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2 0 2 0;9(4):8001–8012

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Original Article

Grain refining with DDRX by isothermal MDF of

Al-Zn-Mg-Cu alloy

Jiuhui Zhao a , Yunlai Deng a,b,c , Jianguo Tang a,b,∗

a Light Alloy Research Institute, Central South University, Changsha, China
b School of Materials Science and Engineering, Central South University, Changsha, China
c State Key Laboratory of High Performance and Complex Manufacturing, Central South University, Changsha, China

a r t i c l e i n f o a b s t r a c t

Article history: Evolution of grain structure during isothermal multi-direction forging (MDF) of an Al-Zn-Mg-
Received 26 January 2020 Cu alloy at 400 ◦ C and 450 ◦ C with strain rates from 10−3 s−1 to 10−5 s−1 was investigated with
Accepted 9 May 2020 electron backscattering diffraction (EBSD) and transmission electron microscopy (TEM). The
Available online 5 June 2020 results demonstrated that the evolution of grain structure was dominated by discontinuous
dynamic recrystallization (DDRX), during which the continuous forming of new recrystal-
Keywords: lized grains at grain boundaries was found. Characteristics of DDRX was enhanced with the
Multi-directional forging decrease of MDF strain rate or temperature, which promoted the formation of recrystallized
Al-Zn-Mg-Cu grains at grain boundaries. Besides, the increase of total strain enhanced such grain refine-
Discontinuous dynamic ment effect until the grain structure reached the stable state, in which fine recrystallized
recrystallization grains replaced most of the initial coarse grains.
Strain rate © 2020 The Authors. Published by Elsevier B.V. This is an open access article under the
Grain refinement CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

primary properties that benefit from grain refinement [7–12].

1. Introduction Roven et al. [13] reported that grain refinement by forming
fine grains greatly improved the ultimate tensile strength in
MDF is one of the most common used severe plastic defor-
the aluminum alloy. Besides, the ductility was found to be
mation (SPD) method, in which a very high strain could
enhanced with ultrafine grains in the Mg alloy [14–20]. There-
be achieved without changing the overall dimension of the
fore, grain refinement obtained through MDF has attracted lot
deformation materials. Significant grain refining effect was
of attention in recent years.
reported by employing MDF method in various metals, such as
The MDF method was also widely used on aluminum
in the magnesium alloys [1,2], copper alloy [3], titanium alloy
alloys for the reason of that aluminum alloys are high stack-
[4,5], as well as aluminum alloys [6]. Furthermore, the grain
ing fault energy (SFE) alloys, during which dynamic recovery
structure of these metals was regarded as a key factor affecting
quickly occurred and dynamic recrystallization was hindered
most of their properties, the strength and ductility were the
[21–25]. The initial coarse grains would be gradually replaced
by the recrystallized grains formed during MDF, the increase
of the total strain promoted the formation of fine grain within
∗
Corresponding author. grain interiors. The grain structure of aluminum alloys after
E-mail: jgtang@csu.edu.cn (J. Tang). MDF was composed of sub-grains and recrystallized grains
https://doi.org/10.1016/j.jmrt.2020.05.033
2238-7854/© 2020 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
8002 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012

Fig. 1 – (a) EBSD map and (b) misorientation distribution of the homogenized Al-Zn-Mg-Cu alloy.

