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Procedia
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Procedia Manufacturing 50 (2020) 822–830

18th International
18th International Conference
Conference Metal
Metal Forming
Forming 2020
2020 Project
Project
18th International
18th InternationalConference
ConferenceMetal Forming
Metal 20202020
Forming Project

Effect
Effect of
of variable
variable temperature
temperature repetitive
repetitive upsetting-extrusion
upsetting-extrusion on
on
microstructure and texture of Mg-Gd-Y-Zr alloy
microstructure and texture of Mg-Gd-Y-Zr alloy
Yingze
Yingze Mengaaaa,, Jianmin Yub,*
b,*, Huisheng Yub b, Yaojin Wuaa, Zhimin Zhangb
Yingze Meng
Meng , Jianmin
Jianmin Yu b,*,, Huisheng
Huisheng Yu
Yubb,, Yaojin
Yaojin Wu
Wuaa,, Zhimin
Zhimin Zhang
b
Yub,* Zhangbb
College of
a
College
a of Mechanical
Mechanical and
and Electrical
Electrical Engineering,
Engineering, North
North University
University of
of China,
China, No.
No. 3
3 Xueyuan
Xueyuan Road
Road Jiancao
Jiancao District,
District, Taiyuan
Taiyuan 030051,
030051, China
China
College
aa b
Collegeof Mechanical
of of Materials and Electrical
Science and Engineering, North University of China, No. 3
3 Xueyuan Road Jiancao District, Taiyuan 030051, China
College
College
b Mechanical
of Materials and
Science and Engineering,
Electrical
Engineering, North
Engineering,
North University
North
University of
University China,
of of
China, No.
China,
No. 3
3 Xueyuan
No. Road
Xueyuan
Xueyuan Jiancao
Road
Road District,
Jiancao
Jiancao Taiyuan
District,
District, 030051,
Taiyuan
Taiyuan China
030051,
030051, China
China
College of
bb
College of Materials
Materials Science
Science and
and Engineering,
Engineering, North
North University
University of
of China,
China, No.
No. 3
3 Xueyuan
Xueyuan Road
Road Jiancao
Jiancao District,
District, Taiyuan
Taiyuan 030051,
030051, China
China
* Corresponding author. E-mail address: yujianmin@nuc.edu.cn
* Corresponding author. E-mail address: yujianmin@nuc.edu.cn
*
* Corresponding author. E-mail
Corresponding author. E-mail address:
address: yujianmin@nuc.edu.cn
yujianmin@nuc.edu.cn

