Z. WU et al.: EFFECT OF INITIAL TEMPERATURE ON THE MICROSTRUCTURE AND PROPERTIES OF ...
571–577
EFFECT OF INITIAL TEMPERATURE ON THE
MICROSTRUCTURE AND PROPERTIES OF CRYOGENIC ROLLED
AZ31 MAGNESIUM ALLOY
VPLIV ZA^ETNE TEMPERATURE NA MIKROSTRUKTURO IN
LASTNOSTI KRIOGENSKO VALJANE MAGNEZIJEVE ZLITINE
VRSTE AZ31
Zhenyu Wu
1
, Chenchen Zhi
1,2*
, Lifeng Ma
1,2
, Zebang Zheng
3
, Yanchun Zhu
1,2
,
Weitao Jia
1,2
1
College 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
3
State Key Laboratory of Solidification Processing, Shaanxi Key Laboratory of High-Performance Precision Forming Technology and Equip-
ment, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi’an, China
Prejem rokopisa – received: 2022-03-08; sprejem za objavo – accepted for publication: 2022-09-05
doi:10.17222/mit.2022.443
By characterizing the properties of a twin cast-rolled AZ31 sheet after cryogenic rolling, the effects of the initial temperature on
the microstructure and mechanical properties of the sheet obtained by cryogenic rolling were studied. The results indicate that
the hardness of the alloy was a maximum due to the high-density dislocations in the microstructure when the initial temperature
was room temperature. The highest yield strength and elongation appeared at the initial temperature of 200 °C, and the
microstructure was mainly fine equiaxed grains. It was observed that fine grains increased, and the yield strength and elongation
gradually decreased with the increase of the initial temperature. The overall trend of yield strength and elongation increased first
and then decreased. Based on the results of different initial temperature treatments, the optimal microstructure and properties of
AZ31 magnesium alloy were acquired when the initial temperature was 200 °C.
Keywords : cast-rolled AZ31 sheet; cryogenic rolling; microstructure; EBSD
Avtorji ~lanka so preu~ili lastnosti plo~evine iz magnezijeve zlitine vrste AZ3, ki je bila izvaljana neposredno iz taline na duo
valjarni{kem ogrodju. Dolo~ili so vpliv za~etne temperature na mikrostrukturo in mehanske lastnosti izbrane zlitine po njenem
nadaljnjem izotermalnem in kriogenskem valjanju. Rezultati {tudije so pokazali, da ima zlitina maksimalno trdoto zaradi
nastanka visoke gostote dislokacij v mikrostrukturi, ko je za~etna temperatura plo~evine enaka sobni temperaturi (20 °C).
Najvi{jo natezno trdnost in najve~ji raztezek pa ima zlitina, ko je za~etna temperatura 200 °C. in so v mikrostrukturi v glavnem
fina enakoosna kristalna zrna. Ugotovili so, da se z rastjo finih zrn in nara{~ajo~o za~etno temperaturo postopoma zni`ujeta
meja plasti~nosti in raztezek. V splo{nem pa se trend meje te~enja in raztezka spreminja. Sprva nara{~a, nato pada. Na osnovi
preizkusov pri razli~nih za~etnih temperaturah ugotavljajo, da ima magnezijeva zlitina vrste AZ31 optimalno mikrostrukturo in
najbolj{e mehanske lastnosti pri izbrani za~etni temperaturi 200 °C.
Klju~ne besede: magnezijeva zlitina vrste AZ31, kriogensko valjanje, mikrostruktura, EBSD
1 INTRODUCTION
Material strength and plasticity are difficult to im-
prove at the same time: an improvement of one property
is often accompanied by the other property weakening.
1–3
Many techniques, such as severe plastic deformation
(SPD)
4
and advanced thermo-mechanical processes, have
been used to obtain alloys with high strength and good
ductility at the same time, but cryogenic rolling has been
identified as a promising path to produce ultra-fine-grain
structures with small strain and continuous products.
