Precipitation-hardened high-

entropy alloys for high-temperature

applications: A critical review
Boxuan Cao, Tao Yang, Wei-hong Liu, and C.T. Liu
Conventional alloy design based on a single primary element has reached its limits in terms
of performance optimization. An alloy design strategy with multi-principal elements has
recently been uncovered to overcome this bottleneck. Multicomponent alloys, generally
referred to as high-entropy alloys (HEAs), exhibit many promising properties, especially
outstanding mechanical performance at cryogenic, ambient, and elevated temperatures. In
this article, we focus on precipitation-hardened HEAs, which are potential candidates for
next-generation structural materials, especially at high temperatures. The key issues involved
include precipitation behaviors, phase stability, and phase control, all of which provide useful
guidelines for further development of high-temperature materials with superior performance.
In particular, we address the formation of cellular γ′ precipitates at grain boundaries, which is
closely related to the embrittlement of HEAs at intermediate temperatures. Critical issues and
design strategies in developing HEAs for high-temperature applications are also discussed.

Introduction Various precipitate phases have been explored and studied

The concept of high-entropy alloys (HEAs) was initially pro-
posed independently by Yeh1 and Cantor,2 abandoning tradi-
tional single-principal-element alloy systems and adopting a
multicomponent design strategy with chemical element con-
centration for each element ranging between 5 and 35 at.%. In
the early stages of developing HEAs, it was widely accepted
that the formation of a simple solid-solution phase is preferred
rather than complex intermetallic compounds, owing to the
increased configurational entropy with the increased number
of chemical components. For example, the prototypical equi-
atomic CoCrFeMnNi “Cantor alloy”2 is a face-centered-cubic
(fcc) solid-solution phase, which exhibits excellent ductility,
but limited strength.3,4
Second-phase strengthening, as a traditional approach for
strength enhancement, is widely used among Ni-based super-
alloys,5 Al alloys,6 Mg alloys,7 and high-performance steels.8
Precipitation strengthening is also effective for HEAs.9–18 Though
the formation of a second phase deviates from the original inten-
tion to retain a single solid-solution phase in HEAs, second-phase
strengthening leads to unambiguous properties enhancement,
which has become a research hotspot at the present time.
so far, such as the L12-type phase (γ′),9–11 σ and μ phases,13,14
Laves phase,15 B2 phase,16,17 and carbides.18 Ni-based superal-
loys made use of the L12-type Ni3(Al,Ti) phase, which pro-
vides high-temperature strength due to its stability at high
temperatures.19 Molybdenum contributed to the formation
of topologically close-packed (TCP) phases (σ and μ phases),
whose hardnesses are extremely high, up to 15 GPa.13
Niobium addition into CoCrFeNi, as an example, induced
the formation of a Nb-rich Laves phase, resulting in an
increase in yield strength from 147 MPa for CoCrFeNi to 637
MPa for CoCrFeNiNb0.412.15 In Al0.7CoCrFeNi HEA, a high
ultimate tensile strength of 1223 MPa can be attributed to the
CsCl-type B2 precipitates embedded in the disordered body-
centered-cubic (bcc) matrix.16 It should also be noted that the
carbide volume fraction increased as the carbon content increased,
leading to a significant strength enhancement.18 The L12-type
precipitation-hardened HEAs (PH-HEAs), in particular, exhibit
a promising outlook for high-temperature applications. The
addition of Al and Ti atoms into single-phase NiCoFeCr HEA
can induce the formation of coherent L12 precipitation with
a dramatic strength enhancement.10 The crystal structure of

Boxuan Cao, Department of Materials Science and Engineering, City University of Hong Kong, Hong Kong; bocao4-c@my.cityu.edu.hk
Tao Yang, Department of Mechanical Engineering, City University of Hong Kong, Hong Kong; taoyang6-c@my.cityu.edu.hk
Wei-hong Liu, Department of Materials Science and Engineering, Harbin Institute of Technology, China; weihonliu2@gmail.com
C.T. Liu, Department of Materials Science and Engineering, City University of Hong Kong, Hong Kong; chainliu@cityu.edu.hk
doi:10.1557/mrs.2019.255

