REPORTS

Cite as: Q. Pan et al., Science

10.1126/science.abj8114 (2021).

Gradient-cell–structured high-entropy alloy with

exceptional strength and ductility
Qingsong Pan1†, Liangxue Zhang1,2†, Rui Feng3†, Qiuhong Lu1, Ke An3, Andrew Chihpin Chuang4, Jonathan D.
Poplawsky5, Peter K. Liaw6, Lei Lu1*
1Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang, 110016, P.R. China. 2School of Materials Science
and Engineering, University of Science and Technology of China, Shenyang, 110016, P.R. China. 3Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, TN
37831, USA. 4Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439, USA. 5Center for Nanophases Materials Sciences, Oak Ridge National Laboratory,
Oak Ridge, TN 37831, USA. 6Department of Materials Science and Engineering, The University of Tennessee, Knoxville, TN 37996, USA.
†These authors contributed equally to this work.
*Corresponding author. Email: llu@imr.ac.cn

Most multicomponent high-entropy alloys (HEAs) lose ductility with increasing strength, similar to
conventional materials. We controllably introduced novel gradient nano-scaled dislocation-cell structures in
one stable single-phase face-centered-cubic HEA, which result in enhanced strength without apparently
losing ductility. The sample-level structural-gradient induces the progressive formation of a high density of

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tiny stacking-faults (SFs) and twins upon early straining, nucleating from abundant low-angle dislocation
cells. Furthermore, the SF-induced plasticity and the resultant refined structures, coupled with intensively
accumulated dislocations, contribute to the plasticity, extra strengthening and work hardening. Our
findings offer a promising paradigm for tailoring properties with gradient-dislocation cells at the nanoscale
and advance our fundamental understanding of the intrinsic deformation behavior of HEAs.

High-entropy alloys (HEAs), or multi-principal-element al-
loys, have a near-infinite multicomponent phase space that
can lead to interesting mechanical properties (1, 2). Good
strength and ductility, high work hardening, and exceptional
damage tolerance have been achieved in some single-phase
HEAs that have inherent concentration inhomogeneity cre-
ated by tailoring their chemical complexity (3–6). Moreover,
engineering a spatial heterogeneous microstructure consist-
ing of graded grain sizes, nanoclusters, multi-phases, etc.
could also allow HEAs to achieve superior properties (7–9),
similar to that having been achieved in traditional hetero-
structured metallic materials (10–12). However, the long-
lasting strength-ductility paradox for conventional metallic
materials still exists for most HEAs (7, 8, 13).
The tradeoff between strength and ductility for HEAs
exists because the fundamental plastic-deformation features
and mechanisms of HEAs reported so far are similar to
those of conventional metals (13, 14). Elementary line defects
that carry plasticity, i.e., full dislocations and related interac-
tions with different structural defects, such as high-angle
grain boundaries (HAGBs) or twin boundaries (TBs), are
well understood in traditional metals (15–18). Interestingly,
some unusual dislocation behaviors have been identified
in HEAs with highly concentrated solid solutions due to
local inhomogeneity with chemical short-range order (SRO)
and spatially variable stacking fault energy (SFE) at the
atomic scale (14). For example, the changing dislocations
slip modes (6, 14, 19–21), as well as the enhanced friction
resistance to motion/accumulation of dislocations (5, 22, 23),
enabled by increasing local concentration fluctuations
or local SRO at the nanoscale (generally <3 nm) (5, 6, 24),
are believed to contribute to the improved mechanical prop-
erties.
We propose a heterogeneous gradient dislocation-cell
structure (GDS) in a stable single face-centered-cubic (fcc)
phase Al0.1CoCrFeNi HEA containing randomly-oriented,
equiaxed fine grains (FG) with an average size of ~46 μm.
This alloy is a well-studied model material with a locally-
varied SFE of 6 - 21 mJ/m2 (25). We found an unexpected and
extremely high density of tiny stacking fault (SF), twin nucle-
ation and accumulation-dominated plastic deformation in
our GDS HEA upon early tensile straining. This feature re-
sulted in attractive strength and ductility properties, com-
pared to other HEAs (10, 26, 27).
We processed HEA dog-bone-shaped bar specimens with
a gauge diameter of 4.5 mm and a gauge length of 12 mm,
using a cyclic-torsion (CT) treatment without any surface
tooling to form a sample-level multi-scaled hierarchical dis-
location structure under the imposed spatially-gradient plas-
tic strains from the surface to the core (28) (fig. S1). By
controllably tuning CT parameters, i.e., torsion-angle ampli-
tudes of 20 and 6 degrees, we prepared two different GDS
samples with a constant torsion number of 200 cycles, respec-
tively. We refer to these samples as GDS-H (Fig. 1, 20 degrees)

