Materials Science & Engineering A 745 (2019) 450–459

Contents lists available at ScienceDirect

Materials Science & Engineering A

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

Microstructure and mechanical properties of AZ31 magnesium alloy sheets T

processed by constrained groove pressing
⁎
Zongshen Wanga, , Yanjin Guanb, Tao Wangb, Qian Zhanga, Xiuting Weia, Xiaoying Fanga,
Guangming Zhua, Shan Gaoc
a
School of Mechanical Engineering, Shandong University of Technology, Zibo 255000, PR China
b
School of Materials Science and Engineering, Shandong University, Jinan 250061, PR China
c
School of Materials Science and Engineering, Shandong University of Technology, Zibo 255000, PR China

A R T I C LE I N FO A B S T R A C T

Keywords: Constrained groove pressing (CGP) is of great potential for fabricating ultra-fine grained (UFG) sheet metals
AZ31 magnesium alloy sheets based on severe plastic deformation. However, researches on CGP of materials with poor formability and low
Constrained groove pressing ductility at room temperature (RT) are still very limited. Thus, in this work, an experimental setup with heating
Severe plastic deformation systems was developed for an improved processing efficiency by virtue of its new die design. CGP of AZ31
Microstructure
magnesium alloy sheets were performed at RT, 423, 473, 523 and 573 K. Their cracking behavior and the effects
Mechanical properties
of pass number and processing temperature on the evolutions of their microstructure and mechanical properties
were studied in detail. The results showed that the number of effective pressings gradually increased with
processing temperature. Only one pass including four pressings could be finished at 423 K, and twins inside
initial grains and dislocation cells were observed in the end. Two passes could be conducted to the materials at
temperatures higher than 423 K, and bimodal structures formed due to the occurrence of dynamic re-
crystallization (DRX) and experienced various evolutions. The microstructure evolution of the materials was
dominated by continuous DRX, and a relatively refined and homogeneous UFG microstructure was achieved at
473 K after two passes. In this situation, the average grain size was refined to 2.81 µm from the as-annealed
6.92 µm, and subgrains sized about 1 µm were observed. The influence of pass number on tensile properties
gradually decreased with processing temperature. Work hardening, grain refinement and texture modification
together decided the evolution of mechanical properties of the alloy sheets during CGP. The optimum com-
prehensive mechanical properties with yield strength of 240 MPa, tensile strength of 295 MPa, elongation to
failure of 18.5% and average microhardness of 73.9 HV were achieved at 473 K during the second pass. In
addition, the strong basal texture of the as-annealed sheets initially with a maximum intensity of 18.05 was
decreased to 10.61 at 473 K while no significant change was made when processed at higher temperatures.

1. Introduction moderate or high temperatures [5,6]. Therefore, lots of efforts have

Nowadays, the need of utilizing more lightweight materials in
aerospace and automobile structures is increasing for the purpose of
cutting emission and fuel consumption [1–3]. Being one of the lightest
commercialized metallic structural materials, magnesium and its alloys
exhibit tremendous potential in weight saving due to their low density
and high specific strength [4]. However, the industrial applications of
magnesium alloys are greatly restricted by their poor formability and
low ductility at room temperature (RT) associated with their hexagonal
close-packed (HCP) crystal structure and insufficient slip systems, and
the high production costs of wrought magnesium alloys generally at
been devoted to improve the formability and ductility of magnesium
alloys in order to make full use of their benefits. It is well established
that both strength and ductility of the materials can be effectively en-
hanced by grain refinement and, until now, severe plastic deformation
(SPD) methods have proven to be of great potential for achieving ultra-
fine grained (UFG) structure in materials and improving their physical,
chemical and mechanical properties [7].
Constrained groove pressing (CGP), originally developed by Shin
et al., is one of the most promising SPD methods suitable for producing
UFG sheet or plane metallic materials with superior properties [8,9].
During CGP, a set of asymmetrically groove dies and a set of flat dies

⁎
Corresponding author.
E-mail address: wangzsh@sdut.edu.cn (Z. Wang).

https://doi.org/10.1016/j.msea.2019.01.006
Received 17 October 2018; Received in revised form 31 December 2018; Accepted 2 January 2019
Available online 03 January 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
Z. Wang et al. Materials Science & Engineering A 745 (2019) 450–459

Fig. 1. Schematic illustration of CGP process.

