Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
453–460
INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE
AND HOT-PROCESSING MAPS OF Mg-1Ca-0.5Mn ALLOYS
VPLIV DODATKA Ce NA MIKROSTRUKTURO IN PROCESNE
MAPE VRO^EGA ZGO[^EVANJA ZLITIN Mg-1Ca-0,5Mn
Zhihui Cai
1,2
, Yongyong Jia
1
, Qinhong Fan
1,2
, Yaojie Hou
1
, Lifeng Ma
1*
1
School of Mechanical Engineering, Taiyuan University of Science and Technology, Taiyuan, China
2
Heavy Machinery Engineering Research Center of the Ministry of Education, Taiyuan University of Science and Technology, Taiyuan, China
Prejem rokopisa – received: 2022-04-28; sprejem za objavo – accepted for publication: 2022-07-07
doi:10.17222/mit.2022.489
To investigate the processability of Mg-1Ca-0.5Mn alloys with and without the addition of Ce, hot-compression tests were per-
formed on a Gleeble-3800 thermo-mechanical simulator at 300–450 °C and 0.001–5 s
–1
. The flow stress, processing map, and
microstructure characterization of the alloys were investigated. The results show that the flow stress of the Mg-1Ca-0.5Mn-
0.5Ce alloy was significantly improved for all the thermomechanical deformation parameters, and the dynamic recrystallization
phenomenon was delayed. This phenomenon was attributed to the finer grains and the dense distribution of the fine and coarse
particles pinned at the grain boundaries. The processing map shows that the Mg-1Ca-0.5Mn-0.5Ce alloy has better processing
performance at a low strain rate.
Keywords: Mg-Ca-Mn alloy, Ce addition, hot compression, processing map
Avtorji v ~lanku opisujejo raziskavo o procesiranju zlitine Mg-1Ca-0.5Mn brez in z dodatkom cerija (Ce). Izvajali so
primerjalne teste vro~ega tla~nega stiskanja na termomehanskem simulatorju Gleeble-3800 pri temperaturah med 300 °C in
450 °C ter hitrostih deformacije med 0.001 s
–1
i n5s
–1
. Dolo~ili so krivulje te~enja, izdelali procesni mapi in analizirali
mikrostrukturo obeh preiskovanih zlitin. Rezultati raziskave so pokazali, da se je napetost te~enja zlitine z dodatkom cerija
Mg-1Ca-0,5Mn-0,5Ce mo~no izbolj{ala (povi{ala) in prav tako vsi ostali termomehanski deformacijski parametri z zakasnitvijo
pojava dinami~ne rekristalizacije. Avtorji ~lanka ta pojav pripisujejo nastanku finej{ih (bolj drobnih) kristalnih zrn in gostej{i
porazdelitvi finih in grobih delcev pripetih na meje kristalnih zrn. Izdelana procesna mapa je pokazala, da ima zlitina
Mg-1Ca-0.5Mn-0,5Ce bolj{e procesne lastnosti pri ni`ji hitrosti deformacije.
Klju~ne besede: zlitina na osnovi Mg, Ca in Mn, dodatek Ce, vro~e zgo{~evanje, procesna mapa
1 INTRODUCTION
As the lightest engineering material, magnesium
(Mg) alloys have a series of excellent properties, such as
high specific strength, anti-fatigue, high damping, and
shock absorption, so it has a broad application prospect
in the fields of aerospace and automotive.
1,2
However,
Mg alloys have poor mechanical properties due to their
dense hexagonal structure, which severely limits their
widespread application.
3
Therefore, these alloys have at-
tracted plenty of researchers to explore ways to improve
the ductility of Mg alloys.
It is well known that alloying can improve the
strength and plasticity of materials. In recent years, many
researchers have investigated the effect of alloying of Ca
and Mn elements on the properties of Mg alloys.
4–6
For
example, Jiang et al.