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 Precipitation-hardened high-entropy alloys for high-temperature applications: A critical review
the precipitates in L12-type PH-HEAs is analogous to Ni3Al-type
precipitates in Ni-based superalloys.19 Dual-high-entropy
nanostructures,9,11 consisting of high-entropy precipitates in
a high-entropy matrix, are unique to PH-HEAs. The compat-
ibility between the high-entropy matrix (γ phase) and high-
entropy precipitates (γ′ phase) in terms of similar lattice con-
stants enables excellent thermal stability of precipitation as
well as low interfacial energy between the matrix and the
precipitate. γ matrix is a solid-solution fcc phase with lat-
tice constant close in value to that of the γ′ phase, allowing
a coherent interface between the matrix and precipitates. An
incoherent interface between the precipitate and matrix, such
as that of σ and μ phases, usually acts as a source for crack
initiation and propagation, leading to a severe brittle fracture
during deformation.20 In contrast, a coherent L12-type high-
entropy precipitate embedded in the high-entropy matrix
leads to significant strength improvement without sacrificing
ductility.9,21 Severe lattice distortion in the interiors of the
high-entropy matrix and the high-entropy precipitates also
contributes to the strength enhancement by impeding dislo-
cation motion.22
Due to the high-entropy effect, dual-high-entropy nano-
structures can yield HEAs with superior phase stability at high
temperatures, when compared to conventional superalloys.
In some NiFe-based superalloys, γ″ (Ni3Nb) is the principal
strengthener with a crystal structure of body-centered tetrag­
onal. Commercial Inconel 718 superalloy is known to soften
quickly above 650°C due to the transformation from γ″ phase
to δ.23 On the other hand, Ni2CoCrFeNiNb0.15 (atomic molar
ratio) HEAs retained the γ″ precipitate even after annealing
at 650°C for 80 h without further phase transformation.12 In
addition, a stable γ/γ′ microstructure was retained even after
aging at 1100°C for 500 h in the case of Ni40.7Co20.6Fe11.5Cr12.2
Al7.8Ti7.2 (at.%) and Ni48.6Co17.0Fe9.0Cr7.5Al10.3Ti5.8Ta0.6Mo0.8W0.4
(at.%) HEAs.24
Sluggish diffusion effects can also provide extra benefits
for properties of HEAs at high temperatures by enhancing
high-temperature resistance, as compared with conventional
superalloys. First, creep resistance is controlled by the diffu-
sion rate through dislocation climb and cross-slip;25 smaller
diffusion rates suggest potential superb creep properties in
HEAs. Second, the temporal evolution of precipitation in
PH-HEAs affects their performance during the precipitation
coarsening stage under long-time thermal exposure. It was
recently reported that excellent thermal stability26,27 can be
ascribed to the sluggish diffusion in HEAs.
PH-HEAs thus have demonstrated the promise to serve
as new structural materials at elevated temperatures, imply-
ing that they have the potential to replace conventional
Ni-based superalloys and become next-generation high-
temperature structural materials. In this article, we highlight
recent developments in PH-HEAs, focusing on their micro-
structural evolution. The opportunities and challenges faced
by PH-HEAs for high-temperature applications are also
discussed.
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Dual-phase γ + γ′ microstructure
Ni-based superalloys, as classical materials designed for the
high-temperature environment, have been under development
for decades since the emergence of rotating engines.19 There
are several reasons for the application of superalloys for indus-
trial applications and especially aircraft applications, includ-
ing high-temperature strength, creep resistance, and oxidation
resistance.19 The microstructures of some PH-HEAs9,21,28–31 are
analogous to those of superalloys, with γ′ precipitates embed-
ded in a γ matrix, (Figure 1a, left and middle), but with high-
entropy characteristics both in the matrix and precipitates.
Typically, γ′ is a Cu3Au-type high-entropy intermetallic com-
pound with Ni and Co atoms mainly substituting for the center
sites on the cubic faces, and with Al and Ti atoms mainly sub-
stituting for the corner sites of the unit cell. Fe and Cr atoms
evidently partition into the γ matrix and are depleted in the γ′
precipitation, as shown in Figure 1a, right (black circles rep-
resent the precipitates).11 Cu has been proven to promote the
nucleation of the γ′ phase by providing heterogeneous nucle-
ation sites in the form of Cu clusters,28 resulting in a conjoint
γ′ phase/Cu-rich cluster within the fcc matrix.
Detrimental phases
On the path toward optimizing the microstructures of PH-
HEAs, the most urgent task is to achieve a pristine γ/γ′ structure
without the formation of other undesirable brittle intermetallic
phases, especially the TCP phases. Daoud et al.32 and Manzoni
et al.33 observed the formation of a needle-shaped NiAl
phase (β phase in Figure 1b, right) and Cr-Fe-rich platelets
in Ni36Co25Fe15Cr8Al10Ti6 (at.%) and Ni16Co15Fe15Cr23Cu8Al23
(at.%) PH-HEAs, respectively. Niobium contributed to the
formation of the Nb-rich Laves phase during homogenization,
while the B2-type NiAl phase was observed at the γ/Laves
interfaces during aging in the Ni22Co30Fe18Cr18Al8Nb4 (at.%)
alloy (Figure 1c, left).34
Chang et al.35 found that the needle-like Ni3Ti phase (the η
phase) formed in the Ni1.5Co1.5FeCrAl0.1Ti0.4 PH-HEA after ag-
ing at 1000°C (Figure 1c, middle), while the NiAl phase (the β
phase) was observed in the Ni1.5Co1.5FeCrAl0.5 PH-HEA after
aging at 900°C (Figure 1c, right). Furthermore, the formation
of the η phase was found to be suppressed by replacing Ti
with Al addition, but excessive Al will induce the formation
of the β phase.35 The L21-type Heusler phase was found in the
Ni36Co25Fe15Cr8Al10Ti6 (at.%) PH-HEA, which remained even
after a long-time annealing at 900°C.29 The Heusler phase
is a Ni2TiAl-type precipitate with a large unit cell that com-
prises eight small bcc NiAl-type unit cells. For each small
bcc, nickel atoms occupy the corner sites and aluminum or
titanium alternatively occupy the body-center site. These
undesirable phases are generally hard and brittle, and thus
they would act as possible sources for crack initiation and
propagation. On the other hand, they consume valuable Al
and Ti content, which could be used for elevating the γ′ phase
volume fraction and providing alloys with higher strengths
at high temperatures.
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 Precipitation-hardened high-entropy alloys for high-temperature applications: A critical review