5,6
Cryogenic rolling technology is a kind of rolling
technology in which the rolled piece is cooled to liq-
uid-nitrogen temperature for plastic deformation of the
material.
7
At present, cryogenic rolling technology has
been successfully applied in the deformation processing
of aluminum alloy,
8,9
copper alloy,
10,11
and steel,
12
and
has a significant effect on improving the strength and
toughness of the material. Das et al. obtained an ul-
tra-fine-grain structure of Al 7075 alloy after cryogenic
rolling at liquid nitrogen temperature, and the yield
strength and impact toughness of the material after grain
refinement were increased by 108 % and 60 %, respec-
tively.
13
The mechanical property improvement caused
by cryogenic rolling is also suitable for LM6 aluminum
alloy.
14
After comparing AA6061 aluminum alloy sam-
ples at room and low temperatures, it proved that asym-
metric rolling at low temperature could improve the uni-
form elongation and reduce the texture strength.
15
Shi et
al. analyzed the microstructure and mechanical proper-
ties of 5052 aluminum alloy rolled at room and low tem-
peratures. They found that the cryogenic rolling process
can significantly enhance dislocation and boundary
strength to improve the tensile strength and yield
Materiali in tehnologije / Materials and technology 56 (2022) 5, 571–577 571
UDK 669.721.5:536.483 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(5)571(2022)
*Corresponding author's e-mail:
zhicc0629@163.com (Chenchen Zhi)

strength of the 5052 alloy effectively. High-density dislo-
cation of cryogenic rolling could further accelerate the
speed of dynamic recrystallisation and grain refinement
of the alloy.
16
Regarding the application of cryogenic
rolling in copper alloy, Yue et al. carried out large plastic
deformation on a Cu-Ag alloy at the temperature of liq-
uid nitrogen to explore its texture evolution and
recrystallisation behavior.
17
The results showed that the
dynamic recovery was inhibited during the cryogenic
rolling process, which led to the accumulation of high
deformation energy storage in the alloy. Because of the
low lamination fault energy of copper alloy, cryogenic
rolling is more conducive to the generation of ultra-fine
grains and twin crystals, and can simultaneously improve
the strength and plasticity of the alloy.
18–21
Due to the significant improvement of the micro-
structure and properties of materials brought by the cryo-
genic rolling process, many researchers began to apply
this process to magnesium alloys. Preciado et al. found
that through the cryogenic treatment of AZ91 magne-
sium alloy, the grain size was obviously refined, and the
elongation of the material was significantly improved.
22
By carrying out cryogenic multi-pass rolling deformation
on the ZK60 magnesium alloy sheet, the alloy underwent
dynamic recrystallization (DRX), the grain size was sig-
nificantly refined, and the microstructure uniformity was
improved considerably.
23
Discontinuous dynamic
recrystallization and twin dynamic recrystallization were
the main mechanisms of microstructure evolution for the
Mg-14Li-1Al (La141) alloy processed by large deforma-
tion cryogenic rolling. Through these two plastic defor-
mation mechanisms, more submicron dynamic
recrystallized grains were produced, which significantly
improved the mechanical properties of the alloy.
24
Cryo-
genic rolling has been extensively used in enhancing the
properties of magnesium alloys, while the influencing
factors for the cryogenic rolling of magnesium alloys
have not formed a complete processing system, which
cannot have enough impact on production and life.
In this paper, the AZ31 magnesium alloy intermedi-
ates underwent cryogenic rolling and characterization af-
ter treatment. The influence of the initial temperature on
the microstructure and properties of the magnesium alloy
was studied. Compared with the microstructure and
properties of magnesium alloy materials at different
initial temperatures, the optimal initial temperature pa-
rameters to improve the strength and toughness of AZ31
magnesium alloy were obtained.
2 EXPERIMENTAL PART
The experimental work was carried out on twin
cast-rolled AZ31 magnesium alloy sheets. The thickness
of the plates changed from the original 7 mm to 6.8 mm
after grinding and cleaning, and sample sizes were cut
into dimensions of (60 × 45 × 6.8) mm for the subse-
quent rolling. After heating in preservation at 400 °C for
2 h, the samples were isothermally rolled by a dou-
ble-roll mill with a roller diameter of 380 mm, and the
temperature of the rollers was controlled at (70 ± 5) °C.
