Materials & Design 210 (2021) 110057

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Materials & Design

journal homepage: www.elsevier.com/locate/matdes

Deformation heterogeneity induced coarse grain refinement of the

mixed-grain structure of 316LN steel through limited deformation
condition
Yangqi Li a, Ping Shen b, Haiming Zhang a,⇑, Kai Dong c, Yang Deng a, Xianwang Chen a, Zhenshan Cui a,⇑
a
Institute of Forming Technology and Equipment, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200030, China
b
Center for Advanced Solidification Technology (CAST), School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China
c
Shanghai Electric SHMP Casting & Forging Co., Ltd., Shanghai 200245, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 MCG grain size plays a significant role

in strain partitioning.
 MCGs can be refined by limited cold
deformation followed by rapidly
heating process.
 Distinct dislocation piles up in MCG
GBs under small deformation and
initiates SRX.
 SRX occurs at both GBs and interior of
the MCG when deformation is
relatively large.

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

Article history: The defect of mixed-grain structure with millimeter-grade coarse grains (MCGs) is frequently found in
Received 13 July 2021 heavy forgings, such as nuclear main pipes manufactured from 316LN steel. Renovation of such kind forg-
Revised 16 August 2021 ings can only be conducted through recrystallization. However, the allowed deformation is limited
Accepted 19 August 2021
because the geometric size of forgings should be maintained during the renovation. For this purpose,
Available online 20 August 2021
the deformation heterogeneity of 316LN steel with mixed-grain structures were studied experimentally,
which demonstrated that the MCGs were more inclined to deform than fine grains even if MCGs are with
Keywords:
hard orientations. Therefore, a two-stage method was studied to refine MCGs, which takes the advantage
316LN austenitic stainless steel
Mixed-grain structure
of this deformation heterogeneity. The first stage was to impose a limited deformation to the steel at
Deformation heterogeneity room temperature, suppressing the dynamic recovery and leading the preferentially deformed MCGs
Grain refinement to accumulate enough deformation energy storage. The second stage was rapidly heating the deformed
In-situ SRX observation materials to realize static recrystallization (SRX). The results showed that the MCGs were completely
refined by SRX even if the reduction rate is only 8%. The SRX mechanisms and refining assessments of
MCGs under different deformation conditions were discussed. This work, thus, provides an effective
method to salvage the heavy structures in engineering.
Ó 2021 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

⇑ Corresponding authors. Austenitic stainless steel ASTM-TP316LN (316LN) is widely

E-mail addresses: hm.zhang@sjtu.edu.cn (H. Zhang), cuizs@sjtu.edu.cn (Z. Cui). used in the nuclear power station equipment, e.g., the main pipe