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and GDS-L (fig. S2, 6 degrees), based on the high and low
accumulated torsion plastic strains imposed (i.e., 18.4 and 5.2
in the topmost layer, fig. S1E, respectively).
We focus on the GDS-H sample to illustrate the salient
microstructural feature of a sample-level hierarchical dislo-
cation structure. Grains from the surface to the core of the
GDS-H sample are still homogeneously distributed, with
characters of faceted grain morphologies, unchanged grain
size, and random crystallographic orientations (Fig. 1, A and
G), using electron backscatter diffraction (EBSD) with scan-
ning electron microscopy (SEM). The same observations were
made before CT (fig. S1C). The noticeably unchanged grain
features after CT processing is in sharp contrast to traditional
homogeneous or gradient nanostructures with severely-re-
fined grain sizes and higher densities of HAGBs that are pro-
duced by employing conventional severe plastic deformation
strategies (29, 30). Most grains in the sample core have the
typical planar single-slip dislocation configuration in a rela-
tively-low dislocation density (fig. S3C), like that reported
in the same HEA after tension strain (25). Well-developed
single-slip-induced dislocation walls with low-angle bounda-
ries (LABs) are occasionally observed in several grains (Fig.
1H and fig. S3D). Distinctly, massive LABs with misorienta-
tions <15° were introduced in the topmost grain interior and
spatially distributed such that they become smaller in the vol-
ume fraction and larger in size with increasing the depth
from the top surface (Fig. 1B, also schematically illustrated in
Fig. 1C).
We randomly select one grain separated by HAGBs in the
topmost layer (~100 μm from the surface) of the GDS-H sam-
ple and investigate its dislocation structure using transmis-
sion electron microscopy (TEM). We show in Fig. 1D an
example of the numerous equiaxed dislocation cells and cell
walls with a small misorientation ranging from 0.7 to 4.8°,
corresponding to massive LABs in Fig. 1B. We observed a mis-
orientation gradient in the grain interior along the radial di-
rection (white arrow, Fig. 1D), as a result of the imposed
macro-level plastic-strain gradient upon the CT treatment
(Fig. 1F) (31). We measure the cell diameter to be ~200 nm in
the top surface, which gradually increases to ~450 nm for the
dislocation-wall structure in the core (fig. S3). Each cell wall
(~40 nm thickness on average) is decorated with a high den-
sity of dislocations (~1.7 × 1015 m−2) (28), but relatively-fewer
dislocations with curved morphologies in the cell interior
(Fig. 1E and fig. S3). We achieved a similar dislocation struc-
ture in the GDS-L sample at a small cumulative plastic strain,
exhibiting undeveloped dislocation cells with a larger average
size of ~450 nm in the topmost surface (figs. S1 and S2). The
dislocation cells in the GDS HEA sample are primarily caused
by intensive multi-slip full dislocation interactions under a
complex gradient stress/strain state (32) after a large cumu-
lative torsion strain (fig. S1). We observed no visible SFs or
First release: 23 September 2021 science.org
deformation twins in the bulk GDS sample (Fig. 1 and figs. S2
and S3), indicating the dislocation-controlled plastic defor-
mation during the CT process, analogous to that observed in
numerous HEAs with low SFEs (13, 25, 33, 34).
Synchrotron X-ray diffraction (SXRD) scanning on the as-
prepared GDS-H samples from the topmost surface to the
core showed a spatially-gradient-distributed dislocation den-
sity, i.e., up to 8.8 × 1014 m−2 in the topmost ~200 μm-depth
layer (fig. S4). The GDS-H sample still exhibits a stable single
fcc phase, as evidenced by EBSD, TEM, and SXRD/neutron
results (Fig. 1 and figs. S5 and S8). Quantitative compositional
analysis at the atomic scale shows that the GDS structure is
compositionally homogeneous without detectable elemental
segregation at the cell wall, employing three-dimensional
atom probe tomography (3D-APT) (fig. S6).
The hierarchical dislocation-cell structure results in re-
markably improved tensile properties (Fig. 2A). Tensile tests
of both GDS samples show the higher yield strength (σy, at
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0.2% offset) of 362 ± 2 and 539 ± 26 MPa, about 2-3 times
stronger than those of the FG and coarse-grained (CG) coun-
terparts (185 ± 5 MPa and 138 ± 3 MPa, respectively) (25). In
addition, we measured a high uniform elongation (δu) up to
42.6 ± 0.2% for GDS-H, slightly reduced, relative to FG coun-
terparts without GDS (55.4 ± 3.4%). This behavior differs
from the strength gain at the expense of the ductility in
most conventional metals and HEAs (7, 10). Specially, the
GDS-H sample shows steady strain hardening with a slightly-
decreased work-hardening rate, Θ, i.e., from 1.28 GPa at a 3%
strain to 0.99 GPa before necking, distinct from the notably
reduced Θ trend upon straining in its FG counterpart and the
concave Θ shape of CG counterpart (Fig. 2B) dominated by
deformation twinning (35).
The GDS structure that we introduced leads to an unex-
pected deformation-induced continuous hardening behavior
that we found by measuring the microhardness (Hv) along
the depth from the surface to the cores of GDS and FG
samples before and after tension (Fig. 2C). Owing to the pres-
ence of the sample-level gradient dislocation architecture in
the whole cross-section, we identified a distinct, gradiently-
distributed Hv from 3.7 GPa at the topmost surface to 2.2
GPa in the central region in GDS-H. These values are much