7
found that the grain size and den-
sity of the precipitates in the extruded Mg-2Zn-xCa
(w/%) alloy increased with increasing Ca content, result-
ing in increased strength of the alloy. Similarly, by modi-
fying the Mn content, an ultra-high, as-extruded
Mg-5.5Al-3Ca-0.3Mn alloy with a yield strength (YS) of
402 MPa was successfully developed.
8
However, while
the strength of the alloys with Ca and Mn elements was
significantly increased (YS > 351 MPa), the ductility of
these alloys was much lower (< 10 %). In addition,
low-cost Ce rare-earth elements were reported to signifi-
cantly improve the properties of the alloy. Y. Du et al. re-
ported that the elongation of Mg-3Zn was enhanced from
24 % to 35 % after 0.05 w/% Ce addition.
9
Hence, it is
necessary to explore the effect of combined additions of
Ca, Mn, and Ce on the mechanical properties and micro-
structures in Mg-1Ca-0.5Mn alloys.
At present, most studies have focused on the influ-
ence of extruded alloys, but the rolled Mg-Ca-Mn alloy
has not been investigated. Therefore, it is necessary to
study the thermomechanical deformation behavior of the
alloy before rolling to obtain the best processing range to
guide the subsequent rolling experiments. To optimize
the thermomechanical deformation process parameters,
the process parameters such as temperatures, strains, and
strain rates with optimized microstructure and mechani-
cal properties are directly linked by the processing
map.
10,11
Scott C. Sutton et al.
12
studied the constitutive
behavior and processing maps of a new wrought Mg al-
loy ZE20 (Mg-2Zn-0.2Ce) and revealed that a safe re-
gion for processing occurs between 375 °C and 450 °C,
Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460 453
UDK 542.65:661.865.5 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(5)453(2022)
*Corresponding author's e-mail:
tsaizhihui@163.com (Z. H. Cai)

from 0.003 s
–1
to 0.1 s
–1
. In this work the influence of Ce
addition on the microstructure, hot-processing maps of
Mg-1Ca-0.5Mn alloys was investigated.
2 EXPERIMENTAL PART
The materials used in this study were cast Mg-1Ca-
0.5Mn and Mg-1Ca-0.5Mn-0.5Ce alloys. The composi-
tions are shown in Table 1. And the Mg-1Ca-0.5Mn al-
loy and Mg-1Ca-0.5Mn-0.5Ce alloys were encoded as
XM10 and XME100 samples, respectively. The as-re-
ceived alloy was homogenized at 420 °C for 12 h to pro-
mote microstructural uniformity. The sample size used
for the thermal compression experiment is a cylinder
with a length of 15 mm and a diameter of 10 mm. The
uniaxial isothermal compression test was carried out on
the Gleeble-3800 testing machine. The compressive de-
formation processes are shown in Figure 1. Hot-com-
pression conditions are as follows: deformation tempera-
ture in the range 300–450 °C, strain rate 0.001–5 s
–1
, and
the relative pressure reduction of the sample was 60 %.
The sample was heated to the deformation temperature at
a heating rate of 5 K/s, kept for 5 min, and then sub-
jected to compression, followed by quenching to retain
the hot-deformation structure.
Table 1: Chemical compositions of XM10 and XME100 alloy (w/%)
Alloy Mn Ca Ce Mg
XM10 Mg-1Ca-0.5Mn 0.49 1.12 – Bal.
XME100 Mg-1Ca-0.5Mn-0.5Ce 0.50 1.00 0.53 Bal.
The microstructure under different processing param-
eters was characterized by optical microscopy (OM,
PMG3, OLYMPUS, Tokyo, Japan) and scanning electron
microscopy (SEM, Zeiss, Sigma 500). The phase compo-
nent was confirmed by energy-dispersive spectrometry
(EDS, Zeiss, Sigma 500) with 15 kV and the working
distance of 12.5 mm. The metallographic specimens
were ground on 400, 800, and 1000 grit silicon carbide
paper, followed by grinding on waterproof abrasive pa-
per. Then the samples were etched for OM and SEM
with an acetic glycol solution (60 mL ethylene glycol,
10 mL acetic acid) containing saturated picric acid.
