Materials Science & Engineering A 780 (2020) 139211

Contents lists available at ScienceDirect

Materials Science & Engineering A

journal homepage: http://www.elsevier.com/locate/msea

Investigation of severe plastic deformation effects on microstructure and

mechanical properties of WS2/AZ91 magnesium metal matrix composites
Aqeel Abbas , Song-Jeng Huang *
Department of Mechanical Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei, 10607, Taiwan, ROC

A R T I C L E I N F O A B S T R A C T

Keywords: AZ91 reinforced with four different concentrations (0,0.3,0.6,1)wt% of WS2 micro particles were fabricated
ECAP using stir casting method. The samples were deformed by equal channel angular pressing (ECAP) after ho­
Texture mogenization. The scanning electron microscopy and X-ray diffraction were used to investigate the micro­
Crystallite size
structure and phase composition respectively. The results reveal that rod-like precipitates produced during the
Microstrain
WS2/AZ91
homogenization process are refined and bounded in the grain boundaries by the combined effect of WS2
Mechanical properties enrichment and increasing number of passes of ECAP. The needle precipitates are eminent in 1pass 0.3 wt%WS2/
Severe plastic deformation AZ91. The β-Mg17Al12 and extracted Al particles are dissolved and secondary phases are produced by dynamic
Microstructure recrystallization after 2pass 1 wt%WS2/AZ91. The maximum crystallite size and microstrain distribution have
been observed for 1pass 0.6 wt%WS2/AZ91. The mechanical properties investigation represents that 2pass 0.6 wt
%WS2/AZ91 has optimal yield strength and ultimate tensile strength. The (22.143)%, (44.735)% and (92) %
increment in yield strength, ultimate tensile strength and elongation have been observed in 2pass 1 wt%WS2/
AZ91 compared with homogenized monolithic AZ91 alloy respectively. The maximum young’s modulus
(6696.218MPa) has been found for 1pass homogenized WS2/AZ91 and minimum (4108.165MPa) for homoge­
nized 0.6 wt%WS2/AZ91. The ECAP deformed 1pass 0.3 wt%WS2/AZ91 exhibits the maximum strain hardening
rate. The YTS, UTS, and elongation are (30.41) %, (47.6) % and (51.9)% increased after 2pass-0.6 wt%WS2/
AZ91.

1. Introduction
The world is trending to develop numerous lightweight engineering
materials that have a high strength to weight ratio for the automotive
and aviation industry [1]. Magnesium alloys have a lower density, easy
recycling and high specific strength [2]. The Mg-Al-Zn alloys are the
most commonly used and cost-effective materials because of their good
damping capacity, high strength to weight ratio, reasonable ductility,
good machinability and corrosion resistance [3]. Among this AZ series of
magnesium alloys, AZ91 alloy containing more Al contents have higher
strength and corrosion resistance. However, it has worse formability of
intermetallic compounds in stoichiometric composition along interface
boundaries. However, poor ductility restricts its application in various
industries [4]. The researchers have shifted from alloying system to
metal matrix composites (MMCs) systems to achieve the properties
which are unattainable from single materials [5].
The performance of MMCs depends on the type and composition of
reinforcement, fabrication methodology and processing techniques [5].
Several reinforcements such as SiC, Al2O3, graphene, B4C, TiC (parti­
cles/whiskers) have been manufactured using solid-state techniques
(powder metallurgy, diffusion bonding), liquid state technique (stir
casting, squeeze casting, centrifugal casting) and semi-solid state tech­
niques (chemical vapor deposition and physical vapor deposition) to get
superior mechanical properties suited for advanced application such as
automotive, communication, electronics, optoelectronics and cutting
tools [6–12]. Previous studies have proven that the size of reinforcement
has a significant role in mechanical properties as reinforcement alters
the microstructure of the matrix. The ductility is adversely affected by
the quantity of reinforcement while size and shape affect the modulus
[3,13]. Nanoscaled particles have negative effects on the ductility and
small refining effects on microstructure, if they have been pushed to gain
boundaries and agglomerated when solidified [1,14]. Microscaled par­
ticles stimulate the recrystallization, improve the strength, transmit the
load to increase the strength and randomize the texture [15,16].
Therefore during deformation micron-sized particles obviously affect
the microstructure and enhance the strength. Huang et al. [17]studied

* Corresponding author.
E-mail address: sgjghuang@mail.ntust.edu.tw (S.-J. Huang).