higher than that of GDS-L (from 2.3 to 1.7 GPa). Compared to
the uniform increase in Hv for the FG sample after tensile
straining, we found remarkably continuous hardening in
both tensioned GDS samples from the top surface to the
core. This hardening feature is quite different from the
deformation-induced continuous softening in conventional
metals with gradient nanograins (10, 36).
We attributed the pronounced increase in yield strengths
to the nanoscaled dislocation-cell unit with LABs (Fig. 1).
Specifically, the contribution of LABs to strength has been
demonstrated to be comparable with that of conventional
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HAGBs, and an ultrahigh hardness was observed in a nano-
laminated Ni with LABs (18, 37). For the topmost GDS surface
layer of the GDS-H sample, ultra-high Hv that we measured
indicates that the massive low-angle dislocation cells are ef-
fective in resisting dislocation motion. This trend results
from their structural features, including a nano-scaled size
and high density of dislocations. We argue that this feature,
together with the obvious continuous hardening in the top-
most GDS surface and the unusual work-hardening response
of the whole GDS samples, indicates an extra-strengthening
and ductilizing mechanism in gradient dislocation structures
upon straining.
We further characterized the microstructural evolution at
the top surface of GDS-H at different strains of 3% (the onset
stage of a steady work hardening) and 40% (the later stage of
plasticity) to unravel the intrinsic deformation mechanism of
the gradient dislocation-cell-structured HEA. At a strain of
3%, we found almost no detectable changes to the grain-level
characteristics, including the grain shape, grain size, and ori-
entation (Fig. 3, A and H). However, the density of LABs in
the subsurface layer and the core were notably reduced. The
presence of these dislocation patterns is because they are in
a poorly-developed or unstable state at relatively-small cumu-
lative plastic strains (38, 39), while the pattern remains al-
most unchanged for the topmost grains (Fig. 3, B and I).
Specifically, a widespread class of long parallel lamellae bun-
dles, with an average spacing of ~1.7 μm, were detected in the
majority of the topmost grain, which decreases in the number
density with increasing the depth (Fig. 3, C and D, and fig.
S7). The main components of these lamellae bundles are SFs,
with a few TBs, which we observed in the selected area elec-
tron diffraction (SAED) (Fig. 3E) and high-resolution TEM
image (Fig. 3F). We detected most parallel SFs and TBs (i.e.,
the dashed lines) across a dislocation wall (i.e., a white con-
trast region). Close-up atomistic-resolution TEM views show
that each individual long lamellae interface is essentially
composed of numerous nanoscaled SFs or twin segments,
several to tens of nanometers in length (Fig. 3G). Measure-
ments of the thickness between adjacent SFs or TBs show an
extremely-smaller value, i.e., 2.9 nm on average, correspond-
ing to a super high volume density (~4.14 × 108 m2/m3) in the
bundle. Moreover, the dislocation cells remain almost un-
changed in shape and size. By contrast, the plastic defor-
mation of most grains in the core of GDS-H is still dominated
by intensive parallel full dislocations along {111} primarily
slip planes (Fig. 3, J and K).
With the tensile strain increased to 40% before necking,
the density of planar SF interfaces increases in volume frac-
tion, prevailing in the grain interior (Fig. 4, A and B). Besides,
more numbers of ultrafine nanotwins are also detected (Fig.
4C). The average spacing between adjacent SFs or TBs that
we measured is small, about 4.4 nm (Fig. 4C). The generation
First release: 23 September 2021 science.org
of both SFs and deformation twins, according to conventional
wisdom, are associated with the emission and slip of partial
dislocations from GBs (16), in this case most likely from
dislocations-cell walls instead. Besides, numerous short SFs
along the other inclined {111} slip plane are widely detected
in between neighboring SF/TBs, thereby forming a unique
3-dimensional SF-twin structure network (Fig. 4C).
We conducted in-situ neutron-diffraction tensile experi-
ments to confirm that the formation of SFs with detectable
splitting of (111) and (222) planes happens at a very small
tensile strain of ~5% for GDS-H samples, while setting in
at a large strain of ~30% for the FG counterpart (Fig. 4D).
Our analysis of the neutron-diffraction results yields for the
GDS-H sample a higher value of the SF probability, compared
to that of the FG counterpart upon straining (Fig. 4E), which
is the evidence of the easier formation of SFs at an early de-
formation stage in GDS samples. Ex-situ SXRD measure-
ments further reveal that the enhanced probability of SFs and
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twins primarily stems from the contribution of GDS (fig. S8),
consistent with our ex-situ SEM and TEM observations (Figs.
3 and 4). By contrast, both SFs and deformation twins are
rarely observed in FG and at the core of GDS samples even at
a 40% strain, as confirmed by results in fig. S9, and in agree-
ment with that reported in numerous single fcc phase HEAs
deformed at ambient temperature (4, 9, 13, 40–42).
Based on the above results, we rationalize that the
extremely-high density of SFs and TBs-mediated plastic de-
formation are primarily responsible for the superior mechan-
ical properties of the gradient dislocation-cell-structured
