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Keywords: Simultaneous strength–ductility enhancement of a high-entropy alloy via cold rolling and annealing is difficult.
High entropy alloy Cold rolling and annealing were performed on an as-cast Fe35Co21Ni6Cr18Mn20 high entropy alloy (HEA), the
Strength-ductility trade-off microstructure showed single phase face centered cubic (fcc) solid solution without phase transformation and the
Cold rolling
grains were fully recrystallized accompanied by additional grain growth. The grain size decreased significantly
Annealing twins
Tension
from 179.4 ± 15.3 μm to 15.2 ± 1.4 μm. A large number of annealing twins and twin boundaries (TBs) (fraction
up to 44.2%) were observed. The dislocation slip and twinning were observed as the dominant plastic defor
mation mechanism. Meanwhile, dislocations plugging was also seen near the twin boundaries. Tensile tests
revealed for the first time that the rolling-annealing HEA overcame the strength-ductility trade-off because the
yield strength dramatically increased from 516.7 ± 3.4 MPa to 725.4 ± 4.7 MPa and ductility retained excellent
(from 0.51 ± 0.01 to 0.53 ± 0.01) as compared with as-cast HEA, this behavior was attributed to the grain
refinement and substantial annealing twins including transgranular annealing twins and suspened annealing
twins.
* Corresponding author. School of Mechanical and Aerospace Engineering, Jilin University, Changchun, 130025, China.
E-mail addresses: zw199617@163.com (W. Zhang), zcma@jlu.edu.cn (Z. Ma), hwzhao@jlu.edu.cn (H. Zhao), lqren@jlu.edu.cn (L. Ren).
https://doi.org/10.1016/j.msea.2020.140264
Received 25 June 2020; Received in revised form 28 August 2020; Accepted 8 September 2020
Available online 21 September 2020
0921-5093/© 2020 Elsevier B.V. All rights reserved.
W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
of recrystallized grains [26]. Focus on studying the texture evolution of intercept method was used to calculate the grain size. Prior to EBSD
cold-rolled Fe34.95Ni27.5Co17.5Al11.5Cr8.5B0.05 HEA at annealing tem analyses, samples were argon-ion polished using Leica EM RES 102 with
peratures 1200 ◦ C and 1300 ◦ C, respectively. Experimental results cutting rate of 150 μm/h. The microstructure of the tensile-deformed
revealed that the enhanced ductility but inevitably reduced strength of alloys and the corresponding representative twin orientation relation
cold-rolled HEA after annealing at 1300 ◦ C in comparison to 1200 ◦ C, ship was observed with JEOL 2100F transmission electron microscope
this behavior was attributed to the weaker grain restraint determined by (TEM) and selected area electron diffraction pattern (SEAD), respec
larger grain size and stronger texture [27,28]. Our previous study on the tively. TEM samples were prepared by mechanical polishing followed by
as-cast single-phase fcc Fe24Co23Ni24Cr23Ti2Al4 HEA [29] indicated that ion milling. Surface scans of energy spectrum were performed in TEM
the cold-rolled and annealed HEA present higher strength but slightly equipped with energy dispersive X-ray spectroscopy (EDS) to obtain the
lower ductility due to the new precipitations of bcc phase. Rolling at low distribution of elements.