https://doi.org/10.1016/j.matdes.2021.110057
0264-1275/Ó 2021 Published by Elsevier Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Y. Li, P. Shen, H. Zhang et al.
[1,2], due to its excellent combination of high strength, good corro-
sion resistance, and adequate weldability [3,4]. However, the
mixed-grain structures were frequently detected in the 316LN
steel forgings, in which coarse grains of sub-millimeter or even
millimeter size (MCGs) arise due to the unavoidable temperature
gradient and inhomogeneous deformation during multi-pass hot
forging process [5]. The existence of the mixed-structure with
abnormally large grains will have catastrophic effects on the
mechanical performances of materials [6,7], so that the forgings
should be scrapped if the large grains cannot be refined. Heavy
forgings like the main pipes often cost million dollars or even more,
therefore, refining the mixed-grain structures of the steel is crucial
to avoid the forgings abandoned. However, the renovation of the
mixed-grain forgings is limited by the allowable deformation:
large deformation will cause a forging distorted in shape and also
leads it to be scrapped. Therefore, for the austenitic stainless steel
whose grain cannot be refined by heat treatment, a suitable grain
refinement method under the limitation of deformation is crucially
required.
In order to prepare metallic materials with good mechanical
performances, the formation mechanisms [8,9] and refining meth-
ods [10,11] of the mixed-grain structure have attracted extensive
research interest over the past few decades. Two common pro-
cesses to obtain fine grains without changing the chemical compo-
sition are the phase transformation and recrystallization,
respectively [12,13]. However, the 316LN austenitic stainless steel
is a single-phase material and no phase transformation takes place
during the conventionally thermo-mechanical treatment [14].
Consequently, the recrystallization is the only way for the grain
refinement of this steel in the practical engineering. In our previous
work, the refinement of the mixed-grain structure with MCGs was
studied through isothermal compression experiments, i.e., through
dynamic recrystallization (DRX) [15]. It was concluded that the
MCGs can be completely fragmented and refined under the defor-
mation condition of temperature of 1200 °C and reduction rate of
50%. However, this method is not suitable for the renovation of
forgings with coarse grains because of the limitation of allowed
deformation.
In our recent work [16], it is observed in the room temperature
condition that MCGs were preferentially deformed than fine grains
even if some of them are with hard orientations, and local shear
bands were found to be intensively formed inside MCGs. Since
many literatures have reported that shear bands are privileged
sites for the nucleation of new grains and provides driving force
for recrystallization [17–19], it is inferred that the MCGs are possi-
bly refined if they receive more dislocation density than fine grains
due to the deformation heterogeneity, even in small deformation
conditions. However, if the deformation happened in high temper-
ature environment, large part of dislocation can be annihilated due
to dynamic recovery. Therefore, we assume that the refinement of
the MCGs may be achieved through a two-stage method: the first
stage is to deform the materials by a limited deformation at room
temperature or a low temperature that can suppress the dynamic
recovery [20,21]; the second stage is rapidly heating the deformed
materials to realize static recrystallization (SRX). This idea is aimed
to take full advantages of the deformation energy to prompt the
recrystallization.
To realize this idea, this study takes the nuclear grade 316LN
austenitic stainless steel with the MCG mixed-grain structure as
the research object, and the SRX processing conditions were imple-
mented to refine the coarse grains. In order to find the minimum
deformation amount that is effective to refine the MCGs, tests with
different deformation conditions were carried out. To probe the
characteristics of microstructure evolution of mixed-grain struc-
ture, the SRX processes were in-situ observed by applying high
temperature laser scanning confocal microscopy (HTLSCM). Trans-
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Materials & Design 210 (2021) 110057
mission electron microscopy (TEM) was also employed to observe
the dislocation distribution and to elucidate the SRX mechanism of
samples under different deformation conditions. The effects of
MCG refinement were compared and evaluated.
2. Materials and methods
2.1. Specimen preparation
The materials investigated in this study are from as-forged
316LN stainless steels, which is provided by Shanghai Electric
SHMP Casting & Forging Co., Ltd. The chemical composition of
the studied material is exhibited in Table 1. The as-received mate-
rials with MCG mixed-grain structure were shaped into cuboid
compression samples by wire cut. The dimension of the sample
was designed as 3.5 mm (length)  2.5 mm (width)  5 mm
(height, compression direction) for the convenience of in-situ
observations. Before and after the mechanical testing, all the sam-
ples underwent the standard mechanical grinding followed with
the electrochemical polishing as well as the EBSD measurements
using a SEM-EBSD system from the FEI Nova 230/IAC SEM. The
electrolyte for electrochemical polishing is 10% oxalic acid solution,
the voltage is 2 V, and the electrolytic time is 5 min at a room tem-
perature. The electrochemical polishing is a suitable method for
austenitic stainless steel to remove the layers strained by mechan-
ical polishing and grinding. The results show that, for specimens of
316LN steel, the resolution rates of EBSD tests can reach more than
95% when the surface layer of 15 lm in thickness was removed by
the electropolishing process.
2.2. Experimental methods
2.2.1. Compression experiments at room temperature
The compression experiments were conducted at room temper-
ature (RT) and strain rate of 0.001 s 1 on a SANS CMT5305 (MTS)
universal testing machine. To minimize the effect of the friction
between the die and the sample during compression tests, the sur-
faces of upper and lower die were polished. Fig. 1a shows the con-
figuration of compression tests, and Fig. 1b shows the typical
mixed-grain structure with MCGs observed by an optical micro-