The plates were rolled from 6.8 mm to 1.9 mm after five
passes.
The intermediate plates were air-cooled to room tem-
perature or placed in a furnace for supplementary tem-
perature for 15 min to a different initial temperature re-
quired by the experiment. To find the optimal initial
temperature of cryogenic rolling, four initial tempera-
tures were designed as room temperature, (200, 250, and
300) °C respectively (marked as AR, A200, A250, and
A300 respectively below). Cryogenic rolling was carried
out by dipping the samples in liquid nitrogen for 1 min-
ute and rolling for three passes. After each pass, samples
were immersed into the liquid-nitrogen tank for cooling.
These samples were rolled from 1.9-mm-thick to
1.6-mm-thick after cryogenic rolling. Figure 1 is the
schematic of the cryogenic equipment. The flow chart of
this experiment is shown in Figure 2.
3 RESULTS AND DISCUSSION
3.1 Influence of initial temperature on microstructure
Figure 3 gives the inverse pole figure (IPF) maps of
samples that were held at different initial temperatures.
When the initial temperature is room temperature, the
microstructure of AR is shown in Figure 3a. Most grains
are elongated parallel to the rolling direction and a small
Z. WU et al.: EFFECT OF INITIAL TEMPERATURE ON THE MICROSTRUCTURE AND PROPERTIES OF ...
572 Materiali in tehnologije / Materials and technology 56 (2022) 5, 571–577
Figure 2: Flow chart of the process Figure 1: Schematic diagram of liquid nitrogen cooling equipment

number of equiaxed submicron grains exist. Fine grains
formed because many dislocations accumulated in the in-
termediate plate after three passes of the isothermal roll-
ing process. The dislocations do not recrystallize or re-
cover at room temperature, so a large number of
dislocations are intertwined during the rolling deforma-
tion. In addition, the intermediate plates enter the cryo-
genic treatment in liquid nitrogen after low-temperature
rolling, and the plastic deformation at low temperature
promotes the formation and retention of high-density
dislocations, as shown in Figure 4, inhibiting the dy-
namic recovery effectively.
25
The formation of high-den-
sity dislocations will increase the energy near the grain
boundary, which not only leads to the formation of new
grains
26
but also reduces the average grain size of the al-
loy.
27
Therefore, fine grains formed near the grain bound-
ary in the AR, and the average grain size is much lower
than A250 and A300. A similar conclusion obtains after
the cryogenic rolling of industrial pure zirconium
plates.
28
When the initial temperature of the intermediate plate
was set at 200 °C, the sample’s microstructure shows in
Figure 3b. The fine grains almost disappeared, the
microstructure showed fine equiaxed grains, and the av-
erage grain size was 4.59 μm. The reason is that the in-
termediate plate accumulates many dislocations after un-
Z. WU et al.: EFFECT OF INITIAL TEMPERATURE ON THE MICROSTRUCTURE AND PROPERTIES OF ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 571–577 573
Figure 3: IPF maps of samples at different initial temperatures: a) AR, b) A200, c) A250, d) A300
Figure 4: KAM maps of samples at different initial temperatures: a) AR, b) A200, c) A250, d) A300

dergoing multiple isothermal rolling processes. When the
initial temperature was 200 °C, recrystallization and re-
covery occurred, which promoted grain refinement,
shortened the displacement range and the dislocation ac-
cumulation, and reduced the stress concentration near the
grain boundary.
29
Therefore, compared with AR, the
KAM of A200 is significantly reduced, and the geomet-
rically necessary dislocation is reduced, suggesting the
recovery was activated at this initial temperature.
30
Due
to atomic diffusion, dislocations are suppressed, and the
microstructure remains recrystallized in subsequent
cryogenic rolling. Some grains are elongated along the
rolling direction to coordinate the deformation during
dynamic recovery.