Abstract
Abstract
Abstract
Abstract
The Mg-Gd-Y-Zr
The Mg-Gd-Y-Zr alloy alloy was
was subjected
subjected to to the
the variable
variable temperature
temperature repetitive
repetitive upsetting-extrusion
upsetting-extrusion process,
process, aa kind
kind ofof severe
severe plastic
plastic deformation.
deformation.
The Mg-Gd-Y-Zr
Mg-Gd-Y-Zr alloy
alloy was
was subjected
subjected to the variable
variable temperature repetitive upsetting-extrusion process,
process, aaIt kind of
of severe plastic deformation.
The
The evolution
evolution of
of microstructure,
microstructure, texturetoand
texture thedeformation
and deformationtemperature
mechanism
mechanism repetitive
under upsetting-extrusion
under different
different passes
passes was
was analysed.
analysed. It kind
is
is found
found severe
that plastic
that when
when thedeformation.
the deformation
deformation
The evolution
The evolution
temperature of relatively
of microstructure,
microstructure, texture
texture and
and deformation
deformation mechanism
mechanism under
under different
different passesequiaxed.
passes was analysed.
was analysed. Itprecipitated
It is found
is found that
thatphases
when were
when the deformation
the deformation
temperature was relatively high at 420℃, the morphology of the grains was approximately equiaxed. Some precipitated phases were distributed
was high at 420℃, the morphology of the grains was approximately Some distributed
temperature
temperature
at the grain was
was relatively
relatively
boundaries and high
high
the at
at 420℃,
420℃,
fraction ofthe
the morphology
morphology
them was of
of the
the
relatively grains
grains
low. Whenwas
was approximately
approximately
the deformation equiaxed.
equiaxed.
temperatureSome
Some
was precipitated
precipitated
decreased, phases
phases
the were
were distributed
distributed
precipitation phases
at the grain boundaries and the fraction of them was relatively low. When the deformation temperature was decreased, the precipitation phases
at
at the grain
the
increasedgrainremarkably,
boundariesplaying
boundaries and the
and the the
fraction
fraction of them
of them was
was relatively
relatively low.
low. When the
When the deformation
deformation temperature
temperature was
was decreased,
decreased, the
the precipitation
precipitation phases
phases
increased remarkably, playing the pinning effect and stimulate the particle stimulated nucleation (PSN) mechanism to significantly refine
pinning effect and stimulate the particle stimulated nucleation (PSN) mechanism to significantly refine the
the
increased
increased
grain. As remarkably,
remarkably,
As the
the number of playing
ofplaying the
deformation pinning
the pinning effect
passeseffect and
increased, stimulate
and stimulate
The grains
grainsthe particle
thewere
particle
were stimulated
stimulated
remarkably nucleation
nucleation
refined (PSN)
(PSN)
from the
the 80.45mechanism
mechanism
μm of to significantly
to significantly
of initial
initial billet to refine
4.08refine
to 4.08 ofthe
μm of the
4-
grain. number deformation passes increased, The remarkably refined from 80.45 μm billet μm 4-
grain. As
grain.sample,the number
As the gaining
numberthe of deformation
of deformation passes increased, The grains were remarkably refined from the 80.45 μm of initial billet to 4.08 μm
μm of 4-
of
pass
pass sample, gaining the more uniformpasses
more uniform increased, With
microstructure.
microstructure. The grains
With the were remarkably
the increase
increase of
of deformationrefined
deformation fromthe
amount,
amount, thecoarse
the 80.45 grains
coarse μm of decreased
grains initial billet
decreased to the
with
with 4.08fraction
the fraction 4-
of
of
pass
pass sample,
sample, gaining the
gaining the more
more uniform
uniform microstructure. Withrecrystallization
the increase
increase ofof deformation
deformation amount, the coarse
coarse grains decreased with
with theThe
fraction of
dynamic
dynamic recrystallization
recrystallization increased
increased andmicrostructure.
and secondary
secondary dynamicWith
dynamic the
recrystallization occurred amount,
occurred inside
inside the the
the grown
grown dynamic
dynamicgrains decreased
recrystallized
recrystallized the
grains.
grains. fraction
The of
(1010)
(1010)
dynamic
dynamic recrystallization
recrystallization
fiber texture
texture disappeared and increased
increased
and and
the texture
texture secondary
and secondary dynamic
dynamic
was weakened.
weakened. Therecrystallization
recrystallization
random of of the occurred
theoccurred inside
high-temperature the grown dynamic
inside thedeformation
grown dynamic
deformation recrystallized
recrystallized
texture was obvious
obviousgrains.
grains. The
due The (1010)
(1010)
to the
the non-
fiber disappeared the was The random high-temperature texture was due to non-
fiber
fiber texture disappeared and the
the texture was
was weakened.
weakened. The
The random
random of of the
the high-temperature
high-temperature deformation
deformation texture
texture waswas obvious
obvious duedue to
to the
the non-
basal texture
basal slip
slip of disappeared
of alloy
alloy which
which was and easier
was easiertexture
to
to activate.
activate. non-
basal slip
basal slip of
of alloy
alloy which
which waswas easier
easier toto activate.
activate.
©
© 2020
2020 The
The Authors.
Authors. Published
Published by
by Elsevier
Elsevier B.V.
B.V.
© 2020
©
© 2020
2020
This is
The
The
The Authors.
Authors.
Authors. Published
Published
Published by by Elsevier
by Elsevier
Elsevier B.V. B.V. license
B.V.
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the 18th International Conference Metal
Peer-review under responsibility of the scientific committee of the 18th International Conference Metal Forming
Forming 2020
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Peer-review under responsibility of the scientific committee of the 18th18th
Peer-review
Peer-review under
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Keywords:
Keywords: microstructure;
microstructure; texture;
texture; Mg-Gd-Y-Zr
Mg-Gd-Y-Zr alloy;
alloy; repetitive
repetitive upsetting-extrusion
upsetting-extrusion
Keywords:
Keywords: microstructure;
microstructure; texture;
texture; Mg-Gd-Y-Zr
Mg-Gd-Y-Zr alloy;
alloy; repetitive
repetitive upsetting-extrusion
upsetting-extrusion