HEA. For the dominance of such dense SFs and TBs, which
are not achievable in conventional metallic materials or most
single fcc phase HEAs in the early deformation stage at am-
bient temperature (8, 13, 25, 42), we mainly attributed it to
the chemical features of the HEA, nanoscaled dislocation
cells with LABs, and their spatial gradient distribution.
Plastic deformation of conventional polycrystalline fcc
metals is known to be mainly carried by the full dislocation
slip and their intensive interactions within individual grains
(16). Besides, as traditionally-alternative promising ductiliz-
ing strategies of high-strength metals and alloys, twinning or
phase transformation usually come into play, mostly through
either tuning compositions to reduce the SFEs or lowering
the deformation temperature (16, 43). Under such circum-
stances, deformation twinning or phase transformation be-
comes prevalent, primarily owing to the ready partial
dislocation glide on consecutive (or every other) {111} atomic
planes in fcc metals (16, 43). By contrast, for most single-
phase fcc HEAs (3, 13, 44), neither twinning nor phase trans-
formation dominates. Instead, the planar full dislocations
usually dominate the plastic deformation, as detected in FG
(fig. S9) and the core of the GDS (Fig. 3K) after tension. Spe-
cially, the SF-dissociation distance of full dislocations in the
(Page numbers not final at time of first release) 3
deformed HEA is wider than that in conventional metals,
which can be as large as 34 nm under tension tests at room
temperature for the same HEA in the literature (25). We ar-
gue that the larger probability for partial dislocations and SFs
nucleation, rather than twinning or phase transformation, is
closely related to the intrinsically-spatially variable, low SFE
associated with the saliently-rugged local atomic environ-
ments (14, 22, 23, 25) and chemical SRO (5, 6, 24), inherent to
HEAs, although we do not have the direct evidence. The SF is
a planar defect whose energy is relative to the lattice energy
level where it forms. In particular, the increase in the lattice-
distortion energy induced by high-density dislocations in the
GDS can more readily adjust the local atomic positions to fur-
ther decrease the SFE (45), making the SF width between par-
tial dislocations potentially larger.
In addition to the atomic-scaled compositional effect, the
activity of the dislocations-dominated plastic deformation
usually exhibits a strong (grain or cell) size dependence (46).
With decreasing the characteristic size (d), the full disloca-
tion activity is gradually inhibited, whereas the partial dislo-
cation activity becomes more favorable. In terms of the
classical Orowan relation (15, 47), the critical stress required
for initiating the full dislocation (τF) and partial dislocation
(τP) as a function of the cell size, d, can be expressed as:
2αµb
τF ( d ) =τ0 + (1)
d
γ 2αµbp
τP ( d ) = + (2)
bp d for nucleating partial dislocations. Both large numbers and
where τ0 and γ are the lattice-friction stress (57 MPa) and SFE
(6 - 21 mJ/m2) (25); α is a parameter that reflects the charac-
teristic of dislocations (0.5 for an edge dislocation and 1.5 for
a screw dislocation); μ is the shear modulus (80 GPa); b and
bp are the Burgers vectors of full and partial dislocations
(0.253 and 0.146 nm), respectively (28). Using a maximum
SFE of 21 mJ/m2 and α = 1, i.e., roughly assuming the disloca-
tions in cell interiors have curved morphologies (Fig. 1D and
fig. S2) belonging to a mixed type, the estimated critical size
for the transition from a full to a partial dislocation activity
is ~140 nm (fig. S10), which tends to become larger with de-
creasing SFEs, evidently being comparable with the cell size
in the topmost GDS layer (Fig. 1 and fig. S3). In essence, both
the chemical and nanoscaled cell structural characters render
the high favorability of partial dislocations over full disloca-
tions at ambient temperature (Fig. 3, F and G).
The sample-level gradient structure with length scales
spanning 6 orders of magnitude from the millimeter to na-
noscaled [i.e., compositional fluctuation inhomogeneity or
SRO, like those reported in the similar Al-Co-Cr-Fe-Ni sys-
tems (5, 48)] plays a pivotal role in enabling the activation of
partial dislocations in our alloy. First of all, the built-in gra-
dient distribution of dislocation cells causes the progressive
First release: 23 September 2021 science.org
plastic deformation from the core to the topmost surface (fig.
S11), effectively suppressing the overall strain localization. All
nanoscaled dislocation cells jointly mediate plastic defor-
mation, providing the spatial playground for activating par-
tial dislocations and the resultant formation of SFs to
undergo plastic deformation. Secondly, the gradient plastic
deformation in the multiscaled architecture is accompanied
by a complex stress/strain state with the sample-level stress
partition and the presence of the back stress, especially at the
early stage of plastic deformation (32). As we expected, by
conducting tensile load-unload-reload tests, we determined
the back stress of the GDS-H sample at a strain of 0.6% (close
to 0.2% offset) to be as high as 260 MPa, approximately 50%
of the yield strength, much higher than that of the FG coun-
terpart. Consequently, such obvious extra strengthening orig-
inates from the back-stress hardening associated with the
gradient plastic deformation of GDS, effectively contributing
to a higher yield strength than that of the FG counterpart.