are employed to perform alternately groove pressing and flattening on properties like ductility and formability of magnesium and its alloys
sheet metals, as shown in Fig. 1. By virtue of the constraint from the die through grain refinement and texture modification is of great interest
walls, the asymmetry of the groove dies and the 180° rotation of the and attracting more and more attention. However, only a small number
sheet sample around its normal direction (ND), theoretically, pure shear of papers have been published to verify the availability of CGP to
deformation under plane strain condition will be imposed into the process magnesium alloys, and the knowledge about the influences of
whole sheet sample without any changes in its dimensions. Therefore, a pass number and processing temperature on the evolutions of their
large amount of plastic strain can be uniformly accumulated into the microstructure and mechanical properties is still not comprehensive.
materials by repeating this process and, finally, a relatively homo- Thus, in this work, a high-efficiency experimental setup with heating
geneous UFG structure can be obtained and the properties are expected systems was newly developed for performing CGP on sheet metals
to be significantly improved. Accordingly, the groove pressed sample having poor formability and low ductility at RT. Then, the cracking
consists of inclined shear regions (SRs) and flat undeformed regions behavior and evolutions of microstructure and mechanical properties of
(URs), as shown in Fig. 1(b). In fact, there are interface regions (IRs) AZ31 magnesium alloy sheets during CGP were systematically studied,
between SRs and URs causing strain inhomogeneity during practical and the influence mechanism of pass number and processing tem-
deformation process [10]. Additionally, the die structure parameters perature was explored and discussed in detail.
including groove width (T) and groove angle (θ) are of great im-
portance to the evolutions of microstructure, mechanical properties and
2. Experimental materials and procedures
strain distribution of the CGPed materials, as shown in Fig. 1(a), and
the process could be optimized by choosing a proper combination of the
2.1. Materials preparation and CGP experiment
parameters [11].
Obviously, CGP process needs simpler tooling design and is much
The hot-rolled AZ31 magnesium alloy sheets with dimensions of
easier to perform, as compared to other SPD methods [9]. Thus, it offers
100 mm × 100 mm × 2 mm were used in this experiment, and their
great potential in fabricating large-volume UFG sheet metals and, till
chemical compositions are Mg-3.1Al-0.8Zn-0.3Mn (wt%). Before CGP,
now, it has been successfully utilized for grain refinement and property
the sheets were fully annealed at 573 K for 1 h to homogenize their
improvement of various pure metals and alloys. Nevertheless, most
initial microstructure. Fig. 2 shows the experimental setup for CGP
investigations are focused on metallic materials having face-centered
process on a 5000 kN computer-controlled electro-hydraulic servo
cubic (FCC) crystal structure as well as good ductility while there are
compression testing machine. As seen in Fig. 2(a), the dies could be
limited reports about CGP of materials exhibiting low formability at RT
heated to the desired temperature ( ± 5 K) by the built-in heating rods
such as magnesium and its alloys. Ratna Sunil et al. firstly adopted CGP
and, before pressing, the sheet samples were placed between the top
to achieve fine grain size in AZ31 magnesium alloy, and investigated
and bottom dies and stabilized to the processing temperature. The
the influence of microstructure evolution and surface features on
sample temperature was calibrated by a thermocouple probe, as shown
wettability, corrosion resistance, in-vitro bioactivity and cell adhesion
in Fig. 2(b). Previously, an experimental setup with heating systems for
of the materials [12]. It was found that CGP was a potential method to
CGP of AZ31 magnesium alloy sheets was developed by Fong et al. [5].
enhance bioactivity and control degradation of magnesium alloys for
In their work, the groove and flat dies were used interchangeably and,
implant applications. Fong et al. [5] developed a directly orthogonal
for each pressing, the sheet samples were removed from the dies, cooled
CGP procedure involving four groove pressings with a 90° rotation of
in air and reheated in the dies. Thus, the processing and handling times
the sheet sample around its ND after each pressing and a final flat-
required were very long, which reduced the processing efficiency.
tening, and examined the effects of deformation path and temperature
Meantime, when reheating the sheets, the effects of static recovery and
on microstructure, texture and mechanical properties of AZ31B-O
static recrystallization as well as grain growth on their microstructure
magnesium alloy sheets. It implied that deformation path did not sig-
evolution should be considered. Thus, in this experimental setup, a new
nificantly impact the degree of grain refinement, and the new path
die design was firstly employed for a higher efficiency. As shown in
introduced higher strain amount while lower strain homogeneity due to
Fig. 2(b), the groove and flat dies were mounted on the same upper/
its complicated stress and strain fields. Afterwards, the microstructure
lower shoes. The groove pressing and flattening could be conducted
stability during isothermal annealing of AZ31 magnesium alloy pro-
simultaneously and, after pressed by one set of dies, the sample could
cessed by CGP, and the tensile flow behavior at moderately high tem-
be immediately placed to another set for the next pressing. In this way,
peratures of the CGPed and post-annealed alloy sheets were in-
the exchange of the groove/flat dies and the repeat heating of the sheet
vestigated in two separate works carried out by Fong et al. [2,3].
samples were avoided. Thus, the processing efficiency was greatly im-
As mentioned above, applying CGP to improving the mechanical
proved and the heating effect when reheating could be neglected. Here,

