesintered
sinteredsamples
samplesarearesummarized
summarizedin inTable
Table3.3.From
Fromthe
the
summarized
summarized results of compression tests, the effect of reinforcement on the strengthof
results of compression tests, the effect of reinforcement on the strength of
composite
compositecould
couldbebeobserved.
observed.ItItcould
couldbebeseen
seenthat
thatthe
thehardness
hardnessand
andcompressive
compressiveyield
yield
strength
strength(C.Y.S)
(C.Y.S)of
ofAZ91
AZ91increased
increasedafter
afteradding
adding1010wt%
wt%of ofreinforcement.
reinforcement.The
Thehardness
hardness
first increased from 93 HV in AZ91 to 123 HV in the AZ91–SiC composite and further
Materials 2021, 14, 6520 9 of 15

Mechanical properties of the sintered samples are summarized in Table 3. From the
summarized results of compression tests, the effect of reinforcement on the strength of
composite could be observed. It could be seen that the hardness and compressive yield
strength (C.Y.S) of AZ91 increased after adding 10 wt% of reinforcement. The hardness first
increased from 93 HV in AZ91 to 123 HV in the AZ91–SiC composite and further increased
to 138 HV in the AZ91–HEA composite. The C.Y.S increased from 178 MPa in AZ91 to 204
and to 209 MPa in AZ91–SiC and AZ91–HEA, respectively. No degradation of the failure
strain was observed after the addition of HEA and SiC. The failure strain of the AZ91–SiC
was similar to that of AZ91, and the failure strain of AZ91–HEA increased slightly from
12.2% to 13.7%.

Table 3. Mechanical properties of the AZ91 alloy, AZ91–HEA and AZ91–SiC composites (Calculation
of C.Y.S is given in Tables S1 and S2 in the Supplementary Materials).

Sample Hardness (HV) C.Y.S (MPa) Failure Strain (%)

AZ91 93 ± 2 178 ± 4 12.2 ± 0.3
AZ91–HEA 138 ± 2 209 ± 8 13.7 ± 0.5
AZ91–SiC 123 ± 8 204 ± 10 12.0 ± 0.4

4. Discussion
AZ91-based metal matrix composites reinforced by high-entropy alloys (HEA) and
SiC particles were synthesized in the present study by the spark plasma sintering (SPS)
process. The results from the strain hardening rate calculation show that the AZ91–HEA
and AZ91–SiC composites exhibited higher strain hardening rates when compared to
unreinforced AZ91 alloy (Figure 7). The dislocation densities of AZ91 and the AZ91–
HEA and AZ91–SiC composites were calculated by analyzing XRD patterns and were
determined to be ~3.9 × 1015 m−2 for all of the samples. The result showed that no
huge difference was observed in the dislocation densities of the sintered samples, and
the higher strain hardening rates in the composites were related to the reaction between
reinforcements (HEA and SiC) and dislocations. The ability of HEA and SiC to increase the
strain hardening rate may be attributed to the capacity to impede dislocation motion, which
was also observed in other Mg-based composites reinforced with ceramic particles [26].
Moreover, other strengthening mechanisms may also contribute to the enhancement of the
hardening rate.
The effect of HEA and SiC particles on the mechanical properties of the sintered
composites could be discussed in terms of different strengthening mechanisms including
grain boundary strengthening, Orowan strengthening, thermal mismatch strengthening,
load transfer and solid solution strengthening.
The increase in the yield strength due to the refinement of the grain size of the matrix in
the composites can be estimated using the following equation derived from the Hall–Petch
equation [27,28]:  
−1 −1
∆σHall−Petch = k dcom
2
− dAZ91
2
(5)

where k is the Hall–Petch coefficient (0.27 MPam−1/2 [29]), dcom and dAZ91 are the average
grain size of Mg in the composite material and AZ91, respectively. The grain sizes of Mg
in the sintered AZ91, AZ91–HEA and AZ91–SiC were 5.4, 5.3 and 5.1 µm, respectively.
Only marginal changes in grain size were observed after adding HEA or SiC particles.
From Equation (5), the increased yield strengths due to grain refinement in the AZ91–HEA
and AZ91–SiC composites were 1 and 4 MPa, respectively. The addition of HEA and SiC
particles in the composites did not cause a significant grain refinement and led to a slight
increase in yield strength.
In the current study, AZ91 rather than pure Mg was used for preparing composites,
implying that the matrix contained α-Mg solid solution rather than pure Mg. As a result,
the effect of solid solution strengthening should be examined. Impurity atoms in solid
Materials 2021, 14, 6520 10 of 15