https://doi.org/10.1016/j.msea.2020.139211
Received 4 January 2020; Received in revised form 5 March 2020; Accepted 5 March 2020
Available online 9 March 2020
0921-5093/© 2020 Elsevier B.V. All rights reserved.
A. Abbas and S.-J. Huang
the microstructure and mechanical properties of WS2 nanotubes rein­
forced AZ61 manufactured by the stir casting method. In addition to
extrusion effects, severe plastic deformation via equal channel angular
pressing (ECAP) was analyzed on mechanical properties.
Many researchers concluded that stir casting is one of the most cost-
effective manufacturing methods for MMCs for excellent mechanical
properties and good machineability. The conventional secondary
methods such as heat treatments, extrusion, rolling, forging and ECAP
are widely used in metallic materials to obtain finer grain structure [14,
18–21]. The severe plastic deformation using ECAP on MMCs has suc­
cessfully refined the microstructure and enhance the mechanical prop­
erties by the uniform distribution of reinforcement and crystallinity. It
has been proved that it exhibits intense precipitation strengthening. Mg
having a hexagonal closed pack (HCP) crystal structure and Mg17Al12
having body-centered cubic (BCC) structure, Mg/Mg17Al12 interface is
fragile which leads to microcrack formation during ECAP. Thus, the
distribution of Mg17Al12 is very important to microstructure uniformity
and strength enhancement. J. f jiang and Q. jiang [21,22]investigated
the effects of homogenization on mechanical properties, microstructure
and dynamic recrystallization. They effectively proved that homogeni­
zation improves the mechanical properties by the uniform distribution
of Mg17Al12 and homogeneity of microstructure. Consequently, the
strategy of combining heat treatment with SPD has been developed to
improve the strength of materials [14,19]. Many researchers have
characterized the MMCs by interaction by dispersion of particles, grain
refinement, texture, dislocation and secondary phase.
In this research magnesium alloy AZ91 reinforced with WS2 micro­
particles was manufactured by stir casting method. The billets were
extruded by the ECAP technique after homogenization. The combined
effects of WS2 particles and SPD on microstructure and mechanical
properties have been investigated. Moreover, the fundamental mecha­
nism behind the microstructure important and mechanical behavior was
dissected. The developed strategy holds promising for Mg alloys with
intense precipitation strengthening mechanisms.
2. Experimental procedures
2.1. Materials and fabrication method
Micro WS2/AZ91 metal matrix composites were manufactured using
stir casting method. The detailed manufacturing method has been
explained elsewhere [23]. The magnesium alloy AZ91 is mainly
composed of 8.95 wt% Al, 0.84 wt% Zn, and 0.26 wt% Mn. The AZ91
magnesium alloy reinforced with four different concentrations (0, 0.3,
0.6 &1)wt% of WS2 was manufactured under the same processing con­
ditions. The casted ingots were transformed into billets of size (11.5✕
11.5✕ 75)mm3 using wire cutting machine. The billets were kept in
Fig. 1. (a) ECAP plastic deformation channel(b)ECAPed sample.
2
Materials Science & Engineering A 780 (2020) 139211
closed furnace at 410� C for 24h and then quenched in water for 2s. The
severe plastic deformation (SPD) process was performed using equal
channel angular pressing (ECAP) with the die having an intersection
angle of 120� as shown in Fig. 1(a). Prior to ECAP, the die was preheated
to 350 � C and billets were inserted in the channel and held for 40min for
uniform heat distribution. The ECAP plastic deformation was performed
at a deformation rate of 25 mm/min. Teflon was used as a lubricant
during the ECAP process. The route A was used to perform second pass in
ECAP. The billets were 2pass ECAPed and cracks were too eminent to
carry on further passes. The mechanical properties of ECAPed compos­
ites were compared with homogenized metal matrix composites.
2.2. Microstructure characterization
The specimen for metallographic analysis were collected from plane
Y-Z of the billets (Fig. 1(b)). Wire electrical discharge machine (EDM)
was used to cut the sample with the size 10 mm✕ 10 mm✕ 2 mm. The
specimens were ground with the standard 240, 400, 600, 1000,2000 and
4000CW emery papers to remove scratches from the surfaces and sub­
sequently polished with 1 μm alumina suspension to get mirror-like
surfaces. The samples were etched in 25 ml DI water, 75 ml ethanol,
1 ml acetic acid and 1 ml nitric acid solution for the 80s to expose the
grain boundaries.
The microstructure and surface morphology of the composites was
examined using a scanning electron microscope (SEM) equipped with
energy dispersive spectroscopy (EDS). X-ray diffractometer (Cu-Kα,
Bruker D2) was used to analyze the texture and phase composition of the
composites. Crystallite size, crystallinity, dislocation density and
microstrain distribution were determined using XRD data. The standard
metallographic procedures similar to SEM microstructure analysis
except etching was adopted to prepare a specimen for X-ray diffraction
analysis.
2.3. Mechanical characterization
All the samples used for microstructural analysis were later used to
measure microhardness. MVK-H1 machine was used to measure the
Vickers hardness under 300gmf for dwelling time of 10s. The average of
five points of each sample was used in the final results. The tensile
samples were prepared as ASTM-E8 standards. The universal testing
machine (10 KN MTS) was employed to perform uniaxial tensile tests
with a deformation rate of 0.5 mm/min. The dog-bone shaped tensile
samples were cut from plane Z-X of the billets (Fig. 1(b)) using EDM. The
specimens have 41 mm length, 6.2 mm width, 2.2 mm thickness, 14 mm
gauge length, and 14 mm shoulder radius. Three tensile samples were
tested under the same conditions and medians were taken into account
for final results.
A. Abbas and S.-J. Huang Materials Science & Engineering A 780 (2020) 139211

3. Results

3.1. Microstructure evaluation

The XRD patterns of homogenized, ECAPed 1-pass and 2-pass metal

matrix composites are shown in Figs. 2–4 respectively. It can be seen
that diffraction peaks of homogenized and plastically deformed MMCs
are consist of solid solution of α-Mg, Mg37.5Al25Zn37.5, β-Mg17Al12,
Mg2Al3, Al5Mn3 and Mg-Zn.
It is clear from Figs (2)–(4) that α-Mg and Mg37.5Al25Zn37.5 based
solid solution peaks are more prominent in diffractogram. Small peaks of
β-Mg17Al12 have been observed in homogenized samples (Fig. 2) which
indicate the small amount of precipitates after solid solution. The peak
intensity for solid solution Mg and Mg2Al3(Fig. 2) decreases with the
increase in WS2 concentration which is an indication of the dissolution
of Mg2Al3 in α-Mg.
The decrease in trend in peak intensity of solid solution of α-Mg,
Mg37.5Al25Zn37.5 has noted up to 0.6 wt%WS2/AZ91 homogenized
MMCs and further enrichment causes the increase in peak intensity. The
amount of precipitates decreases for ECAPed WS2/AZ91 MMCs, as
diffraction peaks for Mg (Mg37.5Al25Zn37.5) are stronger in homogenized
Fig. 3. XRD analysis of ECAPed 1-pass WS2-AZ91 MMCs.
MMCs than ECAPed but 2-pass 1 wt%WS2/AZ91 has the highest peak
intensity for above-mentioned phases. Interestingly, WS2 concentration
has caused the enhancement in Mg (Mg37.5Al25Zn37.5) peaks in 1-pass
WS2/AZ91 MMCs (Fig. 3) but oppressing effects in 2-Pass up to 0.6 wt
%WS2/AZ91 MMCs and uplifted for 2-pass 1 wt%WS2/AZ91 drastically
(Fig. 4).
The 2pass 1 wt%WS2/AZ91 has a relatively stronger basal (0002)
texture and weak ð1010Þ texture. A clear deformation texture ð1010Þ has
been observed in all WS2/AZ91 MMCs from which diffraction peaks
increase (Fig. 3). The peaks for homogenized and 1pass 1%WS2/AZ91
are shifted to the right as compared to other composites due to the in­
crease in lattice parameters owing to alloying elements. In order to
investigate the ECAP effects on the texture of the basal plane, I (0002)
and Ið1010Þ were chosen to denote the intensity of the basal plane and
pyramidal plane peak. So the relative intensity of the basal plane can be
achieved by I (0002)/I ð1010Þ. The values of I (0002)/I ð1010Þ were
found to be much higher for 2-pass ECAPed composites than homoge­
nized samples which indicate the restoration of stronger basal plane
through dynamic recrystallization (DRX) [24]. The degree of crystal­
linity was computed for homogenized and ECAPed WS2/AZ91 MMCs
and is presented in Fig. 5. The degree of crystallinity is significantly