451
Z. Wang et al.
Fig. 2. The (a) experimental apparatus and heating systems, (b) groove and flat dies, and sheet samples for CGP process.
the groove dies had a groove angle of 45° and a groove width of 2 mm
which was equal to the sample thickness, and molybdenum disulfide
was chosen as the lubricant. A constant press speed of 5 mm/min was
used in this experiment. When pressing, the groove direction (GD) of
the groove dies was perpendicular to the rolling direction (RD) of the
sheet samples, as illustrated in Fig. 1. Theoretically, by adopting the die
structure parameters mentioned above, an equivalent plastic strain of
about 1.16 could be uniformly accumulated into the sheet sample after
one CGP pass including two groove pressings and two flattenings.
2.2. Materials characterization
Optical microscopy (OM), electron backscatter diffraction (EBSD)
and transmission electron microscope (TEM) were employed to ex-
amine the microstructure and texture evolutions of AZ31 magnesium
alloy sheets during CGP. The OM specimens were mechanically po-
lished and then etched for 30 s using a solution of 1 g oxalic acid, 1 mL
acetic acid, 1 mL nitric acid, and 150 mL distilled water. For EBSD
analysis, small specimens were extracted from the sheet thickness cross
section parallel to its RD and mechanically polished to achieve fine
surface finish. Then, the specimens were electro-polished with a mix-
ture of perchloric acid, ethanol and water. The EBSD observations were
conducted on a Hitachi S-3400N scanning electron microscopy (SEM)
equipped with an HKL-EBSD system. An area of at least
100 µm × 100 µm for each specimen was investigated using a step-size
of 0.3 µm, and the analysis of EBSD maps was undertaken by the HKL
CHANNEL 5.0 software package. For TEM observations, specimens
were cut from the central region of the sheet plane and conventionally
prepared by mechanical polishing and ion thinning. The observations
were performed on an FEI Tecnai G2 F20 S-TWIN field emission TEM
operated at 200 kV.
In order to explore the evolution of tensile properties of AZ31
magnesium alloy sheets, uniaxial tensile tests were carried out at RT on
a CMT5205 electronic universal testing machine with a constant cross
head speed of 3 mm/min. The specimens were machined with gage
Fig. 3. The (a) optical microstructure, (b) EBSD map and (c) {0001} pole figure of the as-annealed AZ31 magnesium alloy sheet sample.
452
Materials Science & Engineering A 745 (2019) 450–459
dimensions of 25 mm × 6 mm× 2 mm according to ASTM E8M stan-
dard, and the gage length was aligned to be perpendicular to the RD of
the sheet samples. Each test was repeated three times to obtain re-
presentative results. Vickers microhardness tests were accomplished
using an HV-1000 Vickers hardness tester at a load of 200 g applied for
10 s. For each sample, ten measurements were taken for an average.
3. Results and discussion
3.1. Initial microstructure of the as-annealed materials and their cracking
behavior during CGP
Fig. 3 shows the optical microstructure, EBSD map measured from
RD-ND plane and {0001} pole figure of the as-annealed AZ31 magne-
sium alloy sheet sample. As shown in Fig. 3(a), the microstructure of
the as-annealed materials mainly consisted of equiaxed grains, and the
average grain size was about 6.92 µm according to the statistical result
based on the EBSD map shown in Fig. 3(b). It can be seen from Fig. 3(b)
and (c) that the as-annealed sheet sample exhibited a strong {0001}
basal texture with a maximum intensity of 18.05, indicating the c-axes
of most grains nearly parallel to ND of the sheet sample.
In this experiment, the as-annealed magnesium alloy sheets were
processed at RT, 423, 473, 523 and 573 K, respectively, to investigate
the influence of processing temperature on the evolutions of micro-
structure and mechanical properties of the materials, and the cracking
behavior of the alloy sheets during CGP is presented in Table 1. Clearly,
the processing temperature had a substantial influence on the cracking
propensity of the sheets. Firstly, CGP of the as-annealed magnesium
alloy sheets could not be accomplished at RT due to their poor form-
ability and low ductility. Secondly, the number of effective pressings
gradually increased with the temperature. For example, only four
pressings (one pass) could be performed on the sheets at 423 K before
fractured while they could experience two passes of CGP at 473 K only
with micro-cracks and crack growth occurring during the second pass.
In this experiment, the cracking usually occurred during groove
Z. Wang et al. Materials Science & Engineering A 745 (2019) 450–459

Table 1
Cracking behavior of AZ31 magnesium alloy sheets during CGP at different temperatures.
Temperature/K Groove 1 Flat 1 Groove 2 Flat 2 (Pass 1) Groove 3 Flat 3 Groove 4 Flat 4 (Pass 2)

RT Fractured – – – – – – –
423 No cracks No cracks Micro-cracks Micro-cracks Fractured – – –
473 No cracks No cracks No cracks No cracks Micro-cracks Micro-cracks Crack growth Crack growth
523 No cracks No cracks No cracks No cracks No cracks No cracks Micro-cracks Micro-cracks
573 No cracks No cracks No cracks No cracks No cracks No cracks Micro-cracks Micro-cracks

pressing at the regions near the groove corners and subjected to the
most severe loading condition, which was in accordance with the pre-
vious reports [11,13,14]. Finally, at higher temperatures of 523 and
573 K, two passes of CGP were successfully carried out on the sheets
without distinct cracks appeared at the sheet surface. It has been known
that the poor ductility of magnesium alloys was attributed to the highly
anisotropic dislocation slip behavior [15]. Plastic deformation of the
alloys at RT occurred almost entirely by basal slip providing only two
independent slip systems. Additional non-basal slip systems such as
prismatic and pyramidal slips were easily activated at higher processing
temperatures due to the significantly reduction in their lower critical
resolved shear stress [5,16]. Thus, by increasing the processing tem-
perature, more non-basal slip systems were activated to accommodate
further plastic deformation of the materials, and more effective press-
ings were achieved. Thus, in the following sections, no more than two
passes of CGP were considered to investigate its effect on the micro-
structure and mechanical properties of AZ31 magnesium alloy sheets.

Fig. 4. The optical and TEM micrographs of AZ31 magnesium alloy sheets processed by CGP at (a, b) 423 K after one pass, (c) 473 K after one pass, (d, e) 473 K after
two passes, (f) 523 K after one pass, (g, h) 523 K after two passes, (i) 573 K after one pass, (j, k) 573 K after two passes.