solution can impede the movement of dislocation and increase the yield strength of the base
metal. The increase in yield strength due to solid solution strengthening can be estimated
using the following equation [30]:
2/3
∆σss = C(X2/3
com − XAZ91 ) (6)

where C equals 197 MPa [30]. Xcom and XAZ91 are the atomic percent (at%) of impurity
atom in α-Mg in the composite and AZ91, respectively. The concentration of Al in Mg
solid solution in AZ91, AZ91–HEA and AZ91–SiC were 7.31, 7.39 and 7.35at%, respectively.
From Equation (6), ∆σss in AZ91–HEA was 0.3 MPa, while that in AZ91–SiC was 0.1 MPa.
The effect of solid solution strengthening led to a slightly increase in yield strength.
The contribution of Orowan strengthening to the increment in yield strength is due to
the interaction of precipitates or reinforcements with dislocations, which can be calculated
using the following equations [26]:

Gb d
∆σOrowan = 0.5 √ ln (7)
πλ 1 − ν b
√ 
λ=d π/4f − 1 (8)

where G is the shear modulus of the matrix (16.5 GPa [31]), b is the value of the Burgers
vector of the matrix (0.32 nm [30]), d is the average diameter of the precipitate or reinforced
particles (28 µm for HEA and 38 µm for SiC), λ is the spacing between particles and f is
the volume fraction of precipitate or reinforcement. In the AZ91-based composite, both
f the precipitation of Mg17 Al12 and the distribution of reinforcements such as HEA and
SiC particles could contribute to the increasing yield strength. The addition of HEA and
SiC into AZ91 did not change the volume fraction and size of Mg17 Al12 significantly. The
volume fractions of Mg17 Al12 in the AZ91, AZ91–HEA and AZ91–SiC were 10, 10.2 and
11.7%, respectively. The particle size of Mg17 Al12 is ~0.5 µm in all of the samples. The
increasing yield strength was 8 MPa in the AZ91 alloy. After adding HEA and SiC, the
values were 8.3 and 9.2 MPa, respectively. The results indicated that the contribution
of Mg17 Al12 on the enhancement of yield strength was similar in the AZ91 alloy and
the composites. As a result, its effect could be neglected when calculating the difference
between the yield strength of AZ91 and AZ91-based composites.
Regarding the strengthening due to the dispersion of HEA and SiC particles, the
values were 0.10 and 0.12 MPa, respectively, indicating that the Orowan strengthening due
to the dispersion of HEA and SiC particles on AZ91 matrix was not the major contributor
for the increment in yield strength in the AZ91–HEA and AZ91–SiC composites. It was
reported that the size of the reinforced particle had to be less than 1 µm to obtain a strong
pinning effect of dislocation [32]. The coarse particle size of HEA and SiC resulted in a
weak pinning effect in Orowan strengthening. The particle size of HEA and SiC has to be
further refined to enhance the Orowan strengthening effect.
The thermal mismatch will lead to the generation of dislocation in the area surround-
ing the reinforced particles upon cooling after the SPS process and eventually increases
the yield strength. The enhancement of yield strength due to the mismatch of CTE can be
estimated using the following equation [33,34]:
s
√ 12fr ∆α∆T
∆σCTE = 3βGb (9)
(1 − fr )bd

where β is the strengthening coefficient (1.25 [34]), G is the shear modulus of matrix, b is
the Burgers vector, fr is the volume fraction of reinforcement, ∆α is the difference between
the coefficient of thermal expansion between the matrix and the reinforcement, ∆T is the
difference between the processing and testing temperatures and d is the diameter of the
reinforced particles.
Materials 2021, 14, 6520 11 of 15