scopy (OM; Zeiss Axio Imager M2m). The reduction rates (RRs)
are designed as 25%, 15%, 10%, 8% and 6.5%. The RRs of compression
experiments were manually guaranteed by the comparison of
height measurements before and after the sample deformation.
2.2.2. In-situ SRX experiments
In order to investigate the SRX mechanism of 316LN steel with
mixed-grain structure, in-situ experiments of the samples
obtained by compression tests at RT were conducted on the
HTLSCM setup (VL2000DX-SVF17SP, Yonekura MFG Co., Japan).
Fig. 2 shows the schematic illustration of temperature history
and the HTLSCM setup. The principle of using the thermal etching
method to display the grain boundary (GB) at high temperature of
HTLSCM can be found in detail in Yogo et al. [22]. The reliability of
this method to reveal GBs has been proved by literature [23]. First,
the samples were heated to 200 °C at a rate of 50 °C/min, which is
equivalent to a drying treatment to the sample. Then, the samples
were directly heated to the testing temperature 1250 °C at the fast-
est rate of 1000 °C/min, with the holding time for 10 min. This tem-
perature is determined for the convenience of observation because
it was observed that the materials turned black when the holding
temperature is between 900 °C and 1200 °C. Also, the austenite
phase is stable at 1250 °C [14]. After holding, the samples were
quenched by nitrogen air to maintain the newly formed
microstructure. During the holding time, the sample was pho-
Y. Li, P. Shen, H. Zhang et al.
Table 1
The chemical composition (wt. %) of the studied material.
Element C Cr Ni Mo
wt. % 0.02 17.46 11.33 2.11
tographed at frequency of 1 Hz to record the microstructure evolu-
tion. After in-situ SRX observations, the tested samples were exam-
ined by EBSD measurements to evaluate the refinement of MCGs.
2.2.3. TEM observations
In order to explore the relationships between deformation con-
dition and the SRX process, TEM by using JEM2100 transmission
electron microscope at the voltage of 200 kV were conducted to
observe the dislocation distribution. For the pre-deformed cuboid
samples with MCG mixed-grain structures in the center, new cylin-
drical specimens with diameter of 3 mm were prepared by wire
cutting, in which the center of each cylinder specimen coincides
with the center of the corresponding sample. Thin slices were then
prepared from the cylindrical specimens. The thin slices for TEM
observations were first mechanically polished down to 80 lm, fol-
lowed by twin-jet electropolishing using an electrolyte (main-
tained at 35 °C) of 4% perchloric acid in ethanol, and finally ion
polished by Gatan PIPS II.
3. Results
3.1. Surface morphologies after compression experiments at RT
After compression experiments at RT, the surface morphologies
of samples under different RRs are shown in Fig. 3, in which the
slip traces are clearly exhibited on the surfaces. It can be found that
MCGs exhibits much more dense slip traces than the fine grains
(FGs), inferring that the deformation is very inhomogeneous and
the MCGs receives much more strain than the FGs. When deforma-
tion is small (e.g., 8% RR shown in Fig. 3d and 6.5% RR shown in
Fig. 3e), some FGs even have no obvious slip trace on their surfaces.
Fig. 4 shows a local morphology and the corresponding Schmid fac-
tor (SF) distribution of the sample underwent 8% compression. It
can be found from Fig. 4a that significant surface slip traces were
observed in the MCG 1 and 2, while no slip trace in the clusters
of fine grains 3 and 4 (see Fig. 4c and d). Note that the SFs of the
MCG 1 and 2 are 0.43 and 0.39, respectively, both are lower than
the SFs of the clusters of fine grains 3 and 4. It indicates that at a
small RR, the plastic deformation is mainly undertaken by MCGs
Fig. 1. (a) Configuration of compression tests at room temperature, (b) typical
morphology of mixed-grain structure with MCGs in 316LN austenitic stainless steel.
Materials & Design 210 (2021) 110057
Mn N Si P S Fe
1.62 0.148 0.47 0.02 0.002 66.82
even if some of them are with hard orientations, i.e., the grain size
plays a more important role in strain partitioning than the crystal-
lographic orientation when the difference of grain size is big. When
the deformation increased to some extent (e.g., 10% RR), obvious
slip traces began to appear on the surfaces of FGs.
It is known that annealing twins usually occur when heat treat-
ments are conducted on strained metals with low stacking fault
energies (e.g., the face-centered cubic metallic material). The role
of the annealing twin playing in plastic deformation is usually
thought to resemble that of a new grain, and the twin boundary
acts as a barrier against the dislocation motion [24]. An interesting
phenomenon is shown in Fig. 3e that the MCG was penetrated by
an annealing twin band. However, the slip traces on the MCG sur-
face were not blocked by the twin band, on the contrary, if regard-
ing the twin band as a boundary, the slip traces on the upper and
lower surfaces of MCG have good consistencies both in number
and width, indicating that the internal annealing twin band has lit-
tle effect on the strain partitioning of MCG.
3.2. MCG refinements during in-situ SRX experiments with 25%, 15%
and 10% RRs
After grinding and electrochemical polishing of each
deformed sample, in-situ SRX observations were carried out.
The microstructure evolutions of thermal etched samples with
compression of 25%, 15% and 10% RRs are shown in video 7, 6
and 5, respectively, in which the samples exhibited surface slip
traces in both MCGs and FGs under these deformation conditions
(see Fig. 3). Fig. 5 is a graphical illustration of these videos. Gen-
erally, the SRX incubation time of samples was prolonged with
the decrease of the RR. In the sample with 25% RR, it was
observed that new GBs appeared in the interior of MCGs before
heated to 1250 °C (see Fig. 5a1), while in the sample with 10%
RR, new GBs appeared after being heated to 1250 °C for 60 s
(see Fig. 5c2). Nevertheless, the SRX finish time of each sample
was basically consistent. It indicates that the amount of plastic
deformation plays a significant role in the incubation of SRX
but has less effect on the completion of SRX. Besides, the intra-
granular nucleation was observed in the sample with 25% RR as
Fig. 2. Schematic illustration of the SRX process and the HTLSCM setup.
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Y. Li, P. Shen, H. Zhang et al. Materials & Design 210 (2021) 110057