453
Z. Wang et al.
3.2. Microstructure and texture evolutions
Fig. 4 represents the optical and TEM micrographs of AZ31 mag-
nesium alloy sheets processed by CGP at different temperatures. It can
be seen from Fig. 4(a) that the grain refinement of the materials pro-
cessed at 423 K after one pass was negligible except that many twins
appeared inside some initial grains. Correspondingly, only dislocation
cells with their boundaries exhibiting tangled configuration were found
in the TEM micrograph shown in Fig. 4(b). In general, the grain re-
finement of magnesium alloys during SPD was characterized by the
nucleation of dynamic recrystallization (DRX) fine grains along the
original grain boundaries and twin boundaries [17]. Previous studies
revealed that DRX in magnesium alloys occurred when deformed in the
temperature range from about 420–600 K, which was available for the
consideration of microstructure evolution during ECAP [18–20]. Thus,
for AZ31 magnesium alloy processed by CGP at 423 K in this work, DRX
was not observed after one pass and no further deformation could be
conducted due to its poor formability and low ductility. At 473 K after
one pass, besides more twins, new DRX fine grains appeared at grain/
twin boundaries consuming the coarse matrix grains and a bimodal
microstructure was developed, as shown in Fig. 4(c). It is well known
that the grain refinement of magnesium alloys was greatly influenced
by initial grain size [21]. There was a critical value of the initial grain
size deciding whether a homogeneous or a bimodal microstructure
formed during SPD, and this critical grain size was between 3 and 9 µm
for AZ31 magnesium alloy processed by ECAP at 473 K [21–23]. For
initial grain sizes larger than the critical value, a bimodal grain struc-
ture was developed at the initial stages of ECAP and gradually trans-
formed to be homogeneous afterwards. Similar results were also seen in
this investigation on CGP of AZ31 magnesium alloy sheets, and the
critical grain size in this situation was no more than 6.92 µm. With
increasing strain, as can be seen from Fig. 4(d), more new DRX grains
formed, and a further refined and homogenized microstructure with
few twins and some initial coarse grains was observed after two passes
of CGP at 473 K. Meanwhile, subgrains with an average size of around
1 µm were obtained in Fig. 4(e). Due to more non-basal slip systems
activated at higher temperatures of 523 and 573 K, no twins were found
in the deformed microstructure, even after only one pass, as shown in
Fig. 4(f) and (i), respectively. At 523 K, slightly larger average grain
sizes were evident after one and two passes in Fig. 4(f) and (g), com-
pared with those at 473 K presented in Fig. 4(f) and (i), respectively,
despite that the microstructure was further refined and homogenized by
a higher strain amount after two passes. Moreover, there was no sig-
nificant difference in substructure between Fig. 4(e) and (h) re-
presenting the TEM micrographs of the materials deformed at 473 and
523 K, respectively. As shown in Fig. 4(i) and (j), the grain growth was
more significant when the materials were processed at a higher tem-
perature of 573 K. Nevertheless, the microstructure experienced further
coarsening with increasing strain, especially for the new DRX fine
grains, which differed from the situations at 473 and 523 K. Corre-
spondingly, subgrains with clear boundaries and a larger average size of
around 3 µm were observed in Fig. 4(k).
In fact, there were some discrepancies in the bimodal structures
developed by CGP at 473, 523 and 573 K after one pass, as shown in
Fig. 4(c), (f) and (i), respectively, and these bimodal structures ex-
perienced various evolutions with CGP passes. According to the grain
refinement model of magnesium alloys during ECAP proposed by Fig-
ueiredo and Langdon, both the initial coarse grain size and the size of
fine grains formed by DRX played key roles in microstructure evolution
of magnesium alloys during SPD, and the later was dependent upon the
processing parameters such as temperature and speed [23]. In this ex-
periment, the initial grain size and pressing speed were kept constant so
the size of new DRX grains influenced by processing temperature must
not be neglected. Generally, when processed at a higher temperature,
the newly formed grains were larger in size and occupying a larger
volume fraction after one pass. Thus, compared to the initial coarse
454
Materials Science & Engineering A 745 (2019) 450–459
grains, the size of the new DRX grains were smaller when processed at a
lower temperature of 473 K, as shown in Fig. 4(c), as well as a smaller
volume fraction of these new grains after one pass, leading to a bimodal
structure even after two passes. In practice, the critical grain size, which
was small enough for homogeneous nucleation throughout the original
grains, was associated with the grain size at which non-basal slip was
activated when processing [23]. Despite the identical initial grain
structure, the processing parameters may lead to different values of the
critical grain size, and generally the critical size increased with in-
creasing the processing temperature [21]. Therefore, owing to the
higher processing temperature of 523 K, the critical grain size, the
average size and volume fraction of new DRX grains might simulta-
neously increase, resulting into fewer passes of CGP for homogenizing
the microstructure [21]. However, the remarkable inhomogeneity of
microstructure appeared again at a higher processing temperature of
573 K. This may indicate that the extent of grain growth overpassed
that of DRX occurred in the materials processed by CGP at this tem-
perature. Additionally, in this investigation, the capability of CGP in
grain refinement of AZ31 magnesium alloy sheets was confirmed. If
processed at a proper temperature like 473 or 523 K by two passes of
CGP, a relatively homogeneous UFG microstructure as well as improved
properties could be attained in the materials.
For further examination of the influence of processing temperature
on microstructure and texture evolutions of AZ31 magnesium alloy
sheets during CGP, Fig. 5 gives the EBSD and boundary structure maps,
misorientation angle distribution and {0001} pole figures of the sheets
processed after two CGP passes at different temperatures. It can be
clearly seen that the processing temperature was of great importance to
grain refinement and orientation evolution of the CGPed materials.
According to the statistical results from the EBSD maps, the average
grain size of the materials was refined from 6.92 µm to 2.81 and
4.75 µm at 473 and 523 K, respectively, while increased to 8.95 µm at
573 K, as shown in Fig. 5(a-c). Obviously, the most effective grain re-
finement was obtained at 473 K after two passes of CGP while at 573 K a
larger average grain size was observed compared to that of the as-an-
nealed materials. In Fig. 5(a), a large number of new DRX fine grains
were found with their orientations very close to the initial coarse matrix
grains. With increasing temperature, the volume fraction of new DRX
grains gradually increased, as seen in Fig. 5(b) and (c) and the grain
coarsening was more remarkable at 573 K, which is consistent with the
observation of optical microstructure shown in Fig. 4(g) and (j). In the
boundary structure maps shown in Fig. 5(d-f), the black line indicates
high angle grain boundaries (HAGBs), the green line indicates low
angel boundaries (LAGBs), and the color line indicates different types of
twin boundaries. Correspondingly, Fig. 5(g-i) present the misorienta-
tion angle distribution of the materials processed at 473, 523 and 573 K,
respectively, and the misorientation angles less than 2° were excluded.
Firstly, as can be seen from Fig. 5(g), three significant peaks were ob-
served with the angles ranging from 2° to 10°, near 30 and 86° related to
the LAGBs, {10−11}-{10−12} double twins and {10−12} tensile
twins, respectively [24]. Obviously, the amounts of {10−12} tensile
twin boundaries at both 523 and 573 K were lower than that at 473 K,
attributing to more non-basal slip systems activated to accommodate
further plastic deformation at higher temperatures, as shown in
Fig. 5(d-i). Meantime, the fraction of LAGBs slightly increased with the
temperature and the LAGBs were mainly observed inside the coarse
grains at 573 K shown in Fig. 5(f). The highest frequency of HAGBs
(72.1%) and average misorientation angle (37.0°) appeared in the
materials processed at 473 K, as seen in Fig. 5(g).
Based on the EBSD data, {0001} pole figures of the CGPed materials
at 473, 523 and 573 K were also given in Fig. 5(g-i), respectively. As can
be seen in Fig. 5(g), the texture exhibited a characteristic with the c-
axes of some grains rotating to be almost parallel to the TD of the sheet
sample. This may be caused by the appearance of {10−12} tensile
twins introducing a rotation of about 86° for grains towards the TD of
the sheet sample. Although the basal texture still existed, a much lower
Z. Wang et al. Materials Science & Engineering A 745 (2019) 450–459