Fig. 4. XRD analysis of ECAPed 2-pass WS2-AZ91 MMCs.

affected by severe plastic deformation caused by ECAP and WS2 con­

centration. For homogenized composites, crystallinity increases with
WS2 concentration and was found maximum for 0.6 wt%WS2/AZ91. The
crystallinity of 2-passed ECAP WS2/AZ91 composites decreases with the
increase in WS2 contents and was found minimum for 0.6 wt%
WS2/AZ91.
To quantify the effects of severe plastic deformation along with WS2
concentration on AZ91 alloy, the contribution of crystallite size, dislo­
cation density, and microstrain distribution to peak broadening were
assumed to be independent. The crystallite size of the composites was
determined by Scherer equation (Eq. (1))
L ¼ Kλ=βCosθ (1)

Where L is crystallite size, K is Scherer constant (0.9) λ is X-ray wave­

length (1.5406 Å), θ is the Bragg’s angle and β is the full-wave half
maximum (FWHM). Microstrain was determined using the Williamson-
Hall method (Eq. (2)) from XRD data.
Κλ
βCosθ ¼ þ 4εSinθ (2)
Fig. 2. XRD Analysis of homogenized WS2-AZ91 MMCs. L

3
A. Abbas and S.-J. Huang
Fig. 5. Crystallinity variation with ECAPed and Homogenized WS2-
AZ91 MMCs.
βCosθ was plotted against 4Sin θ and slope was take as microstrain.
The ORIGIN software was used to analyze the data and the least square
curve fitting was used to determine the slope of the curve. The dislo­
cation density was measured using equation (3)
3:4641ε
ρ¼ (3)
Lb
where ρ is dislocation density, L is crystallite size, b is burger vector
(Mge 0.325 nm) and ε is microstrain. The crystallite size of homoge­
nized and ECAPed WS2/AZ91 MMCs is presented in Fig. 6. It can be
visualized that the crystallite size of homogenized 0.6 wt%WS2/AZ91 is
minimum and 2-passed 1%WS2/AZ91 has maximum crystallite size. The
average crystallite size of 2Pass-WS2/AZ91 is increased up to 0.6 wt%
WS2 addition and sharply decreases for 1 wt% which is due to recrys­
tallization caused by WS2 addition during ECAP process. The average
crystallite size for 1Pass-WS2/AZ91 first decreases for 0.6 wt% WS2/
AZ91 and the increment has been noticed for 1 wt%WS2/AZ91.
Average microstrain distribution in the homogenized and ECAPed
Fig. 6. Crystallite size variation with ECAPed and Homogenized WS2-
AZ91 MMCs.
4
Materials Science & Engineering A 780 (2020) 139211
composites is presented in Fig. 7. Homogenized 0.6 wt%WS2/AZ91 in­
dicates the maximum microstrain distribution and 1-pass 1 wt%WS2/
AZ91 shows the minimum microstrain. From Figs. 2 and 3, it is noted
that peak is shifted to a higher angle for homogenized and 1-pass 1 wt%
WS2/AZ91 composites. The dislocation density of homogenized and
ECAPed composites is presented in Fig. 7. The dislocation density varies
inversely with crystallite size as mentioned in equation (3).
The surface morphology of homogenized and ECAPed WS2/AZ91
composites presented in Fig. 9, Fig. 10 and Fig. 11 respectively. The
α-Mg and secondary phases are distributed in rod-like precipitates inside
the grains for homogenized WS2/AZ91 composites (Fig. 9). The spher­
ical shaped secondary phases including Mg2Al3 and Al are dispersed
inside the grain boundaries and between the rod-like precipitates.
Agglomeration has been observed in homogenized 1 wt%WS2/AZ91 as
marked by the blue circle in Fig. 9(d).
The spherical shaped secondary phases are dissolved in the grains
with the increase in WS2 concentration. The rod-like precipitates are
broken into smaller and finer particle shaped precipitates. For homog­
enized 0.6 wt%WS2/AZ91 composites, the precipitates become wider
and thinner. It is clear that rod-like precipitates are originated at
different angles in different grains (Fig. 9(a)). The rod like precipitates
are centered from different directions and lead to small finer one (Fig. 9
(c)).
The SEM morphology of 1-pass WS2/AZ91 MMCs is shown in Fig. 10.
The microstructure of WS2/AZ91 composites has been changed after 1-
pass ECAP and significant refinement in grain size and precipitation has
been observed. The Al particles are extracted and dispersed in the vi­
cinity of grain boundaries after 1pass ECAP of 0.3 wt%WS2/AZ91
(Fig. 10(b)). The grains start dividing with an increase in WS2 percent­
age. Some rod-like precipitates are more prominent in 1pass-0.6 wt%
WS2/AZ91 composites which are reshaped into the petal-like structure
with 1 wt% addition of WS2.
The morphology of 1 wt%WS2/AZ91 composites composed of long
broken rods and smaller pieces of the precipitates. Every longer or short
precipitates have cracks, indicating the deformation caused by the se­
vere plastic deformation. The solid solution of Mg2Al3 and
Mg37.5Zn37.5Al25 are more prominent phases in 1pass 1 wt%WS2/AZ91
composite. Fig. 11 shows the SEM micrographs of 2-pass WS2/AZ91
composites. It is very interesting to analyze the microstructure of 2-Pass
WS2/AZ91 composites that Al particles are extracted on the surface of
grains which are spherical and lamellar in shape. The rod-like pre­
cipitates oriented in different directions have become wide and thick in
0.3 wt%WS2/AZ91 composites. The average thickness of the rod is 2.28
Fig. 7. Micro strain variation with ECAPed and Homogenized WS2-
AZ91 MMCs.
A. Abbas and S.-J. Huang
Fig. 8. Dislocation density variation with ECAPed and Homogenized WS2-
AZ91 MMCs.
μm and gapped 3.67 μm from each other. The spherical Al particles and
secondary phases are dissolved or mixed in fine needle-like precipitates
in 0.3 wt%WS2/AZ91. The further addition of 0.6 wt%WS2 contents
leads to the complete dissolution of Al particles in the matrix. The rod-
like precipitates became wider and thick but are constrained inside the
grain boundaries. The precipitates are oriented at an angle varying from
102� to 160� . The addition of 1 wt% WS2 breaks the precipitates inside
the grain boundaries and tiny Al particles are dissolved in solid solution.
It is evident from Fig. 9–11 that the equiaxed grain boundaries are
developed with the increase in number of passes and higher angle grain
boundaries are transformed from sub-grain boundaries. In coarse-grain
regions, DRX was not provoked since rod-shaped precipitates are not
Fig. 9. SEM images of Homogenized (a)0 wt% (b) 0.3 wt% (c) 0.6 wt% and (d) 1 wt% of WS2/AZ91.
5
Materials Science & Engineering A 780 (2020) 139211
broken. The diameter of these precipitates ranges from 1.8 μm to 6.99
μm in length. The results indicate that non-uniform growth of discon­
tinuous precipitates colonies at grain boundaries took place under se­
vere plastic deformation, revealing significant heterogeneous
precipitation.
3.2. Microhardness distribution
The Vickers hardness for all homogenized and ECAPed composites is
presented in Fig. 12. One can easily analyze that 2-pass WS2/AZ91
MMCs have higher micro-hardness values as compared to homogenized
composites. The hardness of homogenized composites escalates with the
higher concentration of WS2 and reaches the maximum value (84.6HV).
The further enrichment of 1 wt%WS2 causes a reduction in microhard­
ness to 81.12 HV. An almost similar trend has been observed for 1-pass
WS2/AZ91 MMCs and maximum value (86.58HV) was observed for 1 wt
%WS2/AZ91.
The micro-hardness is linearly proportional to the number of passes
and WS2 concentration. The maximum hardness (94.66HV) has been
measured for 2-pass 1 wt%WS2/AZ91. After 2-passes of severe plastic
deformation by ECAP for 1 wt%WS2/AZ91 MMCs, 10.46% microhard­
ness is increased than homogenized 1 wt%WS2/AZ91. The composites
enforced with higher WS2 contents have higher hardness than mono­
lithic AZ91.
3.3. Mechanical characterization
The typical stress-strain curves for homogenized, 1-pass and 2-pass
ECAPed WS2/AZ91 MMCs are presented in Figs. 13–15 respectively.
All mechanical properties including yield tensile strength (YTS), ulti­
mate tensile strength (UTS), ductility, and elastic modulus are summa­
rized in Table 1. As depicted in Fig. 13 that the addition of 0.3 wt%WS2
causes the maximum ductility in homogenized AZ91 alloy. A continuous
increment in true strain has been noted with negligible enhancement in
stress. The phenomenon is referred to as pop-in behavior which happens
A. Abbas and S.-J. Huang Materials Science & Engineering A 780 (2020) 139211