1.
1. Introduction improve their performance [6-8]. The Mg-10Gd-3Y-0.6Zr
1. Introduction
1. Introduction
Introduction
improve
improve
improve
(wt.%)
their
their
their
alloy
performance
performance
performance
subjected to aging
[6-8].
[6-8].
[6-8].
The
The
The
treatment
Mg-10Gd-3Y-0.6Zr
Mg-10Gd-3Y-0.6Zr
Mg-10Gd-3Y-0.6Zr
and extruded reached
(wt.%)
(wt.%) alloy
alloy subjected
subjected to
to aging
aging treatment
treatment and
and extruded
extruded reached
reached
High strength
High strength andand high
high elongation
elongation magnesium
magnesium alloys alloys have
have (wt.%) alloy
the ultimate
the subjected
ultimate tensile to
tensile strength aging
strength (UTS)treatment
(UTS) of of 462and
462 MPa extruded
MPa and the
and reached
the yield
yield
High
High strength
attracted strength
much and
and high
attention elongation
high[1].
elongation
However, magnesium
magnesium
the magnesiumalloys have
alloys alloy
have the
the ultimate
ultimate
strength (YS)tensile
tensile
of strength
strength
383 MPa (UTS)
(UTS)
[9]. of
of
The 462
462 MPa
MPa
main and
and the
the yield
yield
strengthening
attracted
attracted much
much attention
attention [1].
[1]. However,
However, the
the magnesium
magnesium alloy
alloy strength
strength (YS)
(YS) of
of 383
383 MPa
MPa [9].
[9]. The
The main
main strengthening
strengthening
attracted
has
has poor
poor much
flow
flow attention
strength [1].
and However,
formability the
at magnesium
room alloy
temperature strength
mechanism (YS) ofof 383 MPa
Mg-Gd-Y-Zr [9]. The
alloy main
are strengthening
precipitation
has
has poor
[2,3].poor flow strength
flow
Therefore, strength
strength
and
and formability
and formability
formability
the optimization
optimization of the
at
at room
at room temperature
room
the microstructure
microstructuretemperature
temperature
is very
very
mechanism
mechanism
mechanism
strengthening of
of
of Mg-Gd-Y-Zr
Mg-Gd-Y-Zr
and Mg-Gd-Y-Zr
solid solution
alloy
alloy are
alloy
solution hardening.
hardening. are The
are
precipitation
precipitation
precipitation
uniformly
[2,3].
[2,3]. Therefore,
Therefore, the
the optimization of
of the microstructure is
is strengthening and solid The uniformly
[2,3]. Therefore,
important
important to
to the
improve
improveoptimization
the
the of the
formability
formability microstructure
and
and is very
comprehensive
comprehensive very strengthening
strengthening
dispersed
dispersed β′
β′
and
and
phases
phases
solid
solid
are
are
solution
solution
usually
usually the
the
hardening.
hardening.
main
main
The
The
strengthening
strengthening
uniformly
uniformly
phase
phase
important
important
mechanical to
to improve
improve
properties ofthe
the formability
formability
magnesium and
and
alloys. It comprehensive
comprehensive
is reported that dispersed
dispersed
[10,11]. β′
β′ phases
phases are
are usually
usually the
the main
main strengthening
strengthening phase
phase
mechanical
mechanical properties
properties of
of magnesium
magnesium alloys.
alloys. It is
is reported
It canreported that
that [10,11].
[10,11].
mechanical
magnesium
magnesium properties
alloys
alloys with
with of magnesium
ultra-fine
ultra-fine alloys.
grains
grains (UFG)
(UFG) It is
canreported
be
be that
prepared
prepared [10,11].
The
The repetitive upsetting-extrusion is a kind of SPD
magnesium
magnesium
by severe alloys
alloys
severe plastic with
with ultra-fine
ultra-fine
plastic deformation grains
grains
deformation technology (UFG)
(UFG)
technology (SPD), can
can be
be
(SPD), which prepared
prepared
which has has The repetitive
The repetitive
repetitive
technology.
upsetting-extrusion
upsetting-extrusion
upsetting-extrusion
Alloy after
after
is
is aaa kind
is kind of
kind
repetitive upsetting-extrusion
upsetting-extrusion of
SPD
ofusually
SPD
SPD
by
by severe plastic technology. Alloy repetitive usually
by severe
better
better plastic deformation
mechanical
mechanical deformation
properties
properties
technology
technology
than
than
(SPD),
(SPD), which
coarse-grained
coarse-grained which has
has
alloys
alloys
technology.
technology.
has
has weakening
weakening
Alloy
Alloy after
after
texture repetitive
repetitive
[12].
texture [12]. In
In
upsetting-extrusion
upsetting-extrusion
addition,
addition, the the usually
usually
repetitive
repetitive
better
better
prepared mechanical
mechanical
by properties
properties
traditional processing than
than coarse-grained
coarse-grained
techniques [4]. It hasalloys
alloys
been has
has weakening
weakening texture
upsetting-extrusion texture
process [12].
[12].
at In
In addition,
addition,
different the
the repetitive
temperatures repetitive
has an
prepared
prepared by
bythetraditional
traditional processing
processing techniques
techniques [4].
[4].beIt has
has been
It improved
been upsetting-extrusion
upsetting-extrusion process at
processphase different
at different
different temperatures
temperatures has
has an
an
prepared
proved that
proved by
that traditional
the ductilityprocessing
ductility of magnesium
of magnesium techniques
alloys can
alloys [4].
can beIt has been
improved upsetting-extrusion
impact on
impact on the process
the precipitation
precipitation at
phase thetemperatures
and the
and microstructure
microstructure has an
[13].
[13].
proved
proved
through that
that the
the ductility
ductility
microstructure of
of magnesium
magnesium
control and grainalloys
alloys can
can
refinement be
be improved
improved
[5]. impact
impact
However,on
on the
the
thereprecipitation
precipitation
are few phase
phase
reports and
and
on the
the
the microstructure
microstructure
variable [13].
[13].
temperature
through
through microstructure control and grain refinement [5]. However, there are few reports on the variable temperature
through microstructure
microstructure control
control and
and grain
grain refinement
refinement [5]. [5]. However,
However,
repetitive
repetitive
there
there are
are fewfew reports
upsetting-extrusion,
upsetting-extrusion, reports
and
and
on
on the
the variable
further
further variable
analysis
analysis
temperature
temperature
is
is needed.
At
At the
the same
same time,
time, it
it has
has been
been proposed
proposed that
that the
the addition
addition of
of repetitive
repetitive
In this upsetting-extrusion,
upsetting-extrusion,
this paper,
paper, the
the Mg-Gd-Y-Zr and
and
Mg-Gd-Y-Zr alloy further
further
alloy is analysis
subjectedis
analysis
is subjected istoneeded.
needed.
needed.
variable
rareAt
At the
the
earth same
same
(RE) time,
time, it
it
elements has
has
in been
been proposed
proposed
magnesium that
that
alloys canthe
the addition
addition
significantly of
of In to variable
rare earth (RE) elements in magnesium alloys can significantly In
In this
this paper,
paper, the
the Mg-Gd-Y-Zr
Mg-Gd-Y-Zr alloy alloy is
is subjected
subjected to to variable
variable
rare earth
rare earth (RE)
(RE) elements
elements inin magnesium
magnesium alloys
alloys can
can significantly
significantly
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 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830 823
2 Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000