Fig. 5. The EBSD and boundary structure maps, misorientation angle distribution and {0001} pole figures of AZ31 magnesium alloy sheets processed after two CGP
passes at 473 (a, d and g), 523 (b, e and h) and 573 K (c, f and i), respectively.

Fig. 6. Engineering stress-strain curves of AZ31 magnesium alloy sheets processed by CGP at (a) 423, (b) 473, (c) 523 and (d) 573 K, respectively.

455
Z. Wang et al.
Fig. 7. Tensile properties of AZ31 magnesium alloy sheets processed by CGP at (a) 423, (b) 473, (c) 523 and (d) 573 K, respectively.
maximum intensity of 10.61 was obtained after processed by two passes
of CGP at 473 K, compared to the as-annealed sheet sample. Actually,
during CGP, especially for groove pressing, the inclined SRs of the sheet
sample were subjected to not only pure shear strain but also compres-
sion strain along ND and tension strain at RD-TD [5]. In this experi-
ment, the constraint of the sheet sample along its TD was not per-
formed, which was also named semi-CGP in previous reports [25,26]. In
this procedure, slight flow along TD of the sample was allowed, prob-
ably resulting into the occurrence of {10−12} tensile twins and the
weakened basal texture. However, at higher temperatures of 523 and
573 K, strong basal textures similar to that of the as-annealed sample
appeared again with the maximum intensities of 19.45 and 20.97,
owing to the higher volume fractions of new DRX grains whose or-
ientations were close to the initial grains [27].
3.3. Mechanical properties
Fig. 6 presents the engineering stress-strain curves of AZ31 mag-
nesium alloy sheets processed by CGP at (a) 423, (b) 473, (c) 523 and
(d) 573 K, respectively. The corresponding tensile properties are given
in Fig. 7. The as-annealed sheet sample expressed the yield strength and
tensile strength of about 181 and 270 MPa, respectively, and its elon-
gation to failure was around 21%. As shown in Fig. 6(a) and Fig. 7(a),
after one pass of CGP at 423 K, both the yield strength and tensile
strength experienced remarkable increase to 245 and 300 MPa, re-
spectively, while the elongation decreased greatly to 9%. With in-
creasing processing temperature, the increase of strength and the de-
crease of elongation were gradually weakened, and the effect of pass
number on the tensile properties of the materials became not very
significant. After two passes, the yield strength and tensile strength
were increased to 230 and 280 MPa at 473 K, and 230 and 285 MPa at
523 K, as shown in Fig. 7(b) and (c), respectively. Similar elongations to
failure of 16% and 17% were obtained at 473 and 523 K. However, as
seen in Fig. 6(d) and Fig. 7(d), the variation of the tensile properties
against pass number was negligible at 573 K, and the yield strength,
tensile strength and elongation to failure were 205 MPa, 270 MPa and
19%, which were comparable to the as-annealed materials.
456
Materials Science & Engineering A 745 (2019) 450–459
The tensile tests demonstrated that the processing temperature
significantly influenced the RT tensile properties of the CGPed mag-
nesium alloy sheets. It is well established that the mechanical properties
of magnesium alloys were mainly affected by grain refinement and
texture modification [6]. As discussed above, the grain refinement was
not significant at 423 K, thus, the increase of strength accompanied by
the remarkable decrease of elongation was mainly attributed to the
work hardening. It should be noted that the tensile curves and prop-
erties of the sheet sample after the first flattening were also illustrated
in Fig. 6(a) and Fig. 7(a), respectively. Interestingly, despite the in-
complete CGP process as well as inhomogeneous strain distribution at
this stage, the deformed materials still exhibited increased yield
strength and tensile strength of 230 MPa and 295 MPa, respectively,
and a high elongation to failure of about 18%. After the first flattening,
as illustrated in Fig. 1(c), the CGP process was still uncompleted with
SRs and URs alternately existing in the sheet sample. Theoretically, it
was expected that the plastic strain would be localized in the un-
hardened URs and the tensile properties were similar to those of the as-
annealed materials. Actually, a certain amount of plastic strain was
accumulated into the URs, which contributed to the increased strength
and the reduced but still high elongation. When the temperature was
increased to 473 K, both the yield and tensile strength experienced
gradual increase, and the decrease of the elongation was not as dra-
matic as that at 423 K. As shown in Fig. 7(b), the improved tensile
properties were obtained after the third flattening with yield strength of
240 MPa, tensile strength of 295 MPa and elongation to failure of
18.5%. According to the Hall-Petch relationship, the strength of poly-
crystalline materials was inversely proportional to the square root of