Figure 1. Nanostructures and microstructures of precipitation-hardened high-entropy alloys (PH-HEAs). (a) (Left) Transmission electron
microscope (TEM) image showing the morphology of the L12 precipitate. (Inset) Selected-area diffraction patterns taken from zone axis
Z = [001]. Red circles show the superlattice diffraction spots of the L12-type precipitates, (middle) high-resolution TEM image showing the
coherent interface between an L12 precipitate and the face-centered-cubic (fcc) matrix, and (right) elemental distribution map obtained by
atom probe tomography.11 (b) Microstructure of Ni36Co25Fe15Cr8Al10Ti6 (at.%) PH-HEAs: (left) high magnification of γ′ precipitation, (middle)
dendritic and interdendritic area, and (right) high magnification of needle-like NiAl precipitates (the β phase).32 (c) Detrimental phases: (left)
NiAl phase at γ/Laves interfaces during aging in Ni22Co30Fe18Cr18Al8Nb4 PH-HEA,34 (middle) needle-like η phase in Ni1.5Co1.5FeCrAl0.1Ti0.4
PH-HEA, and (right) β phase in Ni1.5Co1.5FeCrAl0.5 PH-HEA.35 (d) Microstructure of Ni1.5Co1.5FeCrAl0.2Ti0.3 PH-HEA. (Left) Grain boundary,
(middle) magnification of cellular γ′ precipitation along a grain boundary, and (right) well-developed spherical γ′ precipitates within the
grain interior.37 Note: DP, discontinuous precipitation (cellular γ′ phase); GB, grain boundary.