16
The microstructures of A200 and A300 are still dom-
inated by equiaxed grains, but the grains elongate along
the rolling direction, and the average grain size is
10.97 μm and 14.63 μm, respectively (Figure 3c and
3d). Studies have shown that the increase in annealing
temperature significantly reduces the nucleation and
growth time of recrystallization.
31
Therefore, the increase
of the initial temperature makes the grains of A250 and
A300 grow.
3.2 Influence of initial temperature on tensile proper-
ties
A universal material-testing machine was used to
conduct the tensile tests on the samples obtained from
different rolling process parameters at room temperature,
and the true stress-true strain curves were obtained as
shown in Figure 5.
As can be seen from the figure, the alloy has high
strength and poor plasticity at the initial temperature of
room temperature. This is because a large number of dis-
locations are accumulated during the isothermal rolling,
as shown in Figure 4. When the initial temperature is
room temperature, the necessary conditions for recrys-
tallization and recovery cannot be satisfied. The decrease
in temperature inhibited the dynamic recovery of the al-
loys, which increased the dislocation density and the de-
gree of work hardening;
32
dislocations accumulate more
and intertwine with each other after several passes.
Panigrahi et al. studied the precipitation hardening pro-
cess of an Al-Mg-Si alloy during cryogenic rolling and
found that low-temperature conditions are conducive to
the formation and retention of high-density disloca-
tions.
33
Therefore, after cryogenic treatment in liquid ni-
trogen, the alloy retains this microstructure state and
causes more dislocations because of the internal lattice
of the material.
The specific data and the variation trend of the me-
chanical properties measured by tensile tests at room
temperature are shown in Figure 6. The tensile strength
of the AZ31 magnesium alloy decreases gradually with
the increase of the initial temperature, from 311 MPa to
283 MPa at room temperature. The yield strength and
elongation of the alloy have a similar trend, increasing
first with an increase of the initial temperature and then
gradually decreasing. Compared with AR, A200 and
A250 show a typical trade-off relationship, the growth of
initial temperature leading to the plastic enhancement
and a slight decrease in strength.
With the increase of the initial temperature, the sam-
ple microstructures transferred from deformed grains to
fine and uniform equiaxed grains. When the initial tem-
perature changes from room temperature to 200 °C, the
elongation increases from 8.5 % to 14 %, i.e., by 64.7 %.
When the plastic deformation of the materials with tiny
and uniform grains occurs, each grain shares a certain
amount of deformation so that the distribution of defor-
mation is more uniform. The amount of dislocation
packing and the stress concentration at the grain is re-
markably excluded, the material has less tendency to
crack, and the plasticity of the alloy is improved. Ac-
cording to the Hall-Petch formula shown in Equation (1),
the strength was inversely proportional to the square root
of its grain size,
34
but the dislocations remain in the cryo-
Z. WU et al.: EFFECT OF INITIAL TEMPERATURE ON THE MICROSTRUCTURE AND PROPERTIES OF ...
574 Materiali in tehnologije / Materials and technology 56 (2022) 5, 571–577
Figure 6: Tensile properties of samples at different initial tempera-
tures
Figure 5: True stress-true strain curves of samples at different initial
temperatures: a) AR, b) A200, c) A250, d) A300

genic treatment process; thus, the ultimate tensile
strength (UTS) is slightly reduced.

y
kd =+
−
0
12 /
(1)
Figure 7 shows the basal textures of the cryogenic
rolled samples. The initial temperature of the intermedi-
ate plate is different, but the development tendency of the
basal textures is similar. The base poles were named
from ND to RD, and the base plane remained parallel to
RD. When the initial temperature is 200 °C, the texture
strength is 8.87 mrd (multiple random distributed). The
texture strength increases with the initial temperature in-
crease to 11.39 mrd and 12.07 mrd, respectively. The
prominent {0001} basal texture reduces the ductility of
the AZ31 alloy.