their grain size [28]. The grain refinement was most effective in this
situation, as shown in Fig. 5, which resulted into the optimum tensile
properties for the processed materials. Meanwhile, the texture mod-
ification influencing the change of Schmid factor had an opposite effect
to the variation of the strength. As well known, the yield strength was
greatly dependent on the Schmid factor of basal slip, and a larger
Schmid factor was more beneficial to the basal slip, contributing to the
decrease of the yield strength [6,21]. Fig. 8 represents the Schmid
factors of basal slip for the as-annealed and CGPed sheet samples at
Z. Wang et al.
Fig. 8. The Schmid factors of basal slip for (a) the as-annealed and CGPed sheet samples at (b) 473 K, (c) 523 K and (d) 573 K after two passes.
473, 523 and 573 K after two passes. Obviously, the average Schmid
factor for the as-annealed sample was 0.23, and it gradually increased
to 0.25 with an almost even distribution from 0 to 0.5 after processed at
473 K, as shown in Fig. 8(a) and (b). Thus, at this temperature, the grain
refinement dominated the increase of the strength while the grain re-
finement together with the texture modification contributed to the re-
latively high ductility [29]. With increasing temperature, the DRX and
grain growth became more significant and the effect of grain refinement
was weakened. At 573 K, a highest average Schmid factor of 0.29 was
obtained, indicating the ignorable final effect of this thermomechanical
treatment on the tensile properties of the materials.
Fig. 9 shows the effects of pass number and processing temperature
on the average microhardness of AZ31 magnesium alloy sheets. In this
experiment, the as-annealed materials had an initial microhardness of
about 66.8 HV. As seen in Fig. 9, a dramatic increase to about 82.8 HV
was obtained at 423 K after one pass, which was caused by the domi-
nated work hardening effect. CGP at higher temperatures induced
gradual increase of microhardness with pass number. Similar variation
trends were observed for the materials processed at 473 and 523 K, and
the final average microhardness of about 75.5 and 77.8 HV were
Fig. 9. Average microhardness of AZ31 magnesium alloy sheets processed by
CGP at different temperatures.
457
Materials Science & Engineering A 745 (2019) 450–459
obtained after two passes, respectively. At 573 K, the microhardness
experienced slight fluctuation and finally increased to about 71.4 HV.
Obviously, the variation of average microhardness of the materials
against pass number and processing temperature agreed very well with
that of the yield strength, as shown in Fig. 7.
3.4. Different stages of plastic deformation during CGP
In order to further investigate the microstructure evolution and
explore the plastic deformation mechanism of AZ31 magnesium alloy
sheets during CGP, the EBSD band contrast maps of the sheet samples
processed at 523 K for different stages and regions are shown in Fig. 10.
Correspondingly, based on the EBSD data from Fig. 10, the average
grain size, aspect ratio and misorienation angle as well as frequency of
HAGBs of the samples are listed in Table 2. It should be noted that, in
the band contrast maps, the black line indicates HAGBs and the green
line indicates LAGBs, and the high quality of the maps suggests high
reliability of the EBSD data.
As can be seen from Fig. 10(a), some LAGBs were already observed
inside initial coarse grains after the first flattening, indicating a small
amount of plastic deformation was accumulated in the theoretically
URs. This also confirmed the increased strength and reduced but high
ductility of the materials at this stage, as illustrated in Fig. 7. In the SRs
shown in Fig. 10(b), more LAGBs appeared and new fine grains formed
along the initial grain boundaries resulting into the necklace-like ar-
rangement also mentioned as bimodal structure [30]. This revealed the
typical characteristics of continuous DRX during this stage of CGP [31].
When a whole pass was conducted to the materials, the grains became
more equiaxed and the frequency of LAGBs decreased, as shown in
Fig. 10(c) and Table 2. This could be interpreted by the unique de-
formation characteristics of CGP, that is, the reversal of shear direction
between every two pressings in the same plane resulted into the partly
restoration of equiaxed grains [32]. During the second pass, similar
microstructure evolution was observed with a further grain refinement,
as shown in Fig. 10(d-f).
Evidently from the EBSD data in Table 2, it can be seen that the
Z. Wang et al. Materials Science & Engineering A 745 (2019) 450–459

Fig. 10. The EBSD band contrast maps of the sheet samples processed at 523 K: (a) URs and (b) SRs after two pressings, (c) after four pressings, (d) URs and (e) SRs
after six pressings, and (f) after eight pressings.