Fig. 10. SEM images of ECAPed -1Pass (a)0 wt% (b) 0.3 wt% (c) 0.6 wt% and (d) 1 wt% WS2/AZ91.

Fig. 11. SEM images of ECAPed -2Pass (a)0 wt% (b) 0.3 wt% (c) 0.6 wt% and (d) 1 wt%WS2/AZ91.

when the plastic zone crossed the grain boundaries [25]. The further enhancement in YTS for homogenized 1 wt%WS2/AZ91 has been
addition of WS2 contents leads to a decrease in ductility and ultimate observed as 8.173% when compared to homogenized monolithic AZ91
tensile strength (UTS). In contrast to UTS in homogenized composites, alloy.
yield strength (YS) increases with increase in WS2 concentration. The Fig. 14 presents the stress-strain behavior of 1-pass WS2/AZ91

6
A. Abbas and S.-J. Huang
Fig. 12. Micro-Hardness distribution of Homogenized and ECAPed WS2-
AZ91 MMCs.
Fig. 13. True Stress-Strain relationship for Homogenized WS2-AZ91 MMCs.
composites. It can be concluded that ductility and UTS are directly
related to WS2 concentration. The increase in WS2 contents causes the
enhancement in yield strength also. The 1-pass 0.6 wt%WS2/AZ91 MMC
exhibits maximum YS(93.398MPa). A similar trend has been observed
for 2-pass WS2/AZ91 MMCs also. After analyzing the data available in
Table 1, it can be concluded that the composites under consideration
exhibit an increase in strength and decrease in elongation in contrast to
previous work by Pan et al. [26], in which both strength and ductility
increases as the number of passes increases.
The trend is ascribed by grain refinement and volume fraction
β-Mg17Al12. The YTS, UTS and elongation for 1 wt%WS2/AZ91 in ho­
mogenized conditions are 93.468MPa, 175.402MPa and 16.1% respec­
tively. They are respectively increased to 104.317 MPa, 210.3 MPa,
14.44% after 2-pass ECAP. It can be visualized from Table 1 that young’s
modulus for homogenized composites decreases with the increases in
WS2 contents and 0.6 wt%WS2/AZ91 shows the minimum value
(4108.165MPa). After 1pass ECAP, young’s modulus decreases with
WS2 enrichment and reaches 5017.967MPa for 1 wt%WS2 addition. The
7
Materials Science & Engineering A 780 (2020) 139211
Fig. 14. True Stress-Strain relationship for ECAPed 1-Pass WS2-AZ91 MMCs.
Fig. 15. True Stress-Strain relationship for ECAPed 2-Pass WS2-AZ9.
young’s modulus decreases with enhancing the concentration of WS2
and 0.6 wt%WS2/AZ91 exhibits maximum modulus (6627.507MPa).
The highest YTS (111.380MPa) and UTS (214.7MPa) have been ob­
tained after 2-pass 0.6 wt%WS2/AZ91 MMCs. The YTS, UTS, and elon­
gation are 30.41%, 47.6% and 51.9% after 2pass-0.6 wt%WS2/AZ91 as
compared with homogenized monolithic AZ91 alloy which indicates the
combined effects of severe plastic deformation and reinforcement (WS2).
The ductility is increased for 1pass ECAP and then reduced for 2 pass
which may be due to the presence of the eutectic Mg17Al12 phase which
remained undissolved during ECAP.
The work hardening behavior of WS2/AZ91 MMCs have been
assessed by strain hardening rate as follows (Eq. (4))
dσt
θ¼ (4)
dεt
The work hardening rate as a function of true plastic stress is pre­
sented in Fig. 16. In general, all materials exhibit similar decreasing
work hardening tendency except 2- pass 0.6 wt%WS2/AZ91 which
A. Abbas and S.-J. Huang Materials Science & Engineering A 780 (2020) 139211

Table 1
Mechanical Properties (Summary).
Sample/ 0.2%Yield Ultimate Modulus Strain at strain
Property strength Tensile (MPa) peak hardening
(MPa) Strength (mm/ capacity
(MPa) mm) (Hc)

0 wt% 85.406 145.3 5725.914 0.075 0.7013

WS2-
AZ91-
HM
0.3 wt% 86.761 192.7 4399.247 0.258 1.221
WS2-
AZ91-
HM
0.6 wt% 76.035 178.6 4108.165 0.218 1.3489
WS2-
AZ91-
HM
1 wt% 93.468 175.402 5429.622 0.161 0.8766
WS2-
AZ91-
HM
0 wt% 80.032 153.719 6696.218 0.076 0.9207
Fig. 16. Work-hardening rate versus true stress under uni-axial tension for
WS2-
AZ91- homogenized and ECAPed WS2-AZ91 MMCs.
1Pass
0.3 wt% 86.763 157.458 5663.931 0.098 0.8148 dissolved in a very short period of heating (40min) and facilitated by
WS2-
severe plastic deformation [27]. The rod-shaped precipitates formed
AZ91-
1Pass during heat treatments play an important role during deformation.