3 RESULTS AND DISCUSSION
3.1 Flow characteristics and deformation mechanisms
The experimental flow curves under different defor-
mation parameters are shown in Figure 2. The solid line
represents the XM10 alloy, and the dashed line repre-
sents the XME100 alloy. The deformation curves of the
two alloys exhibit typical thermomechanical deformation
behavior, with the values of the flow stress proportional
to the strain rate and inversely proportional to the tem-
perature. Moreover, the flow stress of the XME100 alloy
was significantly improved with the addition of Ce. For
example, the flow stress of the XME100 alloy at 1 s
–1
was comparable to that of XM10 alloy at 5 s
–1
. And obvi-
ous softening was observed in the XME100 alloy at
450 °C and 5 s
–1
. These phenomena can be attributed to
the addition of Ce, which could refine the grains as well
as promote the precipitation of the second phase and the
occurrence of dynamic recrystallization (DRX). In addi-
tion, it can be seen from Figure 2 that the curves can be
divided into three types according to the changing trend
of the curves:
The trend of the flow stress curve for both alloys ap-
proximates to a constant straight line, which can be re-
garded as ideal plastic flow at 400–450 °C and 0.01 s
–1
.
The temperature of 400–450 °C corresponds to 62–70 %
of the melting point of Mg (648 °C), which means that
the thermomechanical deformation of the alloy is less
hampered in this temperature range. When the strain rate
is low, the deformation of the alloy is unrestricted, result-
ing in a flat curve. And this phenomenon also appears at
350–450 °C and 0.001 s
–1
.
The flow stress at 350–450 °C and 1 s
–1
first rises to a
peak and then decreases slightly. This behavior is classi-
cally attributed to dynamic recovery (DRV), and the
stress increase with the increase of the strain. Moreover,
the slight decrease of the flow stress at high strain is at-
tributed to the occurrence of DRX. And the interaction
between DRX and DRV leads to the phenomenon in the
figure.
The flow stress rises to peak value, followed by sig-
nificant flow softening at 450 °C and 5 s
–1
. The curve
shows an obvious rising trend of hardening until they
reach peak stress, after which the trend of significant
softening down related to DRX is observed.
The true stress-strain curves of the XM10 and
XME100 alloys at different temperatures with 0.001 s
–1
strain rates are shown in Figure 3. It was found that the
peak value of the curves lagged after Ce was added into
the XM10 alloy at 0.001 s
–1
. By a simple inspection of
Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
454 Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460
Figure 1: Schematic diagram and specimen geometry of the hot-com-
pression test

Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460 455
Figure 3: True stress-strain curves for alloys: a) 300 °C, 0.001 s
–1
, b) 350 °C, 0.001 s
–1
, c) 400 °C, 0.001 s
–1
Figure 2: True stress-strain curves for alloys: a) 300 °C, b) 350 °C, c) 400 °C, d) 450 °C

Figure 3, the XM10 alloy reaches the peak stress at
strains of 0.31, 0.25, and 0.24, respectively. The
XME100 alloy reached peak stresses of 74.4 MPa,
33 MPa, and 19.6 MPa at strains of 0.34, 0.58, and 0.35,
respectively. This may be since the addition of Ce is not
conducive to the initiation of the slip system, reducing
the slip and block of dislocations, thereby preventing the
occurrence of DRX. This phenomenon will be further
explained in Section 3.3.
3.2 Processing maps and characterization
The processing map was a graph that characterizes
the inherent processing properties of the materials
through different strain rates, strain, and temperatures. It
was based on the DMM first developed by Wellstead and
improved by Prasad et al.