temperature repetitive upsetting-extrusion deformation. By
analyzing the significantly refined matrix grains, the
dynamically precipitated phases and the gradually weakened
texture of the alloy, we discussed the deformation mechanism
of the alloy during the deformation.
more than 200 grains. EBSD data processing was performed
using TSL OIM 7.3 software. In this paper, Dynamic
recrystallized grains (DRXed) grains were defined as grains
with GOS <2.

2. Experimental procedure

The alloy used in this study was Mg-8.27 Gd-3.18 Y-0.43

Zr (wt%) alloy. The initial material used in the experiment was
a cylinder with a diameter of 330 mm, which was prepared by
extrusion deformation at the strain of 4.57. A 50 mm diameter
cylinder was taken from the center of the material as the initial
material for the experiment. The principle of repetitive
upsetting-extrusion is shown in Fig. 1.
The sample was upset to the diameter of 70 mm in the
mould, and then was further extruded to a diameter of 50 mm.
The end of one pass is completed when the specimen is
extruded. After turning the sample 180 °, repeat the above
process steps to the required processing passes. The cumulative
strain of one pass can be calculated as 1.346 by the formula ɂ ൌ
Ͷ ൈ Ž ݀Ȁ‫ܦ‬.
Fig. 1. Schematic diagram of repetitive upsetting-extrusion.
Fig. 2. Schematic diagram of the experimental process.
3. Results
3.1. Microstructure and texture of the initial alloy
Fig. 3 shows the microstructure of the initial alloy. It can be
observed in Fig. 3a that most areas of the alloy after hot
extrusion showed relatively uniform microstructures
constituted mostly equiaxed grains, with an average grain size
of 42.99 μm. Dynamic precipitation occurred in some areas, as
shown by the blue dashed box in Fig. 3. Due to its pinning
effect, grain growth was effectively suppressed, and the grains
in these areas were relatively fine. In Fig. 3 (a), some coarse
grains can also be observed, with many lines inside. By further
magnified image observation (Fig. 3b), the lines in the coarse
grains extended in almost the same direction in the local area,
the adjacent distances ranged from 1 μm to 4 μm. You et al.
[14] confirmed by TEM that these lines were composed of
dislocations arranged in parallel, and some β ' phases were
precipitated in part of the dislocation arrays.