Fig. 3. Surface morphologies of each sample after compression tests under different RRs: (a) 25%, (b) 15%, (c) 10%, (d) 8%, (e) 6.5%.

shown in Fig. 5a1, while the nucleation at GBs was observed in
the sample with 10% RR as shown in Fig. 5c2. The GB migrations
were observed in recrystallized grains during the temperature
holding, as shown in Fig. 5a3, b4 and c4.
The observed different SRX nucleation mechanisms indicate
different SRX incubation processes. Therefore, the SRX incubation
of samples with 25% and 10% RRs were recorded in detail, and
the results are shown in video 1 (25% RR) and video 2 (10%
RR). Fig. 6 is a graphical illustration of the two videos. From
video 1, it was observed that the SRX process started when
the temperature rose to 1100 °C. The recrystallized area
expanded like a flood tide from the MCG GBs as well as from
the interior of MCG. This movement is actually driven by the
GB bulging. If focusing only on the site marked in Fig. 6a1 and
then examining video 1, two types of flood tide movements
(i.e., GB bulging) can be found: one coming from the GBs on
the upper right and the other coming from an inner-MCG site.
These two movements joined forming a ‘collision front line’,
eventually forming new GBs (see the microstructure after air
quenching in Fig. 6b1 and the corresponding all Euler map
obtained by EBSD measurements in Fig. 6c1). However, in video
2, it was found that the bulging motions from the MCG GBs
joined forming a ‘collision front line’ and new GBs were formed
eventually (see the microstructure after air quenching in Fig. 6b2
and the corresponding all Euler map obtained by EBSD measure-
ments in Fig. 6c2). These experimental phenomena together with
the nucleation mechanisms in Fig. 5 reveal that the new grains
nucleate both at the MCG GBs and inside the MCG when the
sample received a relatively large deformation (e.g., 25% RR),
and grow up in the manner of GB bulging. However, if the sam-
ple received a relatively small deformation (e.g., 10% RR), the
new grains nucleate only at the MCG GBs, and also grow up in
the manner of GB bulging. Additionally, some original MCG
GBs in the sample with 10% RR before heating were observed
as remained after the SRX process; while the original MCG GBs
is not remained in the sample with 25% RR. It indicates that

Fig. 4. The role of grain size in mixed-grain structure playing in the strain partitioning. (a) Surface morphology of the sample under 8% RR, (b) the corresponding Schmid
factor distribution along the compression direction of the undeformed sample, and (c), (d) are zoomed-in observations in (a).

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Y. Li, P. Shen, H. Zhang et al. Materials & Design 210 (2021) 110057

Fig. 5. Thermal etched microstructure evolution of samples with deformation of (a) 25%, (b) 15% and (c) 10% RRs at the holding temperature of 1250 °C for 600 s. HT
represents the holding time.

the deformation energy at MCG GBs of the sample with 10% RR
is nonuniformly distributed. The MCG GBs with high deforma-
tion energy cannot be remained due to the recrystallization
nucleation and growth after heating, while the MCG GBs with
low deformation energy will be remained because they are in
a relatively stable state.
3.3. MCG refinements during in-situ SRX experiments with 8% and 6.5%
RRs
The microstructural evolutions of thermal etched samples with
compression of 8% and 6.5% RRs are then shown in in video 4 and 3,
respectively. Fig. 7 is a graphical illustration of the two videos.

Fig. 6. Graphical illustrations of video 1 and 2: (a) SRX incubations, (b) microstructures after air quenching and (c) all Euler maps (marked by original MCG GBs of samples
before SRX) of two air quenched samples obtained by EBSD measurements. White dash lines in Fig. 6c2 are the identified original MCG GBs. The sample with 25% RR: 1, The
sample with 10% RR: 2.

5
Y. Li, P. Shen, H. Zhang et al.
Fig. 7. Thermal etched microstructure evolution of samples with small deformation of (a) 8% RR and (b) 6.5% RR at the holding temperature of 1250 °C for 600 s. HT
represents the holding time. (a4) and (b4) are all Euler maps (marked by original MCG GBs of samples before SRX) of two air quenched samples obtained by EBSD
measurements. White dash lines in Fig. 7a4 and b4 are the identified original MCG GBs.
Under these small deformation conditions, many surface slip traces
appeared in the MCGs but not in surrounding FGs. As shown in
Fig. 7a2 and b2, new GBs began to appear in the sample with 8%
RR after it was kept at 1250 °C for 70 s, while in sample with
6.5% RR, new GBs appeared after 80 s at the same temperature.
One can that even under 8% RR deformation condition, the MCGs
were significantly refined, as shown in Fig. 7a3 and a4. This obser-
vation is valuable since many reports consistently showed that the
grain refinement of 316LN austenitic stainless steel by DRX
requires a large amount of strain [15,25]. Here, due to its large
grain size, the preferentially deformed MCGs were refined by SRX
method under a small deformation condition, thus providing a
simple and feasible method to refine the mixed-grain structure
in engineering. Additionally, many original MCG GBs were
remained as shown in Fig. 7a4 and b4.
It is noted that an MCG still existed in the sample under 6.5% RR
after heating, as shown in Fig. 7b3. This ‘new’ MCG is inside the
‘old’ MCG. This phenomenon prompted us to further compare the
EBSD measurements in this region before and after heating, and
the results are presented in Fig. 8. The ‘new’ MCG has the same
Euler angles as the ‘old’ MCG, i.e., (153, 37, 45 /deg), revealing that
this MCG is actually a portion of the original MCG and the original
MCG was partially refined. It indicates that the refinement of the
MCG is not significant under 6.5% RR. The incomplete refinement
can be interpreted by the difference in the amount of the deforma-
Fig. 8. Optical observations and all Euler angle maps obtained by EBSD measurements of the sample with 6.5% RR (a) before and (b) after SRX process.
6
Materials & Design 210 (2021) 110057
tion partitioning among MCGs. As shown in Fig. 8a2, white lines
represent the low-angle grain boundaries (LAGBs). Generally, the
LAGBs stands for the misorientation angle between 2 and 15 deg,
but for a clear display, the LAGBs shown by the EBSD result were
defined as misorientation between 3 and 10 deg. It can be seen that
the LAGBs among MCGs of the sample under 6.5% RR was unevenly
distributed before heating. Due to the close relationship between
the LAGBs and local deformation [26], the deformation partitioning
among MCGs was then identified inhomogeneous. It can be found
that the deformation partitioning of this incompletely refined MCG
was lower, which also means that less deformation energy storage
is available for SRX.
4. Discussion
4.1. Refining assessments of MCGs under different deformation
conditions
In this work, three indexes are used to evaluate the MCG refine-
ment in material with the mixed-grain structure: the average grain
size dm, the maximum grain size dmax and the grain size uneven
factor Z0. Note that to reduce the fluctuation of dmax among differ-
ent samples, its value is defined as an average of three MCGs with
largest grain sizes in the visual field. The average grain size dm is
Y. Li, P. Shen, H. Zhang et al.
determined by the linear intercept method [27]. The grain size
uneven factor Z0 is defined as the ratio of dmax to d0, where d0 is
the grain size with the highest occurrence rate, and its value is
determined by the EBSD measurements. The results of refining
assessments are presented in Fig. 9. Fig. 9 also presents the corre-
sponding reference for each index of the uniform FG sample which
is from a well-fined studied material. It can be seen that the
indexes dm and dmax all increase with the decrease of deformation,
revealing that the larger the deformation, the better the refinement
of the mixed-grain structure in SRX process. However, except for
the sample under 6.5% RR, the grain size uneven factors Z0 of other
samples have little difference, and they are all close to that of the
uniform FG material, indicating that the discussed deformation
conditions except 6.5% RR can effectively eliminate the mixed-
grain structure and improve the homogeneity of grain size of the
material. One can find that d0 does not decrease but increase a little
after the recrystallization process. Our previous work studied grain
growth behavior of 316LN steel, and it was concluded that the
grain size becomes coarser severely with the increase of tempera-
ture from 1150 to 1250 °C [15]. Therefore, it is speculated that the
increase of d0 is due to the grain growth because the heating tem-
perature is high enough (1250 °C) even the holding time is 10 min.
4.2. Relationships between dislocation distributions and SRX
mechanisms
Since the holding temperature of the SRX process is the same,
the different SRX behaviors as well as the different refining results
of the mixed-grain structures can be attributed to the dislocation
distributions under different deformation conditions. Fig. 10 shows
the TEM images inside the MCG. As shown in Fig. 10a, the typical
slip band morphology was observed in the sample with 6.5% RR.
Fig. 9. Refining assessments of MCGs under different deformation conditions as well as the corresponding reference for each index of the material with the uniform fine
grains (FGs): (a) dm, (b) dmax and (c) Z0. (d) The table lists the grain size with the highest occurrence rate d0 of each sample determined by the EBSD measurements.
7
Materials & Design 210 (2021) 110057
These slip bands are parallel to each other, indicating that MCGs
undertake the deformation in a primary slip pattern. Different from
the samples under larger deformation conditions, the sample with
6.5% RR presented only the slip band morphology without disloca-
tion tangle or even scattered dislocation lines. For the sample with
8% RR shown in Fig. 10b, an obvious slip band morphology was also
observed, and it is expectable to find that the slip bands are both
larger in number and width than those of the sample with 6.5%
RR. Moreover, scattered dislocation lines between the parallel slip
bands were observed in the sample under 8% RR. It indicates that
the increase of deformation not only leads to the increase of the
overall dislocation density, but also enriches the dislocation struc-
tures. For the sample under 10% RR shown in Fig. 10c, the number
and width of parallel slip bands became larger. Apart from the scat-
tered dislocation lines between parallel slip bands, the dislocation
tangles were also observed. Fig. 11 presents the TEM image in the
GB region of the sample with 10% RR. The selected-area electron
diffraction (SAED) spot patterns (see Fig. 11a and b) corresponding
to the regions in the circles in Fig. 11c reveal the different lattice
structures of the upper and the lower parts, confirming the exis-
tence of GB. One can find the striking dislocation pile-ups in the
MCG GB region. In addition, the slip band moving to the GB also
became the privileged site for dislocation pile-ups. For the sample
with 15% RR as shown in Fig. 10d, slip band tangles were observed,
indicating the activation of multiple slip systems. When the defor-
mation condition came to 25% RR, a new dislocation structure, i.e.,
dislocation cells, were distinctly observed as shown in Fig. 10e and
f. These cell structures with the size range of 0.5 lm to 1.4 lm are
formed based on the tangled slip bands. The phenomena, that only
parallel slip bands were observed in MCGs under small deforma-
tion conditions while slip band tangles and dislocation cells in
MCGs under large deformation conditions, may be connected with
Y. Li, P. Shen, H. Zhang et al.
Fig. 10. TEM images of MCGs in the deformed samples with (a) 6.5%, (b) 8%, (c) 10%, (d) 15% and (e, f) 25% RRs.
the nitrogen element. As presented in Table 1, the studied material
is 316LN austenitic stainless steel with 14 N (0.14 wt%). The addi-
tion of nitrogen is to enhance the creep resistance, corrosion resis-
tance, tensile strength, ductility and fatigue strength [3,4,28].
According to the work of Masumura et al. [29] and Ojima et al.
[30], the nitrogen also plays an important role in dislocation
behavior. Dislocations are aligned on the same slip plane, because
cross slipping is remarkably suppressed, especially at low strains. It
explains why the slip band tangles and the formation of dislocation
cells were delayed to higher strains.
The dislocation distributions and various structures can con-
tribute to discuss the SRX mechanisms of samples under different
deformation conditions. As shown in Fig. 12, the SRX mechanism
with a limited deformation condition can be described as follows.
The plastic deformation partitioning in the MCG mixed-grain
structure is dominated by grain size. At the early deformation
stage, due to its abnormally large grain size, the MCGs in the
mixed-grain structures are more inclined to deform than the sur-
rounding fine grains. The MCG undertakes the plastic deformation
in a primary slip pattern, leading to the formation of parallel slip
bands. Due to the absence of slip band tangles, these parallel slip
Fig. 11. (a, b) SAED spot patterns corresponding to the region in the circles in (c). (c) TEM image in the GB region of the sample with 10% RR.
8
Materials & Design 210 (2021) 110057
bands easily move to the MCG GBs, contributing to dislocation
pile-ups at GBs. Although the dislocation density at the local GBs
has met the nucleation condition for SRX under a small deforma-
tion condition (e.g., 6.5% RR), the number of recrystallization nucle-
ation at MCG GBs is limited, and the driving force for the growth of
nucleated grains is insufficient, which leads to the partial refine-
ment of MCG, i.e., the incomplete SRX during heating process.
As deformation progresses, the MCG continues to undertake the
main deformation, and the dislocation density at MCG GBs
increases gradually. Under a suitable small deformation condition
(e.g., 8% RR or 10% RR), the dislocation density at MCG GBs satisfies
the entire refinement condition for MCG. At this case (see video 2),
the number of the recrystallization nucleation at MCG GBs and the
driving force for the grain growth are adequate. The nucleated
grains grow up through GB bulging, and the SRX is basically com-
pleted when the GB bulging is in a collision with the other. The GBs
will migrate locally during heating process. And eventually a stable
fine microstructure is formed.
Under a relatively large deformation condition, the MCG under-
takes the plastic deformation in a multi-slip pattern. Apart from
the increase of the dislocation density at MCG GBs, a new disloca-
Y. Li, P. Shen, H. Zhang et al.
Fig. 12. Schematic of the fragment and refinement of the MCG in mixed-grain structures based on the relationships between dislocation distributions and SRX mechanisms.
tion structure, i.e., the dislocation cell-structure, is formed in the
interior of the MCG. These dislocation cells based on the slip band
tangles or dislocation walls [31], are excellent sites for recrystal-
lization nucleation [32,33]. Both the nucleated grains at MCG GBs
and the intragranular-nucleated grains grow up in the manner of
GB bulging, leading to a better refinement of MCG. It should be
noted that although we use a description of a relatively large defor-
mation condition, the compression deformation, however, is only
25% RR. Many studies have reported that the deformation condi-
tion of the DRX incubation for austenitic stainless steels is in the
true strain range of 15% to 20% (i.e., 14% to 18% RR of compression
deformation) or even higher [25,34]. Therefore, the advantage to
refine the mixed-grain structure with MCGs using the two-stage
method is emphasized here. More importantly, the refinement pro-
cess based on the limited deformation condition is easier to be
applied in engineering.
5. Conclusions
A two-stage grain refinement method, i.e., a limited cold defor-
mation followed by rapidly heating process, was applied to refine
the mixed-grain structure emerged in the nuclear grade 316LN
austenitic stainless steel. The SRX behaviors of samples under dif-
ferent cold deformation conditions were studied by in-situ obser-
vation technique. The conclusions can be summarized as follows:
(1) The MCGs in the mixed-grain structure were preferentially
deformed than fine grains even if MCGs are with hard orientations,
i.e., the grain size plays a more significant role in strain partitioning
than the crystallographic orientation. Since the MCGs preferen-
tially and continuously undertook the main deformation, the accu-
mulated dislocation density in MCGs can meet the deformation
energy requirement of the SRX process at a limited deformation
condition. It was proved that the compression with only 8% reduc-
tion rate followed by rapidly heating process (1250 °C  360 s) can
completely refine the MCGs in the mixed-grain structure.
(2) Under a small deformation condition, the observed parallel
slip bands inside MCGs indicates that the MCGs undertook the
plastic deformation in a primary slip pattern. The slip bands easily
moved to the MCG GBs due to the lack of slip band tangles, leading
to the striking dislocation pile-ups at GBs. Therefore, the nucle-
ation of SRX preferentially occurred at the MCG GBs, and the nucle-
ated grains grew up in the manner of GB bulging, finally leading to
the refinement of MCGs.
9
Materials & Design 210 (2021) 110057
(3) Under a relatively large deformation condition, slip band
tangles were observed inside MCGs, indicating that the MCGs
undertook the deformation in a multi-slip pattern. The tangled slip
bands in MCGs contributed to the formation of intragranular dislo-
cation cells. Therefore, the nucleation of SRX occurred both at the
MCG GBs and in the interior of MCGs, and the nucleated grain also
grew up in the manner of GB bulging. The MCGs were refined as
well at this deformation condition.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
The authors gratefully acknowledge the funding support from
the National Natural Science Foundation of China with the project
of Nos. 51675335 and 52075329, as well as the support from
Shanghai Rising-Star Program (20QA1405300).
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.matdes.2021.110057.
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