developed within grain interiors. Therefore, the grain struc-

ture containing different number of sub-grains and recrystal-
lized grains could be controlled with different total strain.
It has been generally accepted that great grain refinement
obtained during MDF is based on the characteristic continuous
dynamic recrystallization (CDRX), during which sub-grains
would be gradually formed within grain interiors accompa-
nied by their transformation into fine grains. The increase of
total strain during MDF promoted the formation of fine grains
within grain interiors and enhanced grain refinement effect
[21–25]. Beside, grain refinement effect would also be acceler-
ated with decreasing the MDF strain rate [21] or increasing the
MDF temperature [25]. Diverse grain refinement effect could be
achieved by controlling the deformation parameters of tem-
perature, total strain and strain rate during hot MDF based on
CDRX.
However, the DDRX (discontinuous dynamic recrystal-
lization) characteristic is gradually highlighted with further
decreasing the MDF strain rate or increasing temperature Fig. 2 – Schematic map of isothermal MDF.
during isothermal MDF, recrystallization mechanism would
be transformed gradually from CDRX to DDRX [26,27]. New
recrystallized grains are formed at grain boundaries while the
experiment were machined from the homogenized Al-Zn-Mg-
nucleation and growth of recrystallized grains could be distin-
Cu alloys.
guished, which is considered as characteristic of DDRX [28–30].
Isothermal MDF is conducted at temperatures of 400 ◦ C and
But quite a few literatures reported related recrystallization
450 ◦ C with strain rates of 10−3 s−1 , 10−4 s−1 and 10−5 s−1 with
behavior during MDF of aluminum alloy with dominant char-
total strain of ε = 2.8. The schematic maps of isothermal
acteristics of DDRX. Therefore, an Al-Zn-Mg-Cu alloy was
MDF is shown in Fig. 2, isothermal MDF is performed along
subjected to isothermal MDF at temperatures of 400 ◦ C and
the compression direction X → Y → Z → X, and changing the
450 ◦ C with strain rates from 10−3 s−1 to 10−5 s−1 to explore
compression direction between every two pass with each pass
the effect of deformation temperature and strain rate on grain
strain of 0.7. These MDF samples are heated with heating
refinement based on the DDRX.
rate of 20 ◦ C/s to isothermal MDF temperature and hold at
the temperature for 5 min before isothermal MDF, and then
isothermal MDF was performed with a lubricant powder of
2. Experimental procedure boron nitride, then the samples were quenched with room
temperature water after MDF.
A homogenized Al-Zn-Mg-Cu alloy is used to in this study, Specimens cut from central part of the MDF samples
and the alloy composition is Al-5.47Zn-2.19Mg-2.11Cu-0.12Zr- were used for microstructural characterization with electron
0.01Cr-0.1Fe-0.01Mn (wt.%). The EBSD map and distribution backscattering diffraction (EBSD) analysis as a FEI scanning
of misorientation of the homogenized alloy are shown in electron microscopy with field emission gun. The examina-
Fig. 1, the frequency of HAGB is about 84.5% with the average tion surface was perpendicular to the compression direction.
grain size approximation 47 ␮m. Rectangular samples with the The samples before EBSD examination were electro-polished
size of 10 mm × 9 mm × 5.5 mm subjected to isothermal MDF in a solution of 10% HClO4 and 90% C2 H5 OH at 20 ◦ C. The
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012
Fig. 3 – The EBSD maps of samples after MDF at 10−3 s−1 and 400 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.
EBSD data were collected and analyzed with Oxford software.
The average grain size were evaluated using the line-intercept
technique, the low-angle grain boundaries (LABs) with 2◦ and
15◦ are depicted as thin lines while the high-angle grain bound-
aries with misorientation >15◦ are depicted as thick lines.
The grain structure of the MDF samples were also observed
by transmission electron microscopy (TEM) techniques. MDF
samples for TEM investigation were ground to the thickness
of about 50 ␮m and polished in a solution of 30% HNO3 and
70% CH4O with twin jet instrument. A Libra 200FE transmis-
sion electron microscope (TEM) operated at 200KV was used
to investigate the grain structure.
3. Results
3.1. The evolution of grain structure during MDF at
different strain rates
Fig. 3 shows the EBSD maps of samples after MDF at 400 ◦ C
and 10−3 s−1 with strains of 0.7, 1.4, 2.1 and 2.8, correspond-
ing frequency of HAGB and average size of sub-grains and
recrystallized grains are shown in Fig. 4. For the strain of
0.7, some sub-grains are developed within grain interiors and
a few recrystallized grains are formed at grain boundaries.
8003
As the total strain is increased from 0.7 to 2.8, the number
of recrystallized grains formed at grain boundaries increases
gradually while the number of sub-grains developed within
grain interiors do not change too much. Gradually increased
fine recrystallized grains increases the frequency of HAGB
from 31.4% to 51.4% as the total strain is increased from 0.7 to
2.8. Besides, the average size of recrystallized grains increases
slowly from 9.7 ␮m to 10.4 ␮m while the average size of sub-
grains is kept around 7.8 ␮m.
Fig. 5 shows the grain structure of samples after MDF at
400 ◦ C and 10−4 s−1 with strains of 0.7, 1.4, 2.1, and 2.8, corre-
sponding grain characterizations are shown Fig. 6. In contrast
to the grain structures after MDF at 10−3 s−1 and 400 ◦ C, low-
ering the MDF strain rate to 10−4 s−1 promotes the formation
of fine recrystallized grains while hinders the development of
sub-grains within grain interiors. For the strain of 0.7, many
fine grains are formed at grain boundaries and some sub-
grains are developed within grain interiors. Fine grains are
continuously formed with the increase of the total strain from
0.7 to 2.8, which leads the increase of the HAGB frequency
from 48.2% to 58.4%. The average size of recrystallized grains
increases from 7.8 ␮m to 8.3 ␮m as the total strain is increased
from 0.7 to 1.4, and then it decreases from 8.3 ␮m to 7.7 ␮m
by further increasing the total strain from 1.4 to 2.8. This is
8004 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012

Fig. 4 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains and sub-grains of
samples after MDF at 10−3 s−1 and 400 ◦ C.