Cellular precipitation at grain boundaries
Another key issue is the heterogeneous precipitation of cellu-
lar γ′ precipitates along grain boundaries,36,37 which is also ob-
served in traditional alloys, such as Al alloys,38 Cu alloys,39 and
Ni-based superalloys.40 Such discontinuous precipitation behav-
ior37 is generally ascribed to the chemical supersaturation in the
γ matrix and grain-boundary migration (Figure 1d). It should be
noted that tuning the chemical compositions and heat-treatment
procedures can avoid such precipitation. Cellular precipitation
can possibly be eliminated by changing the quenching method
from water quenching to furnace cooling or substituting Co
content with Ni. The slower cooling rate is expected to provide
more time for γ′ to precipitate at grain boundaries, thus impeding
the grain-boundary migration and preventing cellular precipita-
tion. Substituting Co by Ni increases the γ′ solvus temperature,
which allows more γ′ to precipitate during the cooling process.

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 Precipitation-hardened high-entropy alloys for high-temperature applications: A critical review

The supersaturation degree in the matrix is reduced, resulting at 1000°C in air and vacuum before tensile testing in an argon
in the disappearance of cellular γ′ precipitation. Yeh et al.36 atmosphere. The samples after exposure to air exhibited a
and Tsai et al.37 proposed that such cellular γ′ precipitates at higher level of ductility loss than those under vacuum.44 Apart
the grain boundaries have little influence on room-temperature from oxygen, water vapor in air is also thought to dissociate
tensile properties, but they cause rapid ductility loss at interme- into atomic H on Ni3Al surfaces, resulting in embrittlement.48
diate temperatures (roughly from 600°C to 800°C), as shown in Heterogeneous bonding at the grain-boundary area, which
Figure 2a, which was associated with intergranular fracture.36,41 causes intrinsic grain-boundary weakness, was considered to
Similarly, the precipitation of brittle grain-boundary oxides be the reason for the fracture surface consisting of the pres-
and carbides also caused ductility loss with increased temper- ence of a completely intergranular fracture surface.45
atures above 600°C in Inconel 718, but ductility at ambient A fundamental understanding is still lacking at the pres-
temperatures remained unaffected.42 Apart from the effects of ent time, and more systematic work is required to elucidate
grain-boundary precipitates,1,2 there are several other possible the intrinsic mechanisms of the intermediate temperature
interpretations for the embrittlement, such as interstitial impu- embrittlement phenomenon.
rities segregation,43 environment-induced embrittlement,44 and
intrinsic grain-boundary weakness.45 Impurity (such as Bi and S) Computation-aided alloy design
levels as low as tens of ppm46,47 are sufficient to induce The CALculation of PHase Diagrams (CALPHAD) method,
embrittlement. In one study, pure nickel samples were exposed which is based on thermodynamic calculations, offers reliable
guidance for alloy design in terms of chemical
compositions and heat-treatment conditions.
Different from previous trial-and-error routes for
alloy design, the CALPHAD method accelerates
the search for a target microstructure and com-
position by computational approaches, which
greatly reduces the experiments needed.
It was found that a stable γ + γ′ dual phase can
be maintained by adjusting the compositions and
heat-treatment temperature to avoid the for-
mation of η and σ phases (Figure 2b, left).21
He et al. found that the results of the forma-
tion of the minor detrimental Heusler phase
in (NiCoFeCr)100–x–yAlxTiy PH-HEAs, apart
from the γ matrix and γ′ precipitation, were
in good agreement with experimental obser-
vations.49 For the Ni1.5Co1.5FeCrAlxTiy (x + y =
0.5) PH-HEAs, Chang and Yeh35 successfully
predicted the microstructural evolution of
(γ + η) in Ti0.5 to (γ + η + γ′) in Al0.1Ti0.4, to (γ + γ′)
in Al0.2Ti0.3, to (γ + β + γ′