This experiment used the variable temperature repetitive

upsetting-extrusion process. The experiment temperature was
different in different passes, which was repeated at high and
low temperatures. The specific experimental steps are shown in
Fig. 2. Before the experiment, the mould and the material were
heated to the required temperature at the same time and held
for 2 hours to ensure that the temperature of the mould and the
material is uniform during the experiment. The RUE
experiment was performed on a 4-THP61-630 forging press at
the punch speed of 4 mm / min. In order to reduce friction,
graphite-based lubricants were used for lubrication. The
Fig. 3. (a) OM and (b) BSE images of initial alloys and corresponding (c) XRD
experiment was performed 4 passes in total, and air cooling was
and (d) EDS results.
performed to room temperature at the end of each pass. The
sample was observed from the longitudinal section of the Further observation of the precipitated phase, it can be
sample by the wire cutter, and the observation surface was observed from the BSE image (Fig. 3c) that the precipitated
parallel to the extrusion direction (ED) (Fig. 1). phases exhibited the brighter contrast than the magnesium
The specimen was further observed under the Zeiss Axio matrix, concentrated in some areas. The precipitated phases
Imager A2m optical microscope for microstructure. X-ray were arranged in parallel short bars or staggered in small
diffraction (XRD) analysis was performed, 2θ from 20° to 90 blocks, with the length of about 1-3 μm (Fig. 3c). According to
°. EBSD samples were prepared by ion thinning at 6.8kv, the XRD results, it can be concluded that the initial material
35min, followed by electron backscatter diffraction analysis mainly contains α-Mg and Mg5(Gd,Y) phases (Fig. 3d). From
(EBSD) using Hitachi SU5000 scanning electron microscope the energy dispersive X-ray spectroscopy (EDS) results, it can
(SEM) equipped with EDAX-TSL. The selected area scanned
824 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830
Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000
be determined that the precipitation phase waas the Mg5
(Gd,Y) phase. You et al. have confirmed the β’ phase (Fig. 3e)
[14].
Fig. 4 showed the EBSD results of the initial alloy, and the
OIM (Fig. 4a) showed the similar distribution to the OM. The
(0001) pole figure (Fig. 4b) showed a weaker extrusion texture.
Most of the basal planes tended to be parallel to the ED. The
texture components tended to be uniformly distributed, and the
texture strength was 6.107. The inverse pole figure showed a
strong [1010] fiber texture, most of which [1010] // ED, with
the intensity of 2.170.
Fig. 4. (a) OIM map, (b) (0001) pole figures and (c) inverse pole figures of
initial alloy.
3.2. Microstructure evolution
Fig.5 shows the evolution of the microstructure as the RUE
processes increased from 1 pass to 4 passes at different
temperatures. Obviously, the accumulation of strain due to
severe plastic deformation leaded to continuous refinement of
grains in the matrix. When the number of deformation passes
was small, the grain size was not uniform, forming a bimodal
structure with large deformed grains and small dynamic
recrystallized grains. With the accumulation of the strain, the
microstructure with sufficient fineness was uniformly
distributed over the entire sample in 4 passes, as shown in Fig.
4 (d).
It has been reported that dislocation density, dislocation
migration, and formation of sub-grain structures are all affected
by temperature [13]. It was worth noting that when the
deformation temperature was higher at 420 ° C, the grains were
more equiaxed and there was no obvious elongation. In the 1
pass, corrugated dislocation lines (arrows in Fig. 5a) can be
observed within the grains, which may be the initial stage of
strain accumulation and sub-grain refinement at high
temperatures. Clear dislocation lines were also found in some
grains after 3 passes (arrows in Fig. 5c). These dislocation lines
were more densely distributed and crossed, showing a clear
comparison of dislocation walls and tangles in the grains.
It was believed that significant dynamic recrystallization
occurred at high-energy grain boundaries of coarse grains, and
dislocations could accumulate during the previous deformation
process [14]. In contrast, when the deformation temperature
was reduced, the grains with dense corrugated dislocation lines
inside were significantly reduced, while the precipitated phases
at the grain boundaries were significantly increased.
At 2 passes, the grains were elongated in the direction of
about 45° (Fig. 5f), which was related to the process of
upsetting and subsequent extrusion in the repetitive upsetting-
extrusion [12].At the same time, the precipitated phases at the
grain boundaries played an effective pinning effect, effectively
suppressing the grain growth in the subsequent air cooling
process, maintaining the grain's elongated microstructure
3
during the deformation process.
Due to the continuous increase of the strain in the 4 passes,
the coarse grains were completely refined to form a relatively
uniform microstructure, and the precipitated phases were
uniformly distributed at the grain boundaries. The grain
directionality was not obvious (Fig. 5h).
Fig. 5. OM images of repetitive upsetting-extrusion in different passes: (a,e) 1
pass; (b,f) 2passes; (c,g) 3 passes; (d,h) 4 passes.
Fig. 6 shows the corresponding BSE images of the samples
from different passes. When the deformation temperature was
high, there were few precipitated phases, accounting for about
2% of the number fraction. The number of precipitated phases
in 3 passes was slightly higher than that in 1 pass, which may
be caused by deformation. As the deformation temperature
decreased, the number of precipitated phases increased
significantly. The area number of fractions of the precipitated
phase in 2 passes and 4 passes increased to 0.079 and 0.114,
respectively. In 4 passes, the volume of the precipitated phase
was larger and the distribution was more uniform, indicating
that low temperature deformation was more conducive to
dynamic precipitation.
Fig. 6. BSE images of RUEed alloy after different passes with varying
temperature: (a,e) 1 pass; (b,f) 2passes; (c,g) 3 passes; (d,h) 4 passes.
During the RUE process, most of the precipitated phases
were ellipsoidal (yellow arrows), and there were a few square
phases (blue arrows). XRD and EDS experiments were
performed on the material and precipitated phases of each pass,
as shown in Fig. 7. EDS results were similar for different
passes. According to the results, it can be seen that the
precipitated phases were Mg5 (Gd,Y), and the shape of the
phase was changed from the initial phase but the composition
was unchanged, indicating its great thermal stability. The
fraction of square phases was too small to show in the XRD
results. The XRD pattern of the RUEed sample (Fig. 7a)
confirmed the change in the number of precipitated phases, as
new Mg5(Gd,Y) peaks could be observed in low temperature
deformation compared to high temperature deformed alloys
(dashed box in the Fig.7 a). The increase in the number of
phases allowed some weaker peaks to be identified. Similarly,
due to the RUE processes, which increased the dislocation
 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830 825
4 Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000

density, some small peak shifts could be seen in the XRD shows the distribution of grain boundaries in the sample after
pattern [15]. 1-4 passes at different temperatures. The yellow, red, and blue
lines represent three groups of grain boundaries, respectively,
and their misorientation angles are 2°-5°, 5°-15°, and lager than
15°. Grain boundaries with an angle of less than 2° were not
counted as measurement errors. The number fractions of grain
boundaries with different angles are listed in Table 1. The
KAM maps and orientation difference angle distribution maps
corresponding to different passes are also shown in Fig. 10.