13–15
Modeling the deformation
process of the sample as linear power dissipation by the
principles of the DMM, and an instability criterion sub-
sequently superimposed. Thus, a stable processing zone
for the workpiece processing is obtained.
Figure 4 shows the 3D power-dissipation map under
different strains to explore the influence of different de-
formation parameters on the power-dissipation value. As
shown in Figures 4a to 4c the power-dissipation effi-
ciency increases from 0.34 to 0.38 with the increase of
strain from 0.15 to 0.25. Then, the efficiency of the
power dissipation decreases sharply from 0.38 to 0.14
with an increase in strain from 0.25 to 0.35. A higher value has better processing performance, which indicates
that the workability under 0.35 strain of the alloy be-
comes narrower. The sudden drop of the power dissipa-
tion value around 0.35 true strains at 350 °C and
0.001 s
–1
might be caused by defects within the material.
It can be seen from Figures 4d to 4f that the peak
power-dissipation efficiency of the XEM100 alloy and
the region of values greater than 0.35 increase with the
increase of strain. The higher power-dissipation coeffi-
cient in the XME100 alloy is distributed in the
low-strain-rate region and high temperature.
The value represents the ratio of the energy con-
sumed due to microstructural evolution to the total en-
ergy consumed linearly during the heat-deformation pro-
cess. Phenomena such as DRV or DRX were often found
in areas with high  values. It was generally accepted
that the alloy has better processability at the temperature
and strain rate of DRX. According to the stacking-fault
energy of the material, the DRX usually occurs between
30 % and 55 %.
16
The power-dissipation value of the al-
loy increases with the increase of the strain at a low
strain rate. The main reason is the density of the disloca-
tions in the grains increases with the increase of strain,
resulting in dislocation recombination, climbing, and
other behavior. Meanwhile, the accumulation of disloca-
tions is conducive to accelerating the occurrence of
DRX. Especially at low strain rate, there is enough time
for DRX and grain growth, thus more recrystallized
grains are produced, more deformation energy is con-
sumed, and a higher power-dissipation value is shown.
17
So, the alloy with Ce possesses better processing perfor-
mance, especially at low temperature and low strain
compared with XM10 alloy.
Figure 5 shows the processing maps of the XM10
and XEM100 alloys at different strains. The stable and
unstable regions are marked with rectangular frames and
symbols, respectively. It can be seen from Figures 5a to
5c that in XM10 alloy, under the strain of 0.15, region I
exist between 390 °C and 450 °C below 0.2 s
–1
. Region
II exists between 370 °C and 415 °C below 0.004 s
–1
.
When the strain reaches 0.25, a new stable region ap-
pears at low temperature and low strain rate. However,
this area is so tiny that it cannot be accurately used for
actual processing. When the strain reaches 0.3, in the
medium-temperature and low-strain region (temperature
380–415 °C, strain rate less than 0.0015 s
–1
), there is an
unstable region II, which is extremely detrimental to the
processing of the sample. In the XME100 alloy, it can be
seen from Figures 5d to 5f that when the strain is 0.15,
the image shows two stable regions, which are located at
the low- and medium-temperature strain rate (tempera-
ture 300–390 °C, strain rate less than 0.0025 s
–1
) and
high-temperature medium strain rate (temperature is
420–450 °C, and the strain rate is less than 0.082 s
–1
),
which are respectively represented as processable areas I
and II. As the strain increases to 0.25, a new stable re-
gion appears in the high-temperature and low-strain area,
which indicates that the alloy has good processing ability
under low strain, and this area is collectively referred to
as the stable region I, located at a temperature of
300–450 °C, the strain rate is less than 0.004 s
–1
. Stable
Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
456 Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460
Figure 4: Power-dissipation maps of alloys: a) XM10, strain 0.15, b)
XME100, strain 0.15 c) XM10, strain 0.25, d) XME100, strain 0.25, e)
XM10, strain 0.35), f) XME100, strain 0.35

region II is located at a temperature of 418–450 °C and a
strain rate of 0.003–0.1 s
–1
. When the strain is 0.35, the
processable area is expanded to a temperature of
400–450 °C, and the strain rate is 0.0035–0.5 s
–1
.