35
The stable texture generated at 250 °C
and 300 °C reduced the ductility of the AZ31 alloy. In
conclusion, the alloy elongation at 200 °C obtained
better mechanical properties.
3.3 Influence of initial temperature on the hardness
The hardness of the AZ31 magnesium alloy varies
with the initial temperature, as shown in Figure 8. When
the initial temperature is room temperature, the hardness
of the alloy is up to 69 HV. This phenomenon can be at-
tributed to the accumulated deformation of cast-rolled
AZ31 magnesium alloy during isothermal rolling. Dur-
ing cryogenic rolling, recrystallization is not activated,
and cold hardening and grain slip occur. A lot of disloca-
tion entanglement (as shown in Figure 4) and a mass of
residual stress are generated inside the alloy. However,
with the increase of the initial temperature, the hardness
value of the alloy decreases significantly. When the ini-
tial temperature is 200 °C, the alloy hardness is 57.5 HV,
which is 19.6 % lower than at room temperature. On the
one hand, the change of internal stress has a substantial
effect on the overall hardness of the sheets; the initial
temperature increase releases the internal stress of the
plate. On the other hand, the KAM value of the alloy de-
creases significantly (as shown in Figure 4), which
means that the geometrically necessary dislocation den-
sity decreases, and the plate actively restores in the pro-
cess of plastic deformation,
36
so the sheet’s hardness de-
creases.
The hardness values of the alloy at 250 °C and
300 °C are 58.2 HV and 57.7 HV, respectively. When the
initial temperature increases, the hardness value of the
alloy does not change remarkably, and the value fluctu-
ates within 1 HV. This is because only the grain size of
the magnesium alloy is changed when the alloy is held in
preservation for a short time, and no structural change
has taken place. Therefore, the average grain size grows
with the increase of the initial temperature, but the effect
on the hardness of the alloy is not distinct at the macro
level.
4 CONCLUSIONS
The initial temperature has a significant effect on the
microstructure and mechanical properties of the AZ31
magnesium alloy. When the initial temperature is room
temperature, fine submicron grains appear at the grain
boundaries due to the high-density dislocation accumula-
tion caused by multi-pass isothermal rolling and cryo-
genic treatment. When the initial temperature increases,
the fine equiaxed grains are the primary structures, and
with the increase in temperature, the grains begin to
grow and elongate along the rolling direction. Therefore,
an appropriate initial temperature of 200 °C can provide
a good matrix structure for the subsequent deformation
treatment of the material.
The tensile strength of AZ31 magnesium alloy de-
creases with the initial temperature increase, but the de-
crease is not evident. The yield strength and elongation
first increased and then weakened with the enhancement
of the initial temperature. When the initial temperature
was 200 °C, the yield strength and elongation reached a
maximum. The comprehensive mechanical properties of
AZ31 magnesium alloy are the best when the initial tem-
perature is 200 °C after cryogenic rolling.
Z. WU et al.: EFFECT OF INITIAL TEMPERATURE ON THE MICROSTRUCTURE AND PROPERTIES OF ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 571–577 575
Figure 8: Hardness value of samples at different initial temperatures
Figure 7: {0001} pole figures of samples at different initial tempera-
tures: a) AR, b) A200, c) A250, d) A300

When the initial temperature is room temperature, the
hardness of the AZ31 magnesium alloy is very high and
exceeds 60 HV. When the initial temperature increases,
the hardness value of the alloy decreases significantly.
However, when the temperature continues to rise, the
change of grain size has little effect on the macroscopic
effect of the alloy, so the hardness range of the alloy is
not distinct, not more than 1 HV. Therefore, the initial
temperature of 200 °C is the most suitable for the cryo-
genic rolling of the AZ31 magnesium alloy.
Acknowledgment
This work was supported by the National Natural
Science Foundation of China (U1910213), Taiyuan Uni-
versity of Science and Technology Scientific Research
Initial Funding (TYUSTSRIF) (20212007), and Award
Grants for Outstanding Doctor Working in Shanxi
(20212072).
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