Fig. 7. (a) X-ray diffraction patterns of RUEed alloy after different passes (b)
SEM image of 4 passes RUEed alloy and corresponding EDS results of the
point A (c), point B (d)indicated in the (b).

The EBSD analysis was performed on the material. The

OIM diagrams of different passes are shown in Fig. 8. The
same or similar color represent the same or similar crystal
orientation. The black area is the area with a confidence of less
than 0.2. The change of the grain size of the material was
analyzed by the EBSD results. As the number of deformation
passes increased, the dynamic recrystallization fraction
continued to increase, with the narrower grain distribution
interval and the gradually disappeared bimodal structure. The
grain size was smaller and the distribution was more
concentrated, showing an approximately normal distribution.
Specifically, the average grain size was arranged in descending
order of 37.39 μm, 17.73 μm, 14.52 μm, and 4.08 μm in order
of increasing from 1 pass to 4 passes.
Deformation temperature played an important role in the
formation of fine grain structure. Dynamic recrystallization and
grain growth were also closely related to the applied
temperature. The average grain size and precipitation phases
fraction of different passes are shown in Fig. 9. It can be
observed that the average grain size had been significantly
refined during the decreasing temperature deformation process
(1-2 passes, 3-4 passes). The number of precipitated phases
increased significantly, which stimulated the particle
stimulated nucleation (PSN) mechanism and achieved a good
grain refining effect [13]. Compared with 2-3 passes of Fig. 8. OIM maps of RUEed alloy after different passes and corresponding
deformation, the average grain size decreased only with a small grain size distribution chart: (a,e) 1 pass; (b,f) 2passes; (c,g) 3 passes; (d,h) 4
decrease accompanied by the decrease of the precipitated phase passes.
fraction. This was because the reduction of the precipitated
phase weakened the pinning effect, and the PSN effect
weakened at the same time. During the high-temperature
deformation and subsequent air cooling, grain growth occurred.