0.6 wt% 93.398 194.0 5283.462 0.164 1.0771 Fracture is started mostly from the precipitates and dispersion could
WS2- improve the ductility. The addition of 1 wt%WS2 along with 2passed
AZ91- ECAP dissolves the Mg2Al3 transformed phases including spherical and
1Pass
1 wt% 91.125 207.846 5017.967 0.205 1.2809
rod-like precipitates. The texture change has been observed for the in­
WS2- crease in concentration along with the number of passes.
AZ91- The wider peaks for crystalline phases indicate a higher degree of
1Pass crystallinity for homogenized WS2/AZ91 composites (Fig. 2). Severe
0 wt% 84.936 162.0 5936.220 0.092 0.9073
plastic deformation along with WS2 contents affect the crystal structure,
WS2-
AZ91- enhance the crystallite size (Fig. 6) and reduces the degree of crystal­
2Pass linity as indicated by sharp diffraction peaks in XRD patterns of 2-passed
0.3 wt% 103.654 198.6 5853.760 0.143 0.916 WS2/AZ91 composites (Fig. 4).
WS2- Comparing the crystallite size (Fig. 6) with major peaks in XRD
AZ91-
2Pass
diffraction patterns of major phases present in homogenized and ECA­
0.6 wt% 111.380 214.7 6627.507 0.156 0.9276 Ped WS2/AZ91 composites (Figs. 2, 3&4), it can be concluded that
WS2- crystallite size is linearly related with peak intensity [28]. However, the
AZ91- rule is not valid for polycrystalline materials in which heterogeneous
2Pass
phases affect the crystallite size and microstrain distribution. The WS2
1 wt% 104.317 210.3 5414.398 0.144 1.016
WS2- enrichment affects the peak intensity of major phases which leads to
AZ91- varying the crystallite size accordingly. Dislocation density, the small­
2Pass ness of crystallite size, peak broadening, phase heterogeneity, residual
stresses, precipitations and inclusions are the major reasons [29]. The
microstrain is directly related to dislocation density and inversely
designates that plasticity behavior of all materials is almost same. As
related to crystallite size. The increase in WS2 contents and higher
shown in Fig. 15, homogenized 0.6 wt%WS2/AZ91 has minimum work
plastic deformation via ECAP leads to a reduction in dislocation density
hardening which is attributed to the uniform distribution of Mg17Al12
(Fig. 8), so microstrain distribution. The reduction in crystallite size
that causes higher plasticity in Mg alloys.
causes an increase in microstrain and dislocation density. Higher con­
centration hinders the dislocation movements which maps the higher
4. Discussions
microstrain and lower crystallite size [30]. After 2-passed ECAP, dislo­
cation density tends to reduce leading higher crystallite size. The pres­
AZ magnesium alloys contain aluminum contents in the form of
ence of WS2 in AZ91 alloys leads to enhance dislocation density which
Mg17Al12 precipitates which are formed during solidification of the al­
causes the breakdown of rod precipitates into smaller pieces. The pre­
loys. β-Mg17Al12 has significant role in determining the mechanical
cipitates were refined and well broken into tiny particles, webbed by
behavior and workability of MMCs. It is generally believed that ho­
centered rod-like structures. The results indicate that nonuniform
mogenization heat treatment includes a solid solution and precipitates
growth of discontinuous precipitation colonies leads to heterogeneous
the secondary phases [27].
precipitation.
During the process of homogenization heat treatment, the solubility
The substantial grain refinement and precipitates breakdown are
of Al in the Mg matrix increases as the temperature is increased. Al exists
caused by lattice defects DRX based grain refinement, new grains are
in the form of β-Mg17Al12 at grain boundaries and is dissolved in α-Mg
developed during deformation at initial grain generated by severe
supersaturated solid solution gradually, in the subsequent cooling as
plastic deformation as well as dynamic recrystallization (DRX) [27,31].
small particles [20]. It is worth noting that precipitates are formed
This leads to bimodal grain size distribution during the early stages of
during 24h of homogenization but during ECAP, precipitates are