Table 2 not be carried out at RT and only one pass could be finished at
The average grain size, aspect ratio and misorienation angle as well as fre- 423 K. At temperatures higher than 473 K, two passes including
quency of HAGBs of the sheet samples processed at 523 K for different stages eight pressings could be successfully conducted on the sheets.
and regions. (2) The capability of CGP in grain refinement and property improve-
Pass number Average Average Average Frequency of ment of AZ31 magnesium alloy sheets was confirmed. A relatively
grain size aspect misorienation HAGBs /% refined and homogeneous UFG microstructure was achieved at
/μm ratio angle /° 473 K after two passes. The average grain size was refined to
Flat 1 URs 7.67 1.79 34.7 70.8
2.81 µm from the as-annealed 6.92 µm, and subgrains sized about
SRs 5.19 1.77 18.3 35.6 1 µm were observed. Correspondingly, the superior comprehensive
Flat 2 (Pass 1) 5.62 1.74 26.4 58.9 mechanical properties with yield strength of 240 MPa, tensile
Flat 3 URs 7.29 1.76 24.6 40.7 strength of 295 MPa, elongation to failure of 18.5% and average
SRs 3.74 1.71 24.2 51.5
microhardness of 73.9 HV were obtained in this situation, as
Flat 4 (Pass 2) 4.75 1.71 27.2 66.4
compared with the as-annealed yield strength of 181 MPa, tensile
strength of 270 MPa, elongation to failure of 21% and average
average grain size was decreased to 4.75 µm after the final pass while microhardness of 66.8 HV.
the microstructure was still inhomogeneous throughout the whole (3) Only twins inside initial grains and dislocation cells were observed
process. This was also demonstrated by the average aspect ratio higher at 423 K. Owing to the occurrence of DRX, bimodal structures
than 1.71 although it gradually decreased with pass number indicating formed at higher processing temperatures and experienced various
an improvement of deformation homogeneity. In addition, both the evolutions with CGP passes. The microstructure evolution was
average misorienation angle and the frequency of HAGBs experienced dominated by continuous DRX. The microstructure inhomogeneity
firstly decrease and then recovery during the whole process, as listed in existed throughout the whole process despite some improvement
Table 2. This further confirmed that the microstructure evolution was with increasing pass number.
dominated by continuous DRX in this work. At the initial stages of CGP, (4) The influence of pass number on tensile properties gradually de-
the dislocation accumulation and subgrain formation contributed to the creased with processing temperature. At 423 K, a significant im-
above decrease. Then, the subsequent increase of DRX fine grains ac- provement of strength accompanied by a great decrease of elon-
counted for the recovery of the average misorienation angle and the gation occurred due to work hardening and negligible grain
frequency of HAGBs. refinement. At 473 and 523 K, acceptable strength with high elon-
gation was attained while no significant change of tensile properties
4. Conclusions was made by CGP due to superior grain growth at 573 K. Work
hardening, grain refinement and texture modification together
In this work, a high-efficiency experimental setup with heating decided the evolution of mechanical properties of the alloy sheets
systems was newly developed to conduct CGP on sheet metals with poor processed by CGP.
formability and low ductility at RT. The cracking behavior of AZ31 (5) The as-annealed sheet sample had a strong {0001} basal texture
magnesium alloy sheets during CGP and the effects of pass number and with a maximum intensity of 18.05 which was decreased to 10.61
processing temperature on the evolutions of their microstructure and when processed at 473 K after two passes. This may be related to
mechanical properties were studied in detail. The main conclusions are the appearance of {10−12} tensile twins introducing a rotation of
drawn as follows. about 86° for grains towards the TD of the sheet sample. However,
strong basal textures with maximum intensities comparable to the
(1) The number of effective pressings gradually increased with pro- initial one appeared again at higher processing temperatures.
cessing temperature. CGP of AZ31 magnesium alloy sheets could

