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Journal of Magnesium and Alloys 9 (2021) 1297–1303

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Full Length Article

Effect of extrusion speed on microstructure and mechanical properties of
the Mg-Ca binary alloy
Jingren Li a, Aiyue Zhang a, Hucheng Pan a,∗, Yuping Ren b, Zhuoran Zeng c, Qiuyan Huang d,
Changlin Yang e, Lifeng Ma f, Gaowu Qin b,∗
a Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University,
Shenyang 110819, China
b State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang, 110819, China
c Department of Materials Science and Engineering, Monash University, Vic. 3800, Australia
d Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
e State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi’an, Shaanxi 710072, China
f Shanxi Provincial Key Laboratory of Metallurgical Equipment Design and Technology, Taiyuan University of Science and Technology, Taiyuan 030024,

China
Received 12 January 2020; received in revised form 11 March 2020; accepted 18 May 2020
Available online 25 June 2020

Abstract
This work reported the effect of extrusion speeds on the microstructures and mechanical properties of Mg-Ca binary alloy. The results
showed that yield strength of the as-extruded Mg-1.2 wt.% Ca alloys decrease from ∼ 360 MPa to ∼ 258 MPa as the ram speed increases
from 0.4 mm/s to 2.4 mm/s, and the elongation increases from ∼ 3.9% to ∼ 12.2%. The microstructure changes from bimodal grain feature
to the complete dynamical recrystallization (DRX) with increase of the extrusion speed. The ultrafine DRXed grains in size of ∼0.85 μm,
the numerous nano-Mg2 Ca particles dispersing along the grain boundaries and interiors, as well as the high density of residual dislocations,
should account for the high strength. It is believed that the high degree of dynamic recrystallization and the resulting texture randomization
play the critical roles in the ductility enhancement of the high-speed extruded Mg alloys.
© 2020 Chongqing University. Publishing services provided by Elsevier B.V. on behalf of KeAi Communications Co. Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
Peer review under responsibility of Chongqing University

Keywords: Extrusion speed; Microstructure; Mechanical properties; Mg-Ca alloy.

1. Introduction
As the lightest metallic alloy, Mg alloys have drawn
great interests in the past decades, especially in the fields
of automotive and aerospace industries [1-5]. However, the
widespread applications of Mg alloys are restricted by their
poor workability, which is caused by the few independent slip
systems at room temperature [6,7]. Alloying and the severe
plastic deformation (SPD) process are effective methods to in-
crease the mechanical properties [8-19]. Rare earth elements
∗
Corresponding authors.
E-mail addresses: panhc@atm.neu.edu.cn (H. Pan),
qingw@smm.neu.edu.cn (G. Qin).
https://doi.org/10.1016/j.jma.2020.05.011
2213-9567/© 2020 Chongqing University. Publishing services provided by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/) Peer review under responsibility of Chongqing University
(including Y, Sc, Nd, Er, Ce, Sm and Gd) have been reported
to improve both ductility and absolute strength of Mg alloys
[20-22]. Zhang et al. [23] found that the elongation to fail-
ure (EL) of ZK60–4Sm (wt.%) alloy is increased by 100%
compared with that of ZK60 alloy, reaching ∼ 28.1%.
Recently, it is becoming a new trend to develop of the
low-cost Mg alloys for wider industrial applications. For ex-
ample, Kang et al. [16] reported a low-alloyed Mg-1.38Zn-
0.17Y-0.12Ca (at.%) alloy, which was extruded at 190 °C
with ram speed of 0.1 mm/ s − 1 , showing the ultimate ten-
sile strength (UTS) of ∼ 357 MPa, tensile yield strength (YS)
of ∼ 317 MPa and EL of ∼ 6.4%. Zhou et al. [24] reported
that with only 3% yttrium added, a high EL of ∼33% was
obtained in Mg-Y alloy. In view of the similarity to the RE
1298 J. Li, A. Zhang and H. Pan et al. / Journal of Magnesium and Alloys 9 (2021) 1297–1303

Fig. 1. (a) The tensile engineering stress–strain curves of the as-extruded Mg–Ca alloys. (b, c, d) The OM image of the as-extruded X12–0 alloy, X12–1
alloy, X12–2 alloy, respectively. The extruded direction and the radial direction are denoted as ED and RD, respectively.