8
A. Abbas and S.-J. Huang
deformation. It has been proven that smaller grain size can easily eject
the Al atoms from supersaturated solution to form the more uniform
supersaturated solution (Fig. 10(c)) [32].
Moreover, dynamic recrystallization occurring during the ECAP
limits grain growth which leads to homogeneity and normal distribution
of the grains [33]. The higher sever plastic deformation caused by ECAP
leads to breakdown of rods into smaller pieces and refines the micro­
structure. The observation suggests that particle simulation mechanism
activates DRX by fine precipitates.
In the first pass, coarse grains are broken into many fine grains in a
specific direction surrounded by the large grains and form bimodal
structure. The rapid change happens after one pass which is related to
the high rate of dislocation formation.
Therefore, at higher number of pases of ECAP, grain refinement
become less effective and hence the strength. The grain growth is limited
when higher angle grain boundaries are transformed to sub grains when
DRX is occurred. The normal distribution and homogeneity of the grains
interpret the recrystallization during ECAP [34]. The large deformation
causes contnious DRX which leads to the higher volume fraction of fine
grains. The effects of multiple ECAP on grain refinement can be analyzed
by comparing the texture softening and strengthening effects of grains.
J. sun et al. [35] found the relation between the texture softening and
reducing YTS. They claimed that texture softening has more effects than
YTS. Since there are limited number of slip planes in the material, a high
fraction of the plane rotates to favor the direction for the slip.
The trend in the hardness of WS2/AZ91 composites can be attributed
to the combined effects of refinement caused by ECAP and reinforce­
ment. The change in hardness of WS2/AZ91 MMCs with the number of
passes along with WS2 contents is good agreement with microstructural
evaluations.
The reason for the decrease in hardness for homogenized 1 wt%WS2/
AZ91 composites can be ascribed as some large precipitates absorb some
smaller ones. The enhancement in hardness could be due to grain
refinement as well as dissolution and distribution of β-phase [36]. It
should be noted that β-phases are brittle and hard phases distributed at
grain boundaries. It is proved that metal having HCP structures such as
Mg exhibit stronger grain size dependency of strength and hardness due
to lack of slip systems [3]. The fluctuation in hardness is likely due to the
existence of some non-crystalline region and higher grain size and
massive β phases.
The linear increase in ductility of homogenized 0.3 wt%WS2/AZ91
composite is caused by plastic strains which are localized by severe
plastic deformation. This leads to micro-cracking and grain detachment
[37]. This phenomenon is a major reason for pop-in behavior (Fig. 13).
The pop-in behavior may exist both in crystalline and amorphous solids.
The curve below the pop-in behavior is purely fitted which means that
deformation below pop-in is purely elastic. When dislocation is acti­
vated, it increases the dislocation density. The interaction of dislocation
with other sources causes continuous deformation [30].
Being body-centered cubic (BCC) Mg17Al12 is incompatible with the
hexagonal closed pack (HCP) matrix which causes the nucleation of
micro-crack at the interface of Mg17Al12 during tensile deformation. The
growth and coalescence of micro-cracks cause premature failure. The
vibrant behavior has been observed in the stress-strain curve of 2pass
WS2/AZ91 composites (Fig. 15) which indicates the elastic-plastic
deformation and load transfer mechanism between soft matrix to hard
reinforcement. The enhanced properties of WS2/AZ91 mainly rely on
homogeneous dispersion of WS2 particles. It is thermodynamically
predicted that WS2 particles have been dispersed in the Mg matrix
during the casting process due to Vander Walls forces between particles
and liquid matrix [38].
In following the ECAP process, shear deformation has significant role
in dispersion and redistribution of particles. The strip like precipitates
become thinner and broken into small pieces with an increase in the
number of passes of ECAP. The temperature during ECAP is assumed to
be the effective parameter for redistribution of precipitates [39].
9
Materials Science & Engineering A 780 (2020) 139211
Mechanical properties are significantly improved by severe plastic
deformation due to grain refinement induced by dynamic recrystalli­
zation and rearrangements of agglomeration. The YTS of the composites
can be computed by summation of YTS of the matrix plus the
load-bearing capacity of reinforcement, coefficient of thermal expansion
(CTE) mismatch, Orowan strengthening and Hall-Petch strengthening
[9]. The Orowan strengthen can be predicted as below (Eq. (5))
pffiffiffiffiffi 1ndp
Gb
Δ τ ¼ 2 πλ1 ν
(5)
r0
Where, r0 the radius of dislocation, dp is effective inter-plane spacing, G
is shear modulus (16.5GPa) of the magnesium, ν is poison ratio (0.35)
and b is burger vector (0.325). The improvement in tensile strength can