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Microscopically, the nanoscaled cells with a higher disloca-
tion density at the walls tend to induce a stronger local stress
field (than the measured sample-scaled macro-back stress),
coupled with that caused by the local atomic distortions, en-
dowing the internal driving force for partial dislocations slip-
ping away from the equilibrium separation (13, 38), with
dense SFs stably left behind, as we show in Figs. 3, E to G,
and 4.
Moreover, the ultrahigh density of dislocations at the cell
boundaries naturally serves as abundant sustainable sources
orientation-independence feature of numerous topmost
grains containing SFs (fig. S7) indicate that the nucleation of
SFs is not solely determined by the axial tensile stress state,
but mostly controlled by complex multiaxial stress states in
GDS upon straining.
Taken together, through engineering hierarchical
nanoscaled GDS in a stable HEA, the potentially-new defor-
mation mechanism associated with extensive SFs/Twins
occurs even after a small tensile strain, responsible for
the steady work hardening and large tensile ductility. Such
a super-high density of extremely-fine SFs/TBs themselves
(~4.14 ×108 m2/m3) not only effectively mediates plastic
strains, exhibiting SF-induced plasticity (SFIP), but also
substantially helps delocalize plastic deformation, coupled
with the gradient-induced strain delocalization. First,
the penetrations of more and more density SF/TB bundles
across dislocation walls progressively subdivide stable dislo-
cation structures and built-in a unique three-dimensional
bundle/cell networks (coupled with inherent, spatial local
chemical fluctuations) that act as strong obstacles to disloca-
tion slip (Fig. 3, C to G). In this case, intensive interactions
among SFs/TBs and dislocations are promoted to induce con-
siderable strengthening and work-hardening, thus greatly
(Page numbers not final at time of first release) 4
counteracting the hastily-reduced Θ trend of the GDS struc-
ture associated with the rapid recovery of pre-existing full
dislocations and a relatively-limited capacity of dislocation
multiplications at a small strain (Fig. 2B).
In addition, the progressively refined three-dimensional
SF/cell networks also acts as sustainable sources for high-
density full dislocation storage during uniaxial tension. The
newly-accumulated density of full dislocations in the GDS-H
sample is substantially higher than that in the FG counter-
parts at the same tensile strain (fig. S4), still consequently
offering a progressive and steady work-hardening response
of GDS (Fig. 2B). Benefiting from the roles co-played by such
unexpected high-density linear and planar defects, bulk GDS
exhibits a better strain compatibility without strain localiza-
tion and visible cracks in the grain interior or along GBs, re-
sultantly a comparable high tensile plasticity with FG
counterparts, at higher stress levels (Fig. 2A).
We compare the yield strengths and the product of
strength and ductility of GDS samples with the same compo-
sitional HEA (40, 41, 49–51) and other existing high-
performance metals and alloys with gradient structures (10,
36, 52–55). The strength was normalized by its Young’s mod-
ulus of the corresponding material. When plotted this way,
we found that the GDS HEA achieves the best combination
of uniform tensile elongation and strength. It is not surpris-
ing that conventional gradient nanograined metals and alloys
with a high-density of HAGBs inevitably suffer from struc-
tural coarsening, such as GB migration with concomitant
coarsening (contributing to plasticity) and resultant soften-
ing, albeit which obviously sacrifice their strengths and sta-
bility to a certain extent (10). By contrast, the monotonic
strengthening with high steady work hardening was achieved
in the stable single fcc phase GDS HEA with spatially gradi-
ent LABs, contributed by the above SF and twin behavior,
with gradual structural refinement.
In summary, our observations show that engineering
gradient LABs structures on a single fcc-phase Al0.1CoCrFeNi
HEA can help readily activate a SFIP-strengthening mecha-
nism, leading to an exceptional strength and ductility. The
discovery of such SF/twin behavior in the GDS HEA is essen-
tial for acquiring the common deformation features inherent
to HEAs and widely applicable to other HEA systems to
achieve better performance with superior properties, which
are of both great fundamental and applied importance for
advanced engineering applications, such as automobiles,
power stations, and aeronautic systems.
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ACKNOWLEDGMENTS
We thank Dr. S.Y. He for performing HAADF-STEM experiments, Dr. M.X. Yang for
measuring the back stress, Dr. J. Xu for analyzing EBSD results, Dr. C.J. Zhang,
Dr. L.F. Cheng for performing raw sample forging treatment and Dr. J. Burns for
performing APT experiments. Funding: Q. Pan and L. Lu acknowledge the
financial support by National Science Foundation of China (NSFC, Grant
Numbers. 51931010, 92163202, 52122104 and 52071321), the Key Research
Program of Frontier Science and International partnership program (GJHZ2029)
and Youth Innovation Promotion Association (2019196), Chinese Academy of
Sciences (CAS), and LiaoNing Revitalization Talents Program (XLYC1802026).
P. K. Liaw very much appreciates the support from the National Science
Foundation (DMR-1611180 and 1809640) and the US Army Research Office
(W911NF-13-1-0438 and W911NF-19-2-0049). The present research used
resources at the Spallation Neutron Source (SNS), a U.S. Department of Energy