Fig. 5 – The EBSD maps of samples after MDF at 10−4 s−1 and 400 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.

because many recrystallized grains are formed to replace the
initial coarse grains, and many sub-grains developed within
coarse grains are consumed to provide the driving force for the
growth of recrystallized grains as the total strain is increased
from 0.7 to 1.4. And many more fine recrystallized grains are
gradually formed at grains boundaries by further increasing
the total strain from 1.4 to 2.8, the growth of recrystallized
grains are hindered by each other. Besides, the average size
of sub-grains is kept around 7.2 ␮m accompanied by slowly
decrease with the increase of total strain, because coarse
grains where coarse sub-grains are developed decreases with
the increase of strain.
When isothermal MDF is performed at 10−5 s−1 and 400 ◦ C,
the number of fine recrystallized grains formed at grain
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012 8005

Fig. 6 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains and sub-grains in
the samples after MDF at 10−4 s−1 and 400 ◦ C.

Fig. 7 – The EBSD maps of samples after MDF at 10−5 s−1 and 400 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.

boundaries is much more as compared with that developed
at strain rate of 10−4 s−1 , as seen in Fig. 7. For the strain of
0.7, many fine recrystallized grains are formed and only a
few sub-grains are developed within grain interiors. When
the MDF total strain is increased to 1.4, an almost completely
recrystallized grain structure with an average size of 8.2 ␮m
are developed, which leads to a high HAGB frequency 82.3%.
As the total strain continues to increase from 1.4 to 2.8, the
change of the grain structure is moderate, the frequency of
HAGB is kept around 82%. The average size of recrystallized
grains decreases from 9.4 ␮m to 8.2 ␮m as the total strain is
increase from 0.7 to 1.4 for large number of fine recrystal-
lized grains are formed and the growth of recrystallized grains
are hindered by each other. The average size of recrystallized
8006 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012
Fig. 8 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains and sub-grains in
the samples after MDF at 10−5 s−1 and 400 ◦ C.
grains increases from 8.2 ␮m to 9.2 ␮m by further increasing
the total strain from 1.4 to 2.8, because recrystallized grain
size tends to be larger for the grain structure to reach the
more stable state during subsequent deformation for the grain
structure with completely recrystallized grains. Besides, the
grain structures of the samples after MDF with total strain of
2.1 and 2.8 are consisted of equiaxed recrystallized grains. This
is because of that large number of new equiaxed grains are
continuous formed to replace those elongated grains as large
number of HAGBs provides nucleation sites for the formation
of recrystallized grains (Fig. 8).
3.2. The evolution of grain structure during MDF at a
higher temperature
Compared with the grain structures developed at 400 ◦ C with
strain rates from 10−3 s−1 to 10−5 s−1 , the average grains size
is much larger and the number of fine recrystallized grains is
much less in the samples after MDF at the higher temperature
of 450 ◦ C, as shown from Figs. 9–14.
Fig. 9 shows the grain structures developed at 10−3 s−1 and
450 ◦ C with total strains of 0.7, 1.4, 2.1, and 2.8, corresponding
grain characterizations of grain size and frequency of HAGB
are shown in Fig. 10. Both recrystallized grains and sub-grains
are formed after MDF at 10−3 s−1 with total strains of 0.7. The
number of recrystallized grains increases gradually with the
increases of the total strain from 0.7 to 2.1, which leads to the
increasing of the frequency of HAGB from 34.8% to 45.2% while
the average size of those recrystallized grains formed at grain
boundaries increases from 11.7 ␮m to 16.4 ␮m. Besides, the
change of the grain structure is faint with further increasing
of the total strain from 2.1 to 2.8.
Fig. 11 shows the grain structures developed at 10−4 s−1 and
450 ◦ C with total strains of 0.7, 1.4, 2.1, and 2.8, corresponding
grain characterizations of grain size and frequency of HAGB
are shown in Fig. 12. In contrast to the grain structures devel-
oped at 10−3 s−1 , lowering the strain rate to 10−4 s−1 reduces
the number of sub-grains while the number of recrystallized
grains is similar. In addition, only moderate change occurs in
the grain structure as the total strain is increased from 0.7
to 2.8, the frequency of HAGB increases slowly from 52.3%
to 58.1% and the average size of those recrystallized grains
increases from 13.4 ␮m to 16.1 ␮m.
Fig. 13 shows similar grain structures developed after MDF
at 10−5 s−1 and 450 ◦ C with total strains of 0.7, 1.4, 2.1 and 2.8,
which leads to the formation of most number of recrystal-
lized grains as compared with the grain structures developed
at 10−3 s−1 and 10−4 s−1 . Fig. 14 shows that the frequency of
HAGB increases slowly from 55.8% to 59.5%, the average size of
those recrystallized grains increases from 13.6 ␮m to 15.2 ␮m
as the total strain is increased gradually from 0.7 to 2.8.
4. Discussion
4.1. Greatest grain refinement state
The evolution of the grain structures during MDF at the tem-
peratures of 400 ◦ C and 450 ◦ C with strain rates from 10−3 s−1
to 10−5 s−1 showed that recrystallized grains formed at grain
boundaries increased with the increase of the total strain,
which is the results of DDRX. The initial coarse grains would
be gradually replaced by those recrystallized grains, greatest
grain refinement could be obtained when almost initial coarse
grains disappeared. The grain structure of MDF samples would
reach a stable state after those recrystallized grains replaced
most of initial coarse grains, after which the change of grain
structure was faint with further increasing of the total strain.
This is because the formation of recrystallized grains and the
grain growth were balanced. Fig. 15 shows the change of grain
structure after it reaches the balance state with a sketch map.
A stable state of grain structure with a mixture of coarse
recrystallized grains of 1, 2 and 3, and fine recrystallized grains
of 4, 5 and 6 are shown in Fig. 15(a), dislocations and a few
sub-grains are found within coarse grains while almost none
dislocations and sub-grains appears in the fine recrystallized
grains. Fig. 15(b) shows the grain structure after subsequent
MDF, the grains of 1, 2 and 3 shown in Fig. 15(a) were replaced
by the growth grains of 4, 5 and 6. Besides, new recrystallized
grains of 7, 8, and 9 are formed accompanied by developing
of dislocations and sub-grains within the growth grains of 4,
5 and 6 after subsequent MDF. Therefore, the changes of the
grain structure is faint with the increase of strain after the
grain structure reached the stable state.
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012 8007