also be attributed to grain refinement and is explained by Hall-Petch
relation as given below (Eq. (6))
σy σ0 þ Kd
1
2 (6)
Where σy is yield strength and d is the diameter of the grain. σ0 and K are
the materials parameters. It is believed that grain boundaries possess
significant obstacles to dislocation motion and smaller grain sizes have
higher grain boundaries which could lead to enhance strength. The
average grain size of plastically deformed material is decreased as
deformation twin refinement and dynamic recrystallization which leads
to the formation of secondary phases. The improvement in the
strengthening of AZ91 alloy is limited by these brittle secondary phases
which make subsequent plastic deformation more difficult. If one can
press fit the tiny cracks and refine the secondary phases via plastic
deformation (Fig. 10), the mechanical strength could be improved. The
hot deformation causes the DRX in the composite. The mechanical
properties are improved by grain refinement [40]. The different rod-like
precipitates or plate-like precipitates (Fig. 11) and spherical precipitates
(Fig. 10) were also found which were more likely to be developed during
contnious ECAP deformation. The precipitated particles hinder the
dislocation motion during deformation caused by ECAP. As deformation
continued, dislocations start accumulation around the particles which
provide enough nucleation sites for DRX. Therefore, spherical shaped
precipitates become larger in size and are present abundant around the
grain boundaries.
The metastable phases are spread densely inside the grain. The
enhancement in amount and size of these phases is caused by particle
addition and lead to precipitate hardening [41]. The increased work
hardening has an advantage in both strengths. The ductility of MMCs
reinforced with micro-scaled ceramic particles is low, although they
possess high strength. This happens due to coarse ceramic particles form
the stress concentration at the particles-matrix interface which further
leads to micro-cracks initiation and propagation [15].
Additionally, there may be microcracks in coarse reinforcement
which may cause cracks initiation inside and propagate throughout the
reinforcement. For the nano-scaled reinforcement, the enhancement in
ductility is limited because the behavior of the nanoparticles is non-
separable in metal matrix composites [42]. The ductility of the com­
posite is dependent on volume fraction, size, shape of particles.
The tensile strength of metal matrix composites can be calculated as
(Eq. (7))
σ c ¼ f σr þ ð1 fÞσm (7)
Where f is weight/volume fraction of reinforcement, σm is the tensile
strength of matrix and σr is the tensile strength of reinforcement. The
reduction in strength for 2pass-1wt%WS2/AZ91 might be related to high
porosities and high concentration of reinforcement which causes lower
crystallinity. The enhancement in elastic modulus is due to stiffening
properties of Mg and WS2 and uniform distribution of particles at a
higher ECAP passes.
It has been investigated that microstructure has marked effects on
A. Abbas and S.-J. Huang
work hardening and ductility. In AZ91 Mg alloys higher ductility and
strength are correlated with crystallinity, Mg17Al12, grain refinement
severe plastic deformation. The higher contents of WS2 increases the
interaction between the dislocation movement with severe plastic
deformation and strengthen the composites [10,43]. Moreover, the
spring-like behavior of work hardening curves is caused dislocation
network generated around the reinforcement particles to form disloca­
tion forest and activate dislocation hardening mechanism. The strain
hardening capacity has been computed to analyze the work hardening
ability and weakening behavior of WS2/AZ91 composites by using the
necking section of the uniaxial tensile test. The strain hardening capacity
of homogenized and ECAPed WS2/AZ91 MMCs is presented in Table 1
and can be calculated as (Eq. (8))
σUTS σYTS σUTS
Hc ¼ ¼ 1 (8)
σYTS σYTS
Where σUTS is ultimate tensile strength and σ YTS is 0.2% offset yield
strength.
5. Conclusion
In summary, WS2/AZ91 composites were homogenized and sub­
jected to two-pass ECAP with120� ECAP die. The addition of WS2 par­
ticles and applications of severe plastic deformation have a significant
role in microstructure refinement and mechanical properties enhance­
ment of AZ91 alloy. Based on the results of WS2 addition along with
ECAP, it can be concluded as.
1. The addition of WS2 particles along with ECAP has strong effects to
break long precipitates into the shorter petal-like structure in
1pass1wt%WS2/AZ91 and bounded inside the grain boundaries in 2
pass1wt%WS2/AZ91.
2. The spherical shaped Al particles, Mg17Al12, and Mg2Al3 are uni­
formly dispersed at grain boundaries after 1pass ECAP which leads to
a decrease in ductility and above-mentioned phases are dissolved
after 2 pass which leads to decrease in ductility.
3. The 2pass 0.6 wt%WS2/AZ91 has the highest YTS and UTS due to
reduced agglomeration, improved uniform distribution of WS2 par­
ticles, grain refinement, and increased strain hardening rate.
4. The (22.143) %, (44.735) % and (92) % increment in YTS, UTS, and