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Fig. 1. Typical microstructure and structural gradient of gradient
dislocation structure. Cross-sectional EBSD (A, B) images of the GDS-
H Al0.1CoCrFeNi HEA processed by cyclic-torsion processing at a torsion
angle amplitude of 20° showing the distributions of a grain-scaled
morphology, orientation (A), and three types of boundaries (i.e., HAGB,
LAB and TB) with different misorientation angles (B) within an
approximately 1.2 mm depth from the surface, compared with that in the
core (G, H). (C) Schematic of GDS with a gradiently-distributed low-
angle dislocation structure. The corresponding bright-field TEM images
of the dislocation structures at the topmost surface (D) of treated
samples (indicated in A, C). The misorientation angle of each cell wall in
Fig. 1D is measured and indicated in (D), using an electron procession
diffraction technique (28) in TEM. The up-left inset in (D) is the
corresponding SAED patterns. (E) A closer view of a typical dislocation-
cell structure. (F) Plots of the misorientation-angle variation, measured
with respect to the origin, across multiple cells at the topmost surface of
the GDS-H HEA, along the solid white line arrow in (D).

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Fig. 2. Mechanical properties of the GDS Al 0.1CoCrFeNi HEA.
(A) Tensile engineering stress-strain relations of GDS, CG, and FG
samples. (B) Work-hardening rate and true strain relations of GDS
samples compared with their homogeneous components. (C) The
variations of measured microhardness along the distance from the top
surface to interior of GDS samples after cyclic-torsion processing and
those after a tensile strain of 40%. (D) The product of strength
and ductility versus yield strength normalized by Young’s modulus of
the GDS Al0.1CoCrFeNi HEA, compared with the counterparts with
homogenous and gradient-grained structures and other metals and
alloys with gradiently-distributed nanograins and nanotwins reported
in the literature (10, 36, 52–55). The error bars in (C, D) represent
standard deviations from 10 independent hardness measurements and
more than 3 independent tensile tests. GNG and GNT denote the
gradient nanograin and nanotwin, respectively; TWIP denotes twinning-
induced plasticity.