Therefore, the XME100 alloy with added Ce has
better machinability. It not only has high power-dissipa-
tion values and a stable workable region at low strain
rates, but also has a good workable interval at high tem-
peratures and high strain rates. Since the low strain rates
are not suitable for the actual industrial production, the
best optimal processing region selected is the stable re-
gion II, the temperature is 400–450 °C, and the strain
rate is 0.0035–0.5 s
–1
.
3.3 Effect of Ce element on microstructure
The peak value of the stress-strain curves indicates
the dynamic equilibrium of DRX and strain hardening of
the alloy. The hysteresis of the stress peak indicates the
enhancement of strain hardening or the weakening of the
DRX effect.
18
The strain-hardening capacity (HC) of a metallic ma-
terial is one of the important considerations in the analy-
sis of the strain-hardening effect.
19,20
Therefore, Equation
(1) for HC was as follows:
HC =
−
=−

   ucs
true
0.2
true
0.2
true
ucs
true
0.2
true
1 (1)
Where  0.2
true
is the true YS and  ucs
true
represents the
true ultimate compressive strength (UCS). The calcula-
tion results are shown in Table 2. The HC value of the
XME100 alloy is lower than that of the XM10 alloy, in-
dicating the weaker strain-hardening effect. To sum up,
the peak stress lagged of the alloy may be the result of
the weakening of both strain hardening and DRX, but it
has a more remarkable influence on the strain hardening.
Table 2: Strain-hardening capacity of XM10 and XME100 alloys
Alloy HC
XM10 0.82222
XME100 0.53752
Figure 6 shows the microstructures of the as-cast
XM10 alloy and XME100 alloys. The OM image of the
XM10 alloy showed a coarse microstructure, with a sub-
stantial presence of precipitate phase, and the XME100
alloy has a finer grain with the addition of Ce. It is gen-
erally accepted that the strength and plasticity of an alloy
increase with the decrease in grain size. The strength of
the alloy is enhanced due to the smaller grain size, which
leads to an increase of grain boundaries in the alloy. The
occurrence of dislocation slip needs to pass through the
grain boundary, thus the alloy with fine grains has a
higher strength. The mechanism of improving the plas-
ticity is as follows. The number of grains in a certain vol-
ume increases with the decrease of the grain size. Under
a certain plastic deformation, the average deformation in
each grain is less, which makes the probability of grain
cracking smaller, leading to the enhancement of the plas-
ticity. In addition, fine grains may explain the change in
the strain hardening of the alloy. U.F. Kocks et al.
21
re-
ported that the grain size significantly affects the
strain-hardening behavior and the grain refinement
weakens the effect of the strain hardening. Many schol-
Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460 457
Figure 5: Processing maps for alloys: a) XM10, strain 0.15, b) XM10, strain 0.25, c) XM10, strain 0.35, d) XME100, strain 0.15, e) XME100,
strain 0.25, f) XME100, strain 0.35

ars have also reported that grain refinement can weaken
the ability of work hardening.
22,23
This phenomenon may
be attributed to the reduction of the maximum disloca-
tion density in the grains due to grain refinement, which
leads to the reduction of the work-hardening capacity.