elements, the cheap price and low density, Mg-Ca alloys have Table 1
received extensive attentions [25-28]. For example, Pan et al. Mechanical properties of as-extruded Mg-Ca binary alloys.
[18] reported a Mg-Ca alloy which exhibits high YS of ∼ Samples Ram speed Yield strength Ultimate Elongation
377 MPa and UTS of ∼ 392 MPa. As the extrusion tempera- (mm/s) (MPa) strength (MPa) (%)
ture increases from 230 °C to 250 °C, the EL has enhanced X12–0 0.41 ∼ 360 ∼ 370 ∼ 3.9
by six times (13.2%). Chai et al. [29] also reported that the X12–1 1.09 ∼ 319 ∼ 326 ∼ 8.3
UTS of Mg-1.0Sn-0.5 Zn alloy increases from ∼ 261 MPa to X12–2 2.4 ∼ 258 ∼ 266 ∼ 12.2
∼ 300 MPa as the Ca added from 0 to 2 wt.%. However, there
are few researches on effect of extrusion speed on microstruc-
microstructures of the alloys were characterized via optical
ture and mechanical properties of the binary Mg-Ca alloys,
microscopy (OM), electron backscattered diffraction (EBSD,
which will be the focus of present study.
MAIA3 model 2016) and transmission electron microscopy
(TEM, JEOL-2100F, operated at 200 kV). The volume frac-
2. Materials and methods tion of un-DRXed region was measured by image J software
for the OM images and channel 5 for EBSD images.
Mg–1.2 wt.% Ca was prepared by melting pure Mg
(99.99 wt.%) and pure Ca (99.90 wt.%) in the electronic re- 3. Results and discussion
sistance furnace, under the protection of mixture gas of CO2
and SF6 (100:1). Then the as-cast ingots were homogenized Fig. 1 shows the tensile engineering stress-strain curves
at 500 °C for 24 h. The billets were indirectly extruded at of present Mg-Ca alloys, which were extruded at different
350 °C with extrusion ratio of 20 and ram speed of 0.4 mm/s, ram speeds. The mechanical properties are summarized in
1.0 mm/s, 2.4 mm/s (named X12–0, X12–1 and X12–2, re- Table 1. As compared with the X12–1 and X12–2 alloys, the
spectively). The mechanical properties of the as-extruded bars low-speed extruded X12–0 alloy exhibits higher engineering
were measured at a strain rate of 10−3 s − 1 on universal Ma- stress, with YS of ∼ 360 MPa, UTS of ∼ 370 MPa and the
terial Testing Machine (Shimazu AG-X Plus) at room temper- EL of ∼ 3.9%. With the increasing of ram speed, the UTS de-
ature, with the dog bone specimens in gage length of 25 mm creases from ∼ 370 MPa to ∼ 266 MPa and the EL increases
and the diameter of 5 mm. The tensile yield strength, ulti- from ∼ 3.9% to ∼ 12.2%. The YS, UTS and EL of X12–
mate tensile strength and elongation to fracture are the aver- 1 alloy are measured to be ∼ 326 MPa, ∼ 319 MPa and ∼
age values of at least three individually repeated tests. The 8.3%, respectively. Fig. 1b-d display the OM images of the as-
 J. Li, A. Zhang and H. Pan et al. / Journal of Magnesium and Alloys 9 (2021) 1297–1303 1299

Fig. 2. (a) The band contrast (BC) map of X12–0 alloy, (b) the BC and grain boundaries(GB) map, the black line indicates the high angle grain boundaries
(HAGB) and the red line represents the low angle grain boundaries (LAGB), (c) the inverse pole figure (IPF) of X12–0 alloy. (d, e, f) The BC, BC+GB and
IPF images of X12–1 alloy. (g) The pole figure (PF) of X12–0 alloy and (h) the PF image of X12–1 alloy. (For interpretation of the references to colour in
this figure legend, the reader is referred to the web version of this article.)