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Fig. 3. Deformation microstructure of the GDS-H Al0.1CoCrFeNi HEA
at a tensile strain of 3%. Cross-sectional EBSD (A, B) images showing
the distributions of the grain-scaled morphology, orientation (A), and
three types of boundaries with different misorientation angles (B) within
~1.2 mm depths from the surface, compared with that in the core
(H, I) after tension. The corresponding SEM (C, D), bright-field TEM
(E) images presenting the widespread occurrence of dense tens of
micron-length SF bundles, indicated by the white arrows, cutting
through multiple dislocation-cell structures. The inset in (E) is
the corresponding SAED patterns containing parallel streaks (along
[111] direction, noted by the white arrow) from SFs. (F) An aberration-
corrected high-angle dark-field scanning transmission electron
microscopy (HAADF-STEM) image taken from bundles in the vicinity
of dislocation-cell walls with a relative low dislocation density, revealing
an ultrahigh density of SFs and TBs. (G) Close-up HAADF-STEM image
exhibiting numerous nanoscaled SFs or twin segments. The solid
and dashed lines in (F-G) denote SF/TBs and the (111) plane,
respectively. (J-K) The corresponding SEM (J) and TEM (K) images at
the sample core presenting planar-slip-induced parallel dislocation
morphologies. The white line with double arrows in (C) denotes loading
axis (LA).

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Fig. 4. Deformation feature at 40% tensile strain and in-situ neutron-
diffraction measurements during uniaxial tension of the GDS-H
Al0.1CoCrFeNi HEA. (A-B) SEM and TEM images of a high density of
SF bundles (indicated by white arrows) in the whole grain interior.
(C) Typical atomic-resolution HAADF-STEM image showing an ultrahigh
density of SFs and TBs with inclined short SFs. The solid and dashed
lines in (C) denote SF/TBs and the (111) plane, respectively. (D) The
evolution of the lattice strains for (111)//LA and (222)//LA grains in both
GDS-H and FG samples versus engineering strain measured by in-situ
neutron-diffraction experiments. The error bars are obtained from the
uncertainties of the single-peak fitting on hkl diffraction peaks. The black
arrows in (D) indicate the occurrence of (111) and (222) splitting event.
(E) The variation of the calculated SF probability (SFP) as a function of
engineering strain in both GDS-H and FG samples.

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 Gradient-cell–structured high-entropy alloy with exceptional strength and ductility
Qingsong Pan, Liangxue Zhang, Rui Feng, Qiuhong Lu, Ke An, Andrew Chihpin Chuang, Jonathan D. Poplawsky, Peter K.
Liaw, and Lei Lu

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