As we can see in Figures 6c and 6d,m a n ys e c -
ond-phase particles appear on the grain boundaries of the
two alloys. The difference is that the fine precipitates are
mainly distributed in the XM10 alloy, while some coarse
second-phase particles appear in the XME100 alloy. Ac-
Q. FAN et al.: INFLUENCE OF Ce ADDITION ON THE MICROSTRUCTURE AND HOT-PROCESSING MAPS ...
458 Materiali in tehnologije / Materials and technology 56 (2022) 5, 453–460
Figure 7: Microstructure at 350 °C and 0.001 s
–1
at true strain of 0.25: a) XM10 alloy, b) XME100 alloy
Figure 6: Microstructures of as-cast alloys: a) XM10, OM, b) XME100, OM, c) XM10, SEM, d) XME100, SEM

cording to the study
24
and the EDS analysis, the finely
distributed precipitates in the XM10 alloy and the coarse
second-phase particles in the XME100 alloy are Mg
2
Ca
particles, which indicates that with the addition of Ce,
the precipitation of Ca is promoted, resulting in the
growth of the Mg
2
Ca particles.
Figure 7 shows the microstructures of the deformed
XM10 and XME100 alloys. It can be seen from Figures
7a and 7b that the grains in the XM10 alloy were trans-
formed into uniform equiaxial grains when the true strain
is 0.25, which means that the alloy underwent DRX un-
der this strain. Nevertheless, the volume fraction of DRX
grains in the XME100 alloy is less than that of the XM10
alloy. And many elongated grains were found in the
XEM100 alloy, which means that the alloy is incom-
pletely DRX. The great number of coarse grains present
in the XEM100 alloy may be able to accommodate more
strain during the deformation, resulting in better machin-
ability. As the SEM pictures of Figures 7a and 7b show,
the fine second-phase particles distributed at the grain
boundaries in the XM10 alloy after deformation disap-
pear. In contrast, many fine and coarse second phases
distributed on grain boundaries can still be observed in
the XME100 alloy. Thus, Ce prevents the dissolution of
elements during the deformation and reduces the solubil-
ity of Ca in the alloy.
The pinning effect of the homogenous fine particle is
beneficial to maintaining its deformed grains under high
strains. The occurrence of DRX will be hindered if the
drive energy of the deformation is equal to that of the
pinning energy. It is seen from Figure 7b that the pin-
ning of precipitates not only hinders the rearrangement
of dislocations, but also hinders the movements of the
sub-grain boundaries, inhibiting the nucleation of contin-
uous DRX.
25
J. D. Robson et al.
26
found that DRX grains
were rarely observed around the coarse particle. The
DRX grains would appear occasionally around the large
coarse-grain clusters of an individual deformed micro-
structure, but the effect of these grains on the total DRX
can be ignored. Therefore, the PSN of DRX is retarded
by the combined action of densely distributed fine parti-
cles and coarse particles, leading to the phenomenon of
peak receding.
4 CONCLUSIONS
1. The alloy curve shows typical thermomechanical
deformation behavior. The XME100 alloy has higher
flow stress and a peak lagged effect at 0.001 s
–1
strain
rate. The peak lagged effect was due to the addition of
Ce, promoting the precipitation of the second phase,
which pins on the grain boundary and offsets a part of
the deformation driving force, resulting in the weakening
of the dynamic recrystallization ability.
2. The hot-processing parameter of the XME100 al-
loy exerts a great influence on the power-dissipation effi-
ciency. The higher power-dissipation region is mainly at
a deformation temperature between 320 °C and 360 °C
and the strain rate below 0.004 s
–1
. The lower power dis-
sipation region is mainly when the temperature is be-
tween 300 °C and 360 °C above 0.018 s
–1
.
3. There are two processing regions in the XME100
alloy: stable region I is at 300–450 °C and strain rate is
less than 0.004 s
–1
; stable region II is at 400–450 °C and
strain rate is 0.0035–0.5 s
–1
. To adapt to the actual indus-
trial production, the optimal processing region is the sta-
ble region II, the temperature is 400–450 °C, the strain
rate is 0.0035–0.5 s
–1
.
Acknowledgments
The authors acknowledge support from National Nat-
ural Science Foundation of China (U1910213), Taiyuan
University of Science and Technology Scientific Re-
search Initial Funding (Grant No. 20202039)
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