The coefficient of thermal expansion (CTE) of AZ91, HEA and SiC are 29 × 10−6 /K,
10 × 10−6 /K and 4.7 × 10−6 /K, respectively. Clearly, there exists a difference between the
CTE of the AZ91 matrix and the reinforcements (HEA and SiC). The increment in yield
strength due to thermal mismatch in the AZ91–HEA was 10 MPa, while the increment in
Materials 2021, 14, x the AZ9–1SiC was 9.9 MPa. 12 of 16
In a composite material, load can be transferred from the matrix to the reinforcement
particles, leading to the enhancement of yield strength. The increment in yield strength as
a result of load transfer can be expressed as [34]:
∆σ 0.5f σ (10)
∆σLoad = 0.5fr σm (10)
where σm is the yield strength of the AZ91 alloy, and fr is the volume fraction of reinforce-
where m isestimated
ment.σThe the yield increments
strength of in
theyield
AZ91 alloy, and
strength fr AZ91–HEA
in the is the volume fraction
and AZ91–SiC of rein-
com-
forcement. The estimated increments
posite were 3 and 6 MPa, respectively. in yield strength in the AZ91–HEA and AZ91–SiC
composite
The were 3 and in
increment 6 MPa,
yieldrespectively.
strength caused by different strengthening mechanisms is
The increment
summarized in 4yield
in Table strengthincaused
and plotted Figure by8a. different strengthening
In the AZ91–HEA mechanisms
composite, is
the thermal
summarized in Table 4 and plotted in Figure 8a. In the AZ91–HEA composite,
mismatch effect contributed the most (69%) to the increment in yield strength, followed the thermal
mismatch effect
by the load contributed
transfer effectthe mostthe
(21%), (69%) to the increment
grain-refinement in yield
effect strength, followed
(Hall–Petch) (7%) andby the
the load transfer effect (21%), the grain-refinement effect (Hall–Petch) (7%)
Orowan effect (0.7%). A similar trend was also observed in the AZ91–SiC composite. and the Orowan
effect (0.7%). A similar trend was also observed in the AZ91–SiC composite.

Figure
Figure (a)(a)
8. 8. The increment
The increment inin
compressive
compressive yield strength
yield strengthdue
due to to
thethe
contribution ofof
contribution grain-size strengthening,
grain-size dislocation
strengthening, dislocation
strengthening
strengthening and effect
and of load
effect transfer
of load fromfrom
transfer matrix to particle
matrix in theinAZ91–HEA
to particle and AZ91–SiC
the AZ91–HEA composites.
and AZ91–SiC (b) Theoretical
composites. (b) Theo-
and measured
retical values ofvalues
and measured the increased yield strength
of the increased yield in the AZ91–HEA
strength and AZ91–SiC
in the AZ91–HEA composites.
and AZ91–SiC composites.

Table
Table 4. 4. Contribution
Contribution ofof different
different strengthening
strengthening mechanismstoto
mechanisms increasedyield
increased yield strength
strength ofof AZ91
AZ91
composites.
composites.
Sample
Sample Mechanism
Mechanism Value
Value (MPa)
(MPa)
AZ91–HEA Thermal mismatch 10.0
AZ91–HEA Thermal mismatch 10.0
AZ91–HEA
AZ91–HEA Grainboundary
Grain boundary 1.01.0
AZ91–HEA
AZ91–HEA Loadtransfer
Load transfer 3.03.0
AZ91–HEA
AZ91–HEA Orowan
Orowan 0.10.1
AZ91–HEA
AZ91–HEA Solid
Solidsolution
solution 0.30.3
AZ91–SiC Thermal mismatch 9.9
AZ91–SiC
AZ91–SiC Thermal mismatch
Grain boundary 4.09.9
AZ91–SiC
AZ91–SiC Grain boundary
Load transfer 6.04.0
AZ91–SiC
AZ91–SiC Load transfer
Orowan 0.16.0
AZ91–SiC
AZ91–SiC SolidOrowan
solution 0.10.1
AZ91–SiC Solid solution 0.1

Assuming all of the enhancement brought by various strengthening mechanisms

could be added up linearly [31,35], the total increment in yield strength of AZ91-based
composite estimated by different strengthening mechanisms can be expressed as:
Materials 2021, 14, 6520 12 of 15

Assuming all of the enhancement brought by various strengthening mechanisms

Materials 2021, 14, x 13 of 16
could be added up linearly [31,35], the total increment in yield strength of AZ91-based
composite estimated by different strengthening mechanisms can be expressed as:

As shown ∆σtheoretic
in Figure= ∆σ8b,CTE + ∆σLoadvalues
theoretical + ∆σHall Petch + ∆σin
of −increment Orowan ∆σss
yield+strength (11)
in AZ91–
HEA and AZ91–SiC composites were 14 and 20 MPa, respectively. The measured values
As shown in Figure 8b, theoretical values of increment in yield strength in AZ91–HEA
obtained from compression tests for AZ91–HEA and AZ91–SiC were 31 and 26 MPa, re-
and AZ91–SiC composites were 14 and 20 MPa, respectively. The measured values obtained
spectively. The increment in yield strength could be roughly estimated using strengthen-
from compression tests for AZ91–HEA and AZ91–SiC were 31 and 26 MPa, respectively. The
ing mechanisms.
increment in yield strength could be roughly estimated using strengthening mechanisms.
According to the theoretical calculation, the addition of 10 wt% of SiC in AZ91
According to the theoretical calculation, the addition of 10 wt% of SiC in AZ91 should
should have a slightly higher strengthening effect. However, the weakening effect due to
have a slightly higher strengthening effect. However, the weakening effect due to higher
higher porosity and weaker bonding between the matrix and reinforcement in AZ91–SiC
porosity and weaker bonding between the matrix and reinforcement in AZ91–SiC compos-
composite
ite was notwas takennotinto
taken into account
account in the calculation.
in the calculation. As shownAs shown in Figure
in Figure 3f, debonding
3f, debonding was
was observed
observed in theininterface
the interface
between between
the AZ91the matrix
AZ91 matrix
and SiCand SiC particles,
particles, implying implying
a weakera
weaker interface
interface bonding.bonding. The in
The porosity porosity in the AZ91–SiC
the AZ91–SiC (3.8%)than
(3.8%) is higher is higher
that in than that in
AZ91–HEA
AZ91–HEA (0.8%) and reduced the strength of the AZ91–SiC composite.
(0.8%) and reduced the strength of the AZ91–SiC composite. It was also observed that It was also ob-
served that the theoretical strength was lower than the measured
the theoretical strength was lower than the measured strength. The deviation may be strength. The deviation
may be attributed
attributed to the approximate
to the approximate parametersparameters
used forused
HEA,for HEA, nonuniform
nonuniform particle
particle size and size
the
and the assumption
assumption that irregular
that irregular particlesparticles
could becould
treatedbeastreated
sphericalas spherical
particles.particles.
Hardness and
Hardness and compressive
compressive yieldyield strength
strength ofof AZ91-based
AZ91-based metal metal matrix
matrix composites
composites
prepared by the powder metallurgy route in the current work and
prepared by the powder metallurgy route in the current work and from the literature from the literature are
shown in Figure 9 [35–40]. It can be seen that the hardness and
are shown in Figure 9 [35–40]. It can be seen that the hardness and strength of AZ91– strength of AZ91–HEA
composite
HEA synthesized
composite in thein
synthesized current work work
the current was superior to those
was superior in theinAZ91-based
to those the AZ91-basedcom-
posites reinforced
composites withwith
reinforced oxide, nitride
oxide, and and
nitride boride. The The
boride. harnesses of the
harnesses of AZ91
the AZ91 matrix and
matrix
HEA-reinforced
and HEA-reinforced particles were were
particles 84 and84208
andHV,208respectively.
HV, respectively.In addition to HEA’s
In addition higher
to HEA’s
hardness
higher value compared
hardness to the matrix,
value compared to the its metallic
matrix, its nature,
metallicwhich
nature,resulted
which in a betterinin-
resulted a
better interface bonding between the matrix and reinforcement (Figure 3e), also made HEAa
terface bonding between the matrix and reinforcement (Figure 3e), also made HEA
apromising
promisingreinforcement
reinforcementfor forthe
themetal
metalmatrix
matrixcomposite.
composite.

Figure 9. (a)
Figure 9. Hardness and
(a) Hardness (b) compressive
and (b) compressive yield
yield strength
strength (C.Y.S.)
(C.Y.S.) of
of AZ91
AZ91 alloy
alloy and
and AZ91-based
AZ91-based metal
metal matrix
matrix composites
composites
prepared
prepared byby powder
powder metallurgy
metallurgyroute
routein
inthe
thecurrent
currentwork
workand
andfrom
fromliteratures.
literatures.