extruded X12–0, X12–1, X12–2 alloys. The un-recrystallized
regions can be found in the OM images of X12–0 and X12–1
alloys (as marked by the red arrows in Fig. 1b, c) and the
volume fraction of unDRXed regions are estimated to be ∼
64.5% and ∼ 12.1%, respectively. With the increase of ram
speed, the complete recrystallization microstructure can be
obtained in the X12–2 alloy, and the average grain size has
grown to be ∼ 2.95 μm.
The microstructures of the alloys extruded at ram speed
of 0.41 mm/s and 1.09 mm/s were investigated, and the re-
sults are presented in Fig. 2. For the X12–0 alloy, it can be
seen the un-recrystallized regions are separated by a number
of low angle grain boundaries (LAGB, as indicated by the
red lines in Fig. 2b, c). The number fraction of un-DRXed
region is calculated to be ∼ 19.6%, which indicates the low
degree of DRX. The un-DRXed grains usually exhibit a typ-
ical fiber texture [30], with <10−10>//ED, which is exactly
the case in present Mg-Ca alloys. Consequently, a strong tex-
ture with a ∼ 11.51 multiple random distribution (mrd.) is
obtained in the X12–0 alloy, due to the low degree of DRX
(Fig. 2g). By the way, according to the band contrast image in
Fig. 2a, the average grain size is estimated to be ∼0.85 μm.
As compared with the X12–0 alloy, the X12–1 alloy displays
higher degree of DRX, as shown in Fig. 2D-f. The almost
completely DRXed microstructure can be found in X12–1 al-
loy (Fig. 2e), and a much weaker texture of ∼5.17 mrd., than
that in X12–0 alloy can be detected due to the high degree of
recrystallization, as illustrated by the pole figure in Fig. 2h.
The deviation of recrystallization volume fraction between the
OM and EBSD results was ascribe to the EBSD image area
is too small. In this sense, the DRXed grains have also ap-
parently grown due to the DRX and the average grain size
can be estimated to be ∼1.58 μm (Fig. 2d).
Figs. 3 and 4 show the typical bright-field TEM images of
as-extruded X12–0 alloy. The DRXed grains with the average
grain size of 300 ∼ 500 nm are observed (Fig. 3a), and pro-
fuse dislocation accumulate in front of the bulk Mg2 Ca phase
(Fig. 3b), which is exactly the same case reported in Ref.
[31,32]. It suggests that the DRXed grains prefer to nucleate
at the second-phase boundaries via the well-known particle
simulation nucleation (PSN) mechanism and the particles can
also retard the grain growth to some extent [33]. By the way,
the nano-phases are also seen to densely distribute in the Mg
matrix in Fig. 3c, and d is the higher-magnification image.
The number density of the nano-particles is high, and the av-
erage size is estimated to be ∼25 nm. Besides, the second
phases can be determined to be Mg2 Ca, according to phase
diagram of the Mg-Ca binary system [34].
Particularly, a high volume fraction of un-DRXed grains
exists in the as-extruded X12–0 alloy, and the detailed sub-
grain and dislocation structures are shown in Fig. 4. It can
be seen that the dislocations are invisible in Fig. 4a, under
the two beam condition of g = 10–10, while the dislocations
can be detected in Fig. 4c, d, in the condition of g = 0001.
According to the g•b = 0 invisible criterion [35], the disloca-
tion lines distributed in the α-Mg matrix (Fig. 4c), belong to
the non-basal types and come from the dissociation of per-
fect c + a dislocations [36]. These partial dislocations lying
1300 J. Li, A. Zhang and H. Pan et al. / Journal of Magnesium and Alloys 9 (2021) 1297–1303

Fig. 3. (a-c) The TEM images of as-extruded X12–0 alloy, and (d) the high magnification of the area marked by the red rectangle in Fig. 3c. (For interpretation
of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 4. (a-d) TEM images of the as-extruded X12–0 alloy, and (d) the high magnification of the area marked by red rectangle in Fig. 4c, under the two-beam
condition of (a) g = 10–10, (c, d) g = 0001. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)