Fig. 9 – The EBSD maps of samples after MDF at 10−3 s−1 and 450 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.

Fig. 10 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains and sub-grains in
the samples after MDF at 10−3 s−1 and 450 ◦ C.

As seen from Fig. 16, none dislocations are found within
fine recrystallized grains in the samples after isothermal MDF
at 10−3 s−1 with temperatures of 400 ◦ C and 450 ◦ C. However,
many dislocations and sub-grains appeared in the coarse
grains, which provide the strain energy for the formation and
growth of recrystallized grains.
4.2. Effect of the strain rate and temperature on the
grain refinement
The grain structure would reach a stable state when recrystal-
lized grains replaced most of initial coarse grains during MDF
at temperatures of 400 ◦ C and 450 ◦ C with strain rates from
8008 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012

Fig. 11 – The EBSD maps of samples after MDF at 10−4 s−1 and 450 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.

Fig. 12 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains and sub-grains in
the samples after MDF at 10−4 s−1 and 450 ◦ C.

10−3 s−1 to 10−5 s−1 . Therefore, grain refinement effect would
not be enhanced with further increasing the total stain after
the grain structure reaches stable state. Therefore, occurring
a total strain when the grain structure reaches the stable state
under different MDF conditions, which is named as the turn-
ing point. Fig. 17 shows the effect of the increase of total strain
on the HAGB frequency and grain size during MDF, the turning
points were depicted by yellow hollow shape. The total strain
of the turning point decreases with the increase of the MDF
temperature from 400 ◦ C to 450 ◦ C during MDF at the strain
rates from 10−3 s−1 to 10−5 s−1 , which means that the increase
of MDF temperature accelerates the grain refinement effect, as
shown in Table 1. Because both the movement of dislocation
and migration of grain boundaries would be faster at a higher
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012 8009

Fig. 13 – The EBSD maps of samples after MDF at 10−5 s−1 and 450 ◦ C with strains of: (a) 0.7, (b) 1.4, (c) 2.1, (d) 2.8.

Fig. 14 – The influence of total strain on the (a) the frequency of HAGB, (b) the average of recrystallized grains and sub-grains
in samples MDF at 10−5 s−1 and 450 ◦ C.