458
Z. Wang et al. Materials Science & Engineering A 745 (2019) 450–459

Acknowledgment K. Higashi, The activity of non-basal slip systems and dynamic recovery at room
temperature in fine-grained AZ31B magnesium alloys, Acta Mater. 51 (2003)
2055–2065.
The authors would like to acknowledge the financial support pro- [16] M.R. Barnett, A taylor model based description of the proof stress of magnesium
vided by the National Natural Science Foundation of China (Grant no. AZ31 during hot working, Metall. Mater. Trans. A 34 (2003) 1799–1806.
51605266). [17] S.X. Ding, C.P. Chang, P.W. Kao, Effects of processing parameters on the grain re-
finement of magnesium alloy by equal-channel angular extrusion, Metall. Mater.
Trans. A 40 (2009) 415.
References [18] M.M. Myshlyaev, H.J. McQueen, A. Mwembela, E. Konopleva, Twinning, dynamic
recovery and recrystallization in hot worked Mg-Al-Zn alloy, Mater. Sci. Eng. A 337
(2002) 121–133.
[1] W.J. Joost, P.E. Krajewski, Towards magnesium alloys for high-volume automotive
[19] A. Galiyev, R. Kaibyshev, G. Gottstein, Correlation of plastic deformation and dy-
applications, Scr. Mater. 128 (2017) 107–112.
namic recrystallization in magnesium alloy ZK60, Acta Mater. 49 (2001)
[2] K.S. Fong, M.J. Tan, F.L. Ng, A. Danno, B.W. Chua, Microstructure stability of a fine-
1199–1207.
grained AZ31 magnesium alloy processed by constrained groove pressing during
[20] A.G. Beer, M.R. Barnett, Influence of initial microstructure on the hot working flow
isothermal annealing, ASME J. Manuf. Sci. Eng 139 (2017), p. 081007.
stress of Mg-3Al-1Zn, Mater. Sci. Eng. A 423 (2006) 292–299.
[3] K.S. Fong, A. Danno, M.J. Tan, B.W. Chua, Tensile flow behavior of AZ31 magne-
[21] T. Krajňák, P. Minárik, J. Stráská, J. Gubicza, K. Máthis, M. Janeček, Influence of
sium alloy processed by severe plastic deformation and post-annealing at moder-
equal channel angular pressing temperature on texture, microstructure and me-
ately high temperatures, J. Mater. Process. Technol. 246 (2017) 235–244.
chanical properties of extruded AX41 magnesium, J. Alloy. Compd. 705 (2017)
[4] M. Eftekhari, A. Fata, G. Faraji, M.M. Mashhadi, Hot tensile deformation behavior
273–282.
of Mg-Zn-Al magnesium alloy tubes processed by severe plastic deformation, J.
[22] R.B. Figueiredo, T.G. Langdon, Principles of grain refinement in magnesium alloys
Alloy. Compd. 742 (2018) 442–453.
processed by equal-channel angular pressing, J. Mater. Sci. 44 (2009) 4758–4762.
[5] K.S. Fong, D. Atsushi, T.M. Jen, B.W. Chua, Effect of deformation and temperature
[23] R.B. Figueiredo, T.G. Langdon, Grain refinement and mechanical behavior of a
paths in severe plastic deformation using groove pressing on microstructure, tex-
magnesium alloy processed by ECAP, J. Mater. Sci. 45 (2010) 4827–4836.
ture, and mechanical properties of AZ31-O, ASME J. Manuf. Sci. Eng. (2015)
[24] L. Gao, A.A. Luo, Hot deformation behavior of as-cast Mg-Zn-Mn-Ce alloy in com-
051004.
pression, Mater. Sci. Eng. A 560 (2013) 492–499.
[6] T. Han, G. Huang, Q. Deng, G. Wang, B. Jiang, A. Tang, Y. Zhu, F. Pan, Grain
[25] A. Shirdel, A. Khajeh, M.M. Moshksar, Experimental and finite element investiga-
refining and mechanical properties of AZ31 alloy processed by accumulated ex-
tion of semi-constrained groove pressing process, Mater. Des. 31 (2010) 946–950.
trusion bonding, J. Alloy. Compd. 745 (2018) 599–608.
[26] S. Morattab, K. Ranjbar, M. Reihanian, On the mechanical properties and micro-
[7] R.Z. Valiev, Y. Estrin, Z. Horita, T.G. Langdon, M.J. Zehetbauer, Y. Zhu, Producing
structure of commercially pure Al fabricated by semi-constrained groove pressing,
bulk ultrafine-grained materials by severe plastic deformation: ten years later, JOM-
Mater. Sci. Eng. A 528 (2011) 6912–6918.
US 68 (2016) 1216–1226.
[27] N. Li, G. Huang, R. Xin, Q. Liu, Effect of initial texture on dynamic recrystallization
[8] D.H. Shin, J. Park, Y. Kim, K. Park, Constrained groove pressing and its application
and deformation mechanisms in AZ31 Mg alloy extruded at 573K, Mater. Sci. Eng.
to grain refinement of aluminum, Mater. Sci. Eng. A 328 (2002) 98–103.
A 569 (2013) 18–26.
[9] A.K. Gupta, T.S. Maddukuri, S.K. Singh, Constrained groove pressing for sheet metal
[28] L. Zhang, Q. Wang, W. Liao, W. Guo, B. Ye, W. Li, H. Jiang, W. Ding, Effects of cyclic
processing, Prog. Mater. Sci. 84 (2016) 403–462.
extrusion and compression on the microstructure and mechanical properties of
[10] S.C. Yoon, A. Krishnaiah, U. Chakkingal, H.S. Kim, Severe plastic deformation and
AZ91D magnesium composites reinforced by SiC nanoparticles, Mater. Charact. 126
strain localization in groove pressing, Comp. Mater. Sci. 43 (2008) 641–645.
(2017) 17–27.
[11] Z. Wang, Y. Guan, G. Wang, C. Zhong, Influences of die structure on constrained
[29] R. Zheng, T. Bhattacharjee, A. Shibata, T. Sasaki, K. Hono, M. Joshi, N. Tsuji,
groove pressing of commercially pure Ni sheets, J. Mater. Process. Technol. 215
Simultaneously enhanced strength and ductility of Mg-Zn-Zr-Ca alloy with fully
(2015) 205–218.
recrystallized ultrafine grained structures, Scr. Mater. 131 (2017) 1–5.
[12] B.R. Sunil, A.A. Kumar, T.S. Sampath Kumar, U. Chakkingal, Role of biominer-
[30] A. Fata, G. Faraji, M.M. Mashhadi, V. Tavakkoli, Hot tensile deformation and
alization on the degradation of fine grained AZ31 magnesium alloy processed by
fracture behavior of ultrafine-grained AZ31 magnesium alloy processed by severe
groove pressing, Mater. Sci. Eng. C 33 (2013) 1607–1615.
plastic deformation, Mater. Sci. Eng. A 674 (2016) 9–17.
[13] K. Peng, L. Su, L.L. Shaw, K.W. Qian, Grain refinement and crack prevention in
[31] M. Zhan, C. Li, W. Zhang, An EBSD study on the microstructure and texture evo-
constrained groove pressing of two-phase Cu-Zn alloys, Scr. Mater. 56 (2007)
lution of AZ31 magnesium alloy during accumulative roll-bonding, Acta Metall. Sin.
987–990.
48 (2012) 709–716.
[14] S.S. Satheesh Kumar, T. Raghu, Mechanical behaviour and microstructural evolu-
[32] S.S. Satheesh Kumar, T. Raghu, Structural and mechanical behaviour of severe
tion of constrained groove pressed nickel sheets, J. Mater. Process. Technol. 213
plastically deformed high purity aluminium sheets processed by constrained groove
(2013) 214–220.
pressing technique, Mater. Des. 57 (2014) 114–120.
[15] J. Koike, T. Kobayashi, T. Mukai, H. Watanabe, M. Suzuki, K. Maruyama,

459