temperature followed by annealing under liquid nitrogen was performed
on Al0.1CoCrFeNi HEA with low stacking fault energy revealed that the 3. Results and discussions
tensile ductility could be further enhanced by increasing the annealing
time but the strength was sacrificed [30]. Joint combination of high 3.1. Microstructures
strength and ductility is hard to obtain [31,32]. The nano-lamellar
AlCoCrFeNi2.1 HEA was subjected to cryo-rolling and annealing, Fig. 1 presents the XRD patterns and corresponding full width at half
resulting in obvious increase in strength without sacrificing the ductility maximum diagrams (FWHMs) of Fe35Co21Ni6Cr18Mn20 HEA in the as-
[31]. Although the ductility of rolling-annealing HEA was increased as cast and rolling-annealing condition. The result in Fig. 1a shows that
compared with as-cast HEA, the ultimate elongation (~14%) was still both the as-cast and rolling-annealing HEAs with only fcc peaks,
low to a certain extent. revealing that the addition of cold rolling and annealing has not changed
Fe35Co21Ni6Cr18Mn20 HEA was selected in this study because the single-phase fcc structure of as-cast HEA. The lattice parameter was
Co–Cr–Fe–Mn–Ni system HEA exhibited excellent mechanical properties reduced from 3.588 ± 0.008 nm to 3.571 ± 0.005 nm according to the
including strength and strain hardening capacity, especially at liquid XRD results, this phenomenon can be associated with the solid solution
nitrogen temperature [33-34]. The equi-atomic FeMnNiCoCr exhibited strengthening due to the lattice distortion inside the alloys. After rolling
higher strain hardening levels due to twin interactions, as reported in
recent publications [35-36]. This work examined the microstructures
and mechanical properties on cold rolling-annealing Fe35Co21
Ni6Cr18Mn20 HEA to obtain the HEA with both high strength and
toughness. The results indicated that the combination of fine grain
strengthening induced by the reduced grain size and the twinning
strengthening caused by the interaction between annealing twins and
dislocations improved the strength of HEA, and the plastic deformation
ability of HEA can be enhanced by the presence of twins through acti
vating the slip system in unfavorable orientations.
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W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
and annealing, the intensity of the (200) peak decreased while that of Fig. 2 a-f illustrates the microstructure evolution of the as-cast and
the (220) and (111) peak increased. The intensity of X-ray diffraction on rolling-annealing Fe35Co21Ni6Cr18Mn20 HEA by EBSD analyses. The as-
some specific crystal planes was reduced when grains were broken under cast and rolling-annealing HEA are shown in left and right column,
strong stress during rolling, which resulted in weakening relative atomic respectively. Following 45% thickness reduction cold rolling and sub
planes peaks intensity. Despite the intensities of (220) and (111) peak sequent annealing at 1000 ◦ C for 2 h, the alloy exhibited microstructures
were slightly increased owing to the appearance of the textures in spe with full recrystallization and partial grown grains, and annealing twins
cific direction during plastic deformation, but the intensities were still (marked by arrows) with two kinds of varying characters were also
low in comparison with (200) peak. It is also demonstrated by IF images frequently observed as shown in Fig. 2b. Transgranular annealing twins
in Fig. 3b, which exhibited no strong recrystallization texture but mul were consisted of coherent twin boundaries on both sides and grain
tiple textures. Furthermore, the half-peak width of the rolling-annealing boundaries on both ends, which could penetrate matrix grain and be
HEA significantly increased compared to as-cast HEA in Fig. 1b, this viewed as unbroken annealing twins. Compared to the transgranular
behavior was related to the grain refinement. annealing twins, the other kind of annealing twin possessed non-
Fig. 2. (a–b) EBSD-band contrast images of the as-cast and rolling-annealing HEA specimens. (c–d) GB images from the EBSD scan of the as-cast and rolling-
annealing HEA specimens. (e–f) are IPF images of the as-cast and rolling-annealing HEA specimens, respectively. (g) and (h) are the distributions of the grain
size and GB misorientation angle of the rolling-annealing HEA specimens, respectively.
3
W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
Fig. 3. (a) EDS images show homogeneous distributions of Fe, Ni, Cr, Mn, and Co elements in the rolling-annealing HEA. (b) IF images of the as-cast (left) and rolling-
annealing (right) HEA specimens.