In
In the
the present
present study,
study, we
we proposed
proposed aa new
new approach
approach by by reinforcing
reinforcing AZ91
AZ91 alloys
alloys with
with
HEA particles. Preliminary results showed that the HEA particle has potential
HEA particles. Preliminary results showed that the HEA particle has potential to be used to be used
for reinforcement in
for reinforcement in metal
metalmatrix
matrixcomposites.
composites.The The analysis
analysis performed
performed indicated
indicated thatthat
the
the particle size of HEA reinforcement should be refined to enhance its contribution
particle size of HEA reinforcement should be refined to enhance its contribution of hard- of
hardening effect of HEA. The effects of particle size, fraction of HEA and post-sintering
ening effect of HEA. The effects of particle size, fraction of HEA and post-sintering extru-
extrusion on strength
sion on strength will bewill
thebesubject
the subject
of ouroffuture
our future
study.study.

5. Conclusions
In the current work, AZ91 metal matrix composites reinforced with 10 wt% of HEA
particles were fabricated by spark plasma sintering process. AZ91–SiC composites were
Materials 2021, 14, 6520 13 of 15

5. Conclusions
In the current work, AZ91 metal matrix composites reinforced with 10 wt% of HEA
particles were fabricated by spark plasma sintering process. AZ91–SiC composites were
also synthesized for comparison of their mechanical properties. Microstructure and me-
chanical properties of the sintered composites were studied and the following conclusions
could be drawn:
1. AZ91–HEA composite with a uniform distribution of HEA particles in the matrix
could be manufactured using spark plasma sintering process. The composite consisted
of α-Mg, Mg17 Al12 and FCC phase. Phase transformation was not observed in the
sintered composite compared to the as-milled powder. No reaction layer was formed
in the interfacial region between HEA and α-Mg matrix.
2. The addition of HEA efficiently enhances hardness and compressive yield strength
(C.Y.S) of AZ91–HEA. After adding HEA particles, hardness and C.Y.S of the compos-
ite were increased by 48% and 17%, respectively.
3. In AZ91–HEA composite, thermal mismatch effect, load transfer effect and grain-
refinement effect contributed to the increment in yield strength. Among them, the
thermal mismatch effect was the major factor.
4. AZ91–HEA displayed a slightly higher C.Y.S (209 MPa) than that of AZ91–SiC (204
MPa). The strengthening effect of HEA was comparable to that of the commonly used
SiC reinforcement in metal matrix composite. The reason was due to the less porosity
and enhanced interfacial bonding between α-Mg matrix and HEA particles.

Supplementary Materials: The following are available online at https://www.mdpi.com/article/

10.3390/ma14216520/s1, Figure S1: Enlarged section of engineering compressive stress-strain curves
of AZ91-HEA composite, Figure S2: Enlarged section of engineering compressive stress-strain curves
of AZ91-SiC composite, Table S1: Compressive yield strength (C.Y.S) of AZ91-HEA composite
calculated using stress and strain curves shown in Figure S1, Table S2: Compressive yield strength
(C.Y.S) of AZ91-SiC composite calculated using stress and strain curves shown in Figure S2.
Author Contributions: Conceptualization, C.C.; methodology, C.C.; formal analysis, C.C. and H.-
H.C.; investigation, C.C. and H.-H.C.; resources, C.C.; writing—original draft preparation, C.C.;
writing—review and editing, C.C.; supervision, C.C.; funding acquisition, C.C. All authors have read
and agreed to the published version of the manuscript.
Funding: This research was funded by Ministry of Science and Technology, Taiwan under grant
number MOST 109-2221-E-011-019.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The authors confirm that the data supporting the findings of this study
are available within the article.
Acknowledgments: The authors would like to thank Shih-Hsun Chen, Nano Manufacturing and
Surface Treatment Lab, NTUST for offers of the HEA materials used in this study and for sug-
gestions. The authors would also like to thank V.K. Ranganayakulu for assisting with the spark
plasma sintering.
Conflicts of Interest: The authors declare no conflict of interest.

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