elongation has been noted in 2pass 1 wt%WS2/AZ91 as compared to
homogenized monolithic AZ91 alloy as combined effects of ECAP
and WS2.
5. After 2passWS2/AZ91 exhibit vibrant stress-strain cure before frac­
ture because of elastic-plastic fracture.
6. The microhardness is increased with an increase in WS2 contents
along with SPD and 2pass1wt%WS2/AZ91 has a maximum hardness
(94.66HV).
7. The maximum elastic modulus (6696.218MPa) has been observed in
1pass monolithic AZ91.
Declaration of competing interest
I certify that no funding has been received for the conduct of this
study and/or preparation of this manuscript. I also affirmed that there is
no actual or potential conflict of interest in relation to this article with
co-authors and any institution.
CRediT authorship contribution statement
Aqeel Abbas: Conceptualization, Data curation, Formal analysis,
10
Materials Science & Engineering A 780 (2020) 139211
Investigation, Methodology, Writing - original draft, Writing - review &
editing. Song-Jeng Huang: Supervision, Visualization.
References
[1] Y. Jin, K. Wang, W. Wang, P. Peng, S. Zhou, L. Huang, T. Yang, K. Qiao, B. Zhang,
J. Cai, Mater. Char. 150 (2019) 52–61.
[2] K. M� athis, J. Gubicza, N. Nam, J. Alloys Compd. 394 (2005) 194–199.
[3] B. Sahoo, S. Panigrahi, Mater. Char. 139 (2018) 221–232.
[4] P.K. Krishnan, J.V. Christy, R. Arunachalam, A.-H.I. Mourad, R. Muraliraja, M. Al-
Maharbi, V. Murali, M.M. Chandra, J. Alloys Compd. 784 (2019) 1047–1061.
[5] A. Ramanathan, P.K. Krishnan, R. Muraliraja, J. Manuf. Process. 42 (2019)
213–245.
[6] Q.-h. Yuan, D.-m. Fu, X.-s. Zeng, L. Yong, Trans. Nonferrous Metals Soc. China 27
(2017) 1716–1724.
[7] Q.-h. Yuan, Z.-q. Qiu, G.-h. Zhou, X.-s. Zeng, L. Luo, X.-X. Rao, Y. Ding, Y. Liu,
Mater. Char. 138 (2018) 215–228.
[8] U.K.A.V. Kumar, Mater. Today: Proceedings 4 (2017) 1140–1146.
[9] S.J. Huang, A. Abbas, B. Ball� okov� a, J. Mater. Res. Tech. 8 (5) (2019) 4273–4286.
[10] S.-J. Huang, A.N. Ali, Mater. Sci. Eng. A 711 (2018) 670–682.
[11] M. Qadir, Y. Li, C. Wen, Acta Biomater. 89 (15) (2019) 14–32.
[12] H. Liao, J. Chen, L. Peng, J. Han, H. Yi, F. Zheng, Y. Wu, W. Ding, Mater. Sci. Eng. A
683 (2017) 207–214.
[13] L. Tang, Y. Zhao, R. Islamgaliev, C.Y. Tsao, R. Valiev, E. Lavernia, Y. Zhu, Mater.
Sci. Eng. A 670 (2016) 280–291.
[14] X. Qiao, T. Ying, M. Zheng, E. Wei, K. Wu, X. Hu, W. Gan, H. Brokmeier, I. Golovin,
Mater. Char. 121 (2016) 222–230.
[15] J. Sun, Z. Yang, J. Han, H. Liu, D. Song, J. Jiang, A. Ma, Mater. Sci. Eng. A 734
(2018) 485–490.
[16] F. Aydin, Y. Sun, M.E. Turan, Powder Metall. Met Ceram. 57 (2019) 564–572.
[17] S.-J. Huang, C.-C. Lin, J.-Y. Huang, R. Tenne, Adv. Mech. Eng. 10 (2018),
1687814017753442.
[18] W. Yu, X. Wang, H. Zhao, C. Ding, Z. Huang, H. Zhai, Z. Guo, S. Xiong, J. Alloys
Compd. 702 (2017) 199–208.
[19] L. Zheng, H. Nie, W. Liang, H. Wang, Y. Wang, J. Magnes. Alloys 4 (2016)
115–122.
[20] X. Wang, X. Hu, W. Liu, J. Du, K. Wu, Y. Huang, M. Zheng, Mater. Sci. Eng. A 682
(2017) 491–500.
[21] J.-f. Jiang, L. Xin, W. Ying, J.-j. Qu, S.-j. Luo, Trans. Nonferrous Metals Soc. China
22 (2012) 555–563.
[22] Q. Jiang, H. Wang, B.-X. Ma, Y. Wang, F. Zhao, J. Alloys Compd. 386 (2005)
177–181.
[23] S.-J. Huang, A. Abbas, J. Alloys Compd. (2019), 153321.
[24] E. Tolouie, R. Jamaati, Mater. Lett. 249 (2019) 143–146.
[25] K. Deng, C. Wang, X. Wang, K. Wu, M. Zheng, Mater. Des. 38 (2012) 110–114.
[26] H. Pan, G. Qin, M. Xu, H. Fu, Y. Ren, F. Pan, Z. Gao, C. Zhao, Q. Yang, J. She,
Mater. Des. 83 (2015) 736–744.
[27] C. Wang, A. Ma, J. Sun, H. Liu, H. Huang, Z. Yang, J. Jiang, J. Alloys Compd. 793
(2019) 259–270.
[28] F. Kiani, C. Wen, Y. Li, Acta Biomater. 103 (2019) 1–23.
[29] H. Jafarzadeh, K. Abrinia, Mater. Char. 102 (2015) 1–8.
[30] Z. Yang, A. Ma, H. Liu, D. Song, Y. Wu, Y. Yuan, J. Jiang, J. Sun, Mater. Char. 152
(2019) 213–222.
[31] S. Khani, M. Aboutalebi, M. Salehi, H. Samim, H. Palkowski, Mater. Sci. Eng. A 678
(2016) 44–56.
[32] X. Liu, J. Sun, F. Zhou, Y. Yang, R. Chang, K. Qiu, Z. Pu, L. Li, Y. Zheng, Mater. Des.
94 (2016) 95–104.
[33] E. Dogan, S. Wang, M. Vaughan, I. Karaman, Acta Mater. 116 (2016) 1–13.
[34] K. Nie, X. Wang, K. Deng, F. Xu, K. Wu, M. Zheng, J. Alloys Compd. 617 (2014)
979–987.
[35] J. Sun, Z. Yang, J. Han, T. Yuan, D. Song, Y. Wu, Y. Yuan, X. Zhuo, H. Liu, A. Ma,
J. Alloys Compd. 780 (2019) 443–451.
[36] B. Sahoo, F. Khan, S. Babu, S. Panigrahi, G.J. Ram, Mater. Sci. Eng. A 724 (2018)
269–282.
[37] K.K. Alaneme, E.A. Okotete, J. Magnes. Alloys 5 (2017) 460–475.
[38] A. Abbas, S.J. Huang, B. Ball� okov�a, K. Sülleiov�a, Tribol. Int. 142 (2020), 105982.
[39] A.M. Jorge Jr., E. Prokofiev, M.R.M. Triques, V. Roche, W.J. Botta, C.S. Kiminami,
G.I. Raab, R.Z. Valiev, T.G. Langdon, Int. J. Hydrogen Energy 42 (2017)
21822–21831.
[40] Q. Xu, A. Ma, B. Saleh, Y. Li, Y. Yuan, J. Jiang, C. Ni, Mater. Sci. Eng. A 771 (2020),
138579.
[41] D. Song, A. Ma, J. Jiang, P. Lin, D. Yang, J. Fan, Corrosion Sci. 53 (2011) 362–373.
[42] Y. Yuan, A. Ma, X. Gou, J. Jiang, G. Arhin, D. Song, H. Liu, Mater. Sci. Eng. A 677
(2016) 125–132.
[43] S.-J. Huang, A.N. Ali, J. Mater. Process. Technol. 272 (2019) 28–39.