MDF temperature, which could accelerate the formation and
growth of recrystallized grains. The decrease of the strain rate
from 10−3 s−1 to 10−5 s−1 also reduces the total strain of the
turning point during MDF at temperatures of 400 ◦ C and 450 ◦ C,
which means the grain refinement effect could be accelerated
by decreasing MDF strain rate. Because the time to balance
the formation of fine grains and the growth of recrystallized
grains is much more at the lower strain rate.
The competition between the formation of new grains and
grain growth would be gradually reaching the equilibrium with
the increase of total strain during the MDF based on the DDRX.
The grain growth was driven by grain boundaries migration.
8010 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012

Fig. 15 – The sketch map of the evolution the grain structure after it reaches the stable state.

Fig. 16 – TEM maps of samples after isothermal MDF at 10−3 s−1 and temperatures of: (a) 400 ◦ C, (b) 450 ◦ C.

Fig. 17 – The influence of total strain on the (a) frequency of HAGB, (b) average size of recrystallized grains in samples after
MDF at strain rates range from 10−3 s−1 to 10−5 s−1 and temperatures of 400 ◦ C and 450 ◦ C.

The mobility of the grain boundaries in dynamical recrystal- where Q is activation energy, M0 is a constant, T is the temper-
lization is temperature dependent, and the Arrhenius type ature of deformation, and R is the universal gas constant.
relationship is employed in this study: It is obvious that the growth of recrystallized grains is much
faster at a higher temperature according to the Eq. (1), which
leads to larger average size of recrystallized grains at 450 ◦ C
 Q than 400 ◦ C during MDF, as seen in Fig. 17(b). Furthermore,
M = M0 exp − (1) because of many of the strain energy was consumed for the
RT
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(4):8001–8012
Table 1 – The turning piont of total strain after the grain
structure reaches the stable state during the MDF at
strain rates from 10−3 s−1 to 10−5 s−1 and temperatures
of 400 ◦ C and 450 ◦ C.
Temperature\strain rate 10−3 s−1 10−4 s−1 10−5 s−1
400 ◦ C 2.8 2.1 1.4
450 ◦ C 2.1 1.4 0.7
grain growth, which leads to less strain energy for the for-
mation of new recrystallized grains during MDF at a higher
temperature of 450 ◦ C. Therefore, the number of recrystallized
grains is much less after MDF at 450 ◦ C than that after MDF at
400 ◦ C.
For the samples developed during MDF at the temperature
of 400 ◦ C, the decrease of strain rate from 10−3 s−1 to 10−5 s−1
increases the number of fine recrystallized grains, which indi-
cates that grain refinement effect is gradually enhanced with
the decrease of the MDF strain rate. This is because the num-
ber of sub-grains decreases gradually as the strain rate is
decreased from 10−3 s−1 to 10−5 s−1 , less strain energy is used
for the formation of sub-grains while much more strain energy
is used for the formation of fine recrystallized grains. Besides,
for the samples during MDF at the temperature of 450 ◦ C, the
decrease of strain rate also increases the number of recrystal-
lized grains.
5. Conclusions
The evolution of grain structures during MDF of an Al-Zn-Mg-
Cu alloy at 00 ◦ C and 450 ◦ C with strain rates from 10−3 s−1
to 10−5 s−1 were investigated. The conclusion can be summa-
rized as follows:
(1) DDRX was the key mechanism during the MDF under
different deformation conditions, during which the for-
mation of fine grains at grain boundaries was the main
change of the grain structure. But grain refinement with
forming fine recrystallized grains would not be enhanced
with further increasing of total strain after the grain struc-
ture reaches the stable state, in which recrystallized grains
replacing most of initial coarse grains
(2) The decrease of MDF strain rate from 10−3 s−1 to 10−5 s−1
accelerated and enhanced grain refinement with form-
ing fine recrystallized grains when MDF was performed
at 400 ◦ C and 450 ◦ C.
(3) The increase of MDF temperature from 400 ◦ C to 450 ◦ C
accelerated grain refinement with forming recrystallized
grains but weakened grain refinement effect when MDF
was performed at strain rate from 10−3 s−1 to 10−5 s−1 .
(4) The optimum condition for grain refinement is MDF at
400 ◦ C with strain rate of 10−5 s−1 , during which largest
number of fine recrystallized grains are formed with only
total strain of 1.4.
Conflict of interest
The authors declare no conflicts of interest.
8011
Acknowledgments
This work was supported by Science and Technology on
High Strength Structural Materials Laboratory, Central South
University, Changsha 410083, China, the Foundation for Key
Laboratory of National Defense Science and Technology for
equipment pre-research [grant number 41422010705], and the
Safety Project of National Defense Laboratory (6142912180104).
The authors would like to take this opportunity to express
their appreciation.
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