3.3. Grain boundary characteristics

Grain boundary feature is an important microstructure

feature, which reflects the dynamic recrystallization state of the
material from the side. The EBSD technology was used to
statistically analysis the grain boundary angle of Mg-Gd-Y-Zr
Fig. 9. The trend about average grain size and precipitation fraction of RUEed
alloy after different passes at different temperatures. Fig. 10 alloy after different passes.
826 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830
Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000
The results showed that the grain boundaries of the samples
of 1 pass were mainly low angle grain boundaries (LAGBs). As
can be seen from Table 1, the number of LAGBs reached the
maximum, and 2-5° grain boundaries account for 60.4%. It
showed that the DRX was incomplete after the first pass. In
general, as the number of RUE passes increased, the average
misorientation increased, and LAGBs became less dominant
[16]. However, in the process of variable temperature repetitive
upsetting-extrusion, the amount of LAGBs not decreased
continuously. In the 3 passes with higher deformation
temperature, the fraction of LAGBs increased, and the average
misorientation angle tended to decrease slightly. Finally, in the
sample after 4 passes, the LAGBs fraction decreased again, and
most of the grain boundaries were transformed into high angle
grain boundaries (HAGBs) during the DRX process. The
percentage of remaining LAGBs decreased from 36.2% to
31.8%.
Table 1. Misorientation of RUEed alloy after different passes.
Angle 2°-5° 5°-15° 15°-100°
1 pass, 420Ԩ 0.604 0.119 0.277
2 passes, 410Ԩ 0.164 0.076 0.759
3 passes, 420Ԩ 0.322 0.041 0.637
4 passes, 400Ԩ 0.248 0.070 0.682
Studies have shown that the decrease in LAGB score and
the increase in HAGB score represent the progress of CDRX
[17]. During the deformation process, dislocations slipped,
multiplied, and accumulated, gradually accumulating and
tangling, which promoted the formation of sub-grains. The
continuous movement of dislocations promoted the
transformation of LAGBs into HAGBs, which eventually leads
to the occurrence of DRX. In 3 passes, the precipitation phases
decreased, and the DRXed grains newly formed in 2 passes
Fig. 10. EBSD images of grain boundary structures of RUEed alloy after different passes and corresponding KAM distribution map and corresponding
misorientation distribution：(a,e,i) 1 pass;(b,f,j) 2passes;(c,g,k) 3 passes;(d,h,l) 4 passes.
However, the fraction of LAGBs increased in the samples
treated in 3 passes at 420 ° C. It was well known that as the
deformation temperature increased, dynamic recovery could be
5
grew. As the amount of strain increased, dislocations occurred
inside these DRXed grains, in which continuous dynamic
recrystallization occurred secondary. In 4 passes, the fraction
of LAGBs decreased and the grains continued to refine.
In order to reveal the reason for the formation of grain
boundaries and their evolution, we further analyzed the kernel
average misorientation (KAM) distribution and the
misorientation angle distribution under different deformation
passes, and the results are shown in Fig. 10. It can be found that
there were more regions with higher KAM values at 1 pass and
3 passes with higher deformation temperature, and the average
KAM values were higher than that of the low-temperature
deformed samples. The areas with higher KAM values were
mainly concentrated around the grain boundaries. It was clear
that the KAM values within the coarse grains were higher, and
the fine grain areas were mainly blue, indicating low KAM
values.
Grain refinement occurred first at the grain boundaries and
then extended to the entire grain. According to the mechanism
of the Frank-Read source, dislocations are generated inside the
grains and slip, and they accumulated at the grain boundaries.
Therefore, the dislocation density at grain boundaries was
usually higher than the dislocation density inside the grains
when deformation begins. This was because when the grains
were sufficiently refined, it was more difficult for coarser
grains to activate dislocation generation and movement in
ultra-fine grains [18]. According to the grain boundary
distribution maps, it can be concluded that the area with high
KAM value accumulated a lot of LAGB, which is formed by
the accumulation of dislocations. This provided a sufficient
strain gradient to trigger DRX, which can be inferred as a
potential nucleation site for the upcoming DRXed grains.
promoted [14]. The dislocation recovery in the samples
deformed at 420 °C was higher than the dislocation recovery in
the samples deformed at 410 °C, which resulted in that the grain
 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830
6 Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000
dislocation density in the 3 passed cannot reach the critical
value of the dislocation density for further dynamic
recrystallization. Therefore, as shown in Fig. 10 (c), the LAGB
density in the samples at 3 passes at 420 ° increased. When the
temperature was reduced to 400 ° (4 passes), the speed of
dynamic recovery decreased, and the cumulative strain
increased again, causing the accumulation of dislocations to
reach the density required for dynamic recrystallization, and
further fine grains occurred.
3.4. Texture evolution
Fig. 11 (a-c) shows the inverse pole figure (IPF)and pole
figure (PF) of Mg-Gd-Y-Zr alloy prepared in different passes
along the ED direction. It can be seen from the IPFs that the
[1010] // ED texture was mainly generated in the initial
material. With the increase of processing passes, after 4 passes
of RUE, the [1010] fiber texture disappeared, which was
Fig. 11. IPF and PF images of RUEed alloy after different passes: (a,e,i,m) 1 pass;(b,f,j,n) 2 passes;(c,g,k,o) 3 passes;(d,h,l,p) 4 passes.
As the number of processing passes increased, the grain
orientation changed due to the activation of different strain
paths, and the intensity decreased again (Fig. 11(f-h)). The
strongest intensity point was still deflected about 45 ° from the
ED direction, and the pole density value continued to decrease.
However, the dispersibility of the pole figure increased at high
temperature compared to the deformation at low temperature,
achieving the simultaneous weakening of maximum strength
and texture orientation without any noticeable changes in the
nature of the texture. Observing Fig. 11 (i)-(p), we could find
that the texture intensity of the (1010) (1120) prismatic plane
decreased with the increase of the number of deformation
passes.
827
similar to the results in extrusion Mg-RE alloy [19,20]. A new
rare-earth texture components between [2114] and [2111] and
a new texture component with <2110> orientation parallel to
the ED were generated [21]. As the number of RUE increased,
the maximum texture intensity of inverse pole figure decreased
from 1.839 to 1.228, indicating that the texture was weakening.
Fig. 11 (e-h) shows (0001) pole figures of samples of
different deformation passes. It can be seen (Fig. 11a) that the
RUE sample did not show a typical strong extrusion structure.
After the 1 pass, the peak direction of the texture changed. The
basal plane of most grains was not perpendicular to the
extrusion direction. The strongest value of the pole figure
rotated about 45 °, which may be related to the upsetting and
extrusion process of RUE [12]. Compared with the original
sample, the maximum basal texture intensity of the RUEed
sample decreased to 5.303. The reason for the decrease in
intensity was the change in grain orientation by applying RUE.
It is well known that the strong basal texture of Mg alloys
usually resulted in significant tensile and compression
asymmetry and plastic anisotropy, limiting its application in
many components [22,23]. The Y element in Mg-RE alloy can
promote the activation of the non-basal slip system, thereby
weakening the deformation basal texture [2]. It can be
confirmed that the RUE processes in this study can effectively
randomize and weaken the texture, making the tensile and
compression asymmetry and plastic anisotropy potentially
reduce, improving the formability of the processed Mg alloy
[18].
828 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830
Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000 7