on the basal planes have recently been confirmed by both
experiments and simulations [37,38]. Besides, the sub-grains
are detected to exist in grain interiors of unDRXed regions,
as marked by the green lines in Fig. 4c, and the Fig. 4d is
the high magnification of the rectangle in Fig. 4c. These low
angle grain boundaries should have been formed during DRX
processing and further separate the Mg matrix into lamel-
lae (Fig. 4d). In fact, the present authors have reported the
similar sub-grain lamellae in Mg-2Sn-2Ca alloys [39]. More
interesting, plenty of nano-particles, as marked by the blue
circles in Fig. 4d, are found to distribute along the residual
<c + a>dislocations, which are believed to hinder movement
of the newly activated dislocations and can effectively en-
hance the strength.
With increasing of the extrusion speed, the as-extruded
X12–1 alloy shows a much higher degree of recrystallization,
as compared with the X12–0 alloy, and the corresponding
TEM images are shown in Fig. 5. The grain size of X12–
 J. Li, A. Zhang and H. Pan et al. / Journal of Magnesium and Alloys 9 (2021) 1297–1303
Fig. 5. (a-d) The typical TEM images of the as-extruded X12–1 alloy, and the Fig. 5d is viewed under the two-beam condition of g = 0001.
1 alloy is determined to be ∼1.43 μm, and the average size
of nano-spherical phase is estimated to be ∼75 nm, which
has increased by three times. The nano-phases disperse along
both the grain boundaries and grains interiors, as shown by
the blue circles in Fig. 5c. By the way, the number density
of residual dislocations has dramatically decreased due to the
high degree of DRX (Fig. 5d).
In present Mg-Ca binary alloy, the grain size is obviously
refined after extrusion processing, and both the Ca atoms dis-
solved in Mg matrix and the bulk Mg2 Ca phases should play
the important roles. Firstly, a great number of c + a disloca-
tions should have been activated in Mg-Ca matrix, and con-
siderable amount of residual dislocations can still be found
in as-extruded samples (Fig. 4d). The decreasing of stacking
fault energy of Mg matrix due to the Ca addition is consid-
ered as the main reason [40]. Secondly, the coarse Mg2 Ca
phases can also induce a high density of dislocations around
the interphase between Mg2 Ca and Mg matrix, which would
provide potential nucleation positions for DRX. Readily, the
rearrangement of high density dislocations leads to the forma-
tion of LAGBs (Fig. 2b and Fig. 4d). More importantly, Pan
et al. [18] found the segregations of Ca atoms at the LAGBs,
and such segregation would not only decrease the boundary
energies but also strongly hinder the migration of LAGB via
pining effect, which thereby lead to the obvious grain refine-
ment. Besides, the dispersive nano-particles distributing along
dislocations can also impede the migration of LAGBs and
lead to the formation of fine grains. With increasing of ex-
trusion speed, the grain size becomes larger and excess heat
generated during high-speed extrusion should be the one rea-
son. Nevertheless, the average grain size is still low, around
∼ 1.5 μm in the case of X12–1 alloy, which demonstrates the
high thermal stability in present Ca-containing Mg alloys.
1301
Moreover, it is reported that grain refinement [41,42] and
precipitations [43,44] should account for the improvement
of mechanical properties in Mg alloys. Consequently, in the
present Mg-Ca alloys, the existence of ultrafine grain size,
the sub-grain lamellae, and the dispersive nano-particles can
effectively hinder movement of the newly activated disloca-
tions and enhance the absolute strength. Besides, the ductility
also increases from ∼ 3.9% to ∼ 8.3% as the ram speed im-
prove from 0.4 to 1.0 mm/s. It is seen that the X12–1 alloy
undergoes a higher degree of DRX and exhibits more uni-
form grains than those in X12–0 alloy. The high degree of
DRX leads to the low intensity of fiber texture, as displayed in
Fig. 2h. Texture randomization is important for enhancing the
ductility of Mg alloys, since more grains are suitable for ac-
tivations of both basal and non-basal slips and the von Mises
criterion would be more readily satisfied [13]. Besides, the
fine recrystallized grains distribute homogeneously within the
matrix of X12–1 alloy. Consequently, the lattice strain can
be more uniformly accommodated in the X12–1 alloy, and
the internal stress concentration can be largely decreased, as
compared with X12–0 alloy, which is also beneficial for the
ductility.
Conclusion
This work focuses on the effect of extrusion speed on mi-
crostructure and mechanical properties of the Mg-Ca binary
alloys, and the following conclusions can be drawn.
(1) As ram speed increases from 0.4 to 2.4 mm/s, the UTS
of alloys decreases from ∼ 370 MPa to ∼ 266 MPa and
the elongation increases from ∼ 3.9% to ∼ 12.2%;
1302 J. Li, A. Zhang and H. Pan et al. / Journal of Magnesium and Alloys 9 (2021) 1297–1303
(2) The ultrafine grain size, the sub-grain lamellae, and the
dispersive nano-particles can effectively enhance the ab-
solute strength of the low-speed extruded samples;
(3) The strength decreases and ductility enhancement in the
high-speed extruded samples can be attributed to the
higher degree of DRX, more uniform grain structure
and the weaker texture, as compared with low-speed
extruded alloy.
Acknowledgment
This work is supported by National Natural Science Foun-
dation of China (Nos. 51525101, U1610253, 51701211, and
51971053), and funded by the Project of Promoting Talents in
Liaoning province (No. XLYC1808038). H.C. Pan acknowl-
edges the financial assistance from the State Key Laboratory
of Solidification Processing in NPU (No. SKLSP201920),
the Fundamental Research Funds for the Central Univer-
sities (No. N2002011) and joint R&D fund of Liaoning-
Shenyang National Research Center for Materials Science
(No. 2019JH3/30100040).
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