coherent twin boundaries that terminated at one end in the grains, thus to rolling and annealing, this behavior was in agreement with pole fig
calling it suspended annealing twins [38]. One end of the suspended ures (PF) as shown in Fig. 3b. A large portion of orientations were
annealing twins would grow outwards and become transgranular distributed around 60◦ as summarized in Fig. 2h, indicating that a high
annealing twins during annealing due to the high energy and instability density of annealing twins occurred during recrystallization and grain
of the non-coherent twin boundaries. Fig. 2c and d shows the grain growth due to twins were formed by rotating 60◦ along the {111} plane
boundary maps of the as-cast and rolling-annealing specimens, respec normal in fcc metals [41]. The as-cast specimens with smaller grain size
tively. The blue, green, and black lines are related to high-angle grain are more inclined to form annealing twins during annealing, resulting in
boundaries (HAGBs) with orientation difference greater than 15 ◦ C, the rolling-annealing HEA with a large number of annealing twins in this
low-angle grain boundaries (LAGBs) with orientation difference ranging study [42]. The annealing twins cut the original grains into smaller
from 2 ◦ C to 15 ◦ C and TBs, respectively [39]. The grain boundary type grains, resulting in grain refinement and the grain size were significantly
of as-cast specimen was dominated by HAGBs with a small number of reduced from 179.4 ± 15.3 μm to 15.2 ± 1.4 μm, the grain size distri
LAGBs while a high fraction (approximately 0.442) of TBs appeared in bution is shown in Fig. 2g. Also, the size and thickness of the twins
the rolling-annealing HEA. The TBs cut off the original continuous slip increased with the size of the matrix grains, this property has also been
systems, so that increasing the difficulty of dislocation movement due to demonstrated in other report [43].
the dislocations need to constantly change the slip system and thereby The EDS images (Fig. 3a) obtained from the region marked by red
increasing the strength of the HEA [40]. In EBSD inverse pole figure rectangle in Fig. 2b shows that all elements (Fe, Co, Ni, Cr, Mn) are
(IPF) images (Fig. 2e and f), similar crystal orientations among adjacent uniformly distributed, which demonstrates significant homogeneity of
grains were observed in the as-cast HEA, but noticeable change in the composition in rolling-annealing HEA. S.J. Sun et al. have suggested that
rolling-annealing HEA was the random orientation of grains, confirming the strength and hardness can be significantly improved when the
that no strong recrystallization texture appeared in the specimen subject element particles are small and uniformly distributed [41]. The
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W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
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W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
Fig. 4. (a) shows microstructure image of rolling-annealing HEA after tensile test in TEM. (b) is an enlarged view of a representative annealing twin, the inserted
electron diffraction (SAED) pattern reveals the twin orientation relationship. (c) and (d) are annealing twins with different thicknesses.
Fig. 5. A schematic of deformation mechanisms in rolling-annealing HEA with the increasing strain.
h. The rolling-annealing HEA was characterized by a single fcc solid weakened and all alloying elements were evenly distributed without
solution and exhibited fully recrystallized microstructure accompanied obvious enrichment. The grain size largely reduced from 179.4 ± 15.3
by a few grown grains. The grain boundary type changed from pre μm to 15.2 ± 1.4 μm, the refinement enabled an increase in the area
dominant HAGBs to a combination of HAGBs and TBs (up to 44.2%). The fraction of grain boundaries and then improved the resistance to the
types of texture increased notwithstanding the strength of texture plastic deformation, resulting in a higher strength of rolling-annealing
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W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
Fig. 6. Mechanical behavior of the as-cast and rolling-annealing HEA specimens. (a) Tension engineering stress-strain curves and (b) strain hardening curves with
respect to true strain, the inserted image is the corresponding true stress-true strain curves.
HEA. Annealing twins including transgranular annealing twins and fracture from 0.51 ± 0.01 to 0.53 ± 0.01, respectively. It is noteworthy
suspended annealing twins with different thicknesses formed during the that the ductility of HEA in rolling-annealing condition remained su
recrystallization annealing. The formation of annealing twins simulta perior. Meanwhile, the work hardening rate of rolling-annealing HEA
neously benefits strength and ductility of the HEA. On the one hand, the was at a higher level as compared to the as-cast HEA. The quantitative
interaction between twins and dislocations could enhance the strength analysis on the microstructure suggested that the fine grain strength
and work hardening rate of the material. On the other hand, the pres ening and twinning strengthening were two major contributions for
ence of twins could change the crystal orientation to activate further slip overcoming the strength-ductility trade-off in the rolling-annealing
deformation and thereby leads to a higher ductility. The rolling- HEA.
annealing HEA showed a substantial enhancement of tensile strength
from 516.7 ± 3.4 MPa to 725.4 ± 4.7 MPa and total elongation after
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W. Zhang et al. Materials Science & Engineering A 800 (2021) 140264
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