3.5. Evolution of deformation mechanism
The plastic deformation of Mg alloys during deformation is
limited to two main deformation mechanisms, namely slip and
twinning. Twins were not observed in this study, so twins effect
were not considered. There are three common slip modes in Mg
alloy systems: basal a, prismatic <a>, and pyramidal <c+a>.
The initial texture and deformation conditions (ie, temperature
and strain rate) of the alloy strongly affect the activation of any
deformation mechanism, and the prismatic <a> and pyramidal
<c+a> are easily thermally activated [4].
Fig. 12 illustrates the schmid factor (SF) distribution maps
of the basal and non-basal slip system during the repetitive
upsetting-extrusion of different passes. Histogram distribution
of Schmid factor are also presented. It can be seen from the Fig.
12(a,b) (1, 2 passes) that the inside of the coarse deformed
grains usually showed a higher density of yellow to red,
indicating that it has the advantage of high SF grain orientation.
When deformed at low temperature, the SF maps of the basal
slip had more red grains and had a higher average value as a
whole. However, the deformation at high temperature was just
the opposite, showing the higher value of the SF factor of the
non-basal slip.
A close inspection of these histograms showed that for
alloys under different deformation passes, the Schmid factor of
the same type had the same trend, with slightly different
average values. This finding can confirm the phenomenon in
3.4: the texture orientation of the samples in different passes
did not change much.

Fig. 12. Different slip system SF distribution maps and corresponding distribution histograms of RUEed alloy after different passes: (a,e,i,m,q,u) 1 pass;(b,f,j,n,r,v)
2 passes;(c,g,k,o,s,w) 3 passes;(d,h,l,p,t,x) 4 passes.

Fig. 13 shows the average SF values of different slip systems
in different passes in the line chart. It is worth noting that the
SF value of the basal slip was higher when deformed at low
temperature, and the basal slip was not so popular during high
temperature deformation (1,3 passes). The prismatic <a> and
prismatic <c+a> slip had the same high Schmid factor. This
shows that the initiation of different slip systems was closely
related to the deformation temperature. At higher deformation
temperatures, the prismatic a and pyramidal <c+a> slip became
more important.
 Yingze Meng et al. / Procedia Manufacturing 50 (2020) 822–830
8 Y. Meng et al. / Procedia Manufacturing 00 (2019) 000–000
When non-basal slip was easier to activate, they could make
the grains more easily adapt to the strain along the c-axis, but
common slip modes such as basal slip cannot achieved this
[24]. During the high-temperature deformation process, the
lower Schmidt factor of the basal slip made it difficult to active
the basal slip, while the prismatic slip and the pyramidal slip
were promoted. Their combined action can make the basal
plane rotated to a direction different from the extrusion
direction, leading to a more random distribution of the basal
plane and promoting the weakening of the texture [17]. This
confirmed the phenomenon that the orientation of the basal
plane of the (0001) pole figure at low temperature deformation
was more concentrated than that of higher temperature
deformation (Fig. 7). Abouhilou [17] et al. found the same
phenomenon during high temperature uniaxial compression of
AZ31, that is, non-basic slip can promote randomization of
texture.
Fig. 13. The trend of different slip system SF value of RUEed alloy after
different passes.
4. Conclusions
By performing varying temperature repetitive upsetting-
extrusion deformation on Mg-Gd-Y-Zr alloy, the evolution of
microstructure texture and deformation mechanism under
different deformation passes were studied, and the following
conclusions were obtained:
1. As the number of deformation passes increased, the
dynamic recrystallization fraction continued to increase, the
grains continued to refine with the more uniform
microstructure. The decreasing temperature pass was favorable
for the precipitation of the β phase, resulting in pinning effect
and initiating the PSN mechanism, thereby obtaining a more
ideal grain refining effect.
2. The transformation from LAGBs to HAGBs occurred
during deformation, indicating continuous dynamic
recrystallization occurred. During 3 passes at higher
temperatures, the dynamic recrystallized grains grew up, and
due to the increase in strain, dynamic recrystallization was
triggered again, showing an increase in the LAGB number
fraction.
3. Variable temperature repetitive upsetting-extrusion
deformation can effectively weaken the texture. The (1010)
fiber texture disappeared, gradually shifting to a more uniform
distribution between (2-1-14) and (2-1-10). The textures of
(0001), (10-10), and (11-20) were all weakened, and the
829
maximum intensity of the basal texture decreased from 5.303
to 2.582.
4. Temperature had a significant effect on the activate of the
slip system. When the deformation temperature was relatively
low, the SF value of the basal slip was high. While when the
deformation temperature was high, the non-basal slip was more
easily activated, which promoted the randomization of the
texture.
Acknowledgements
This work was supported by the Natural Science Foundation
of Shanxi Province (No.201901D111176), the Key R&D
program of Shanxi Province (International Cooperation)
(No.201903D421036), Scientific and Technological
Innovation Programs of Higher Education Institutions in
Shanxi (No.2018002) and Shanxi Graduate Education
Innovation Project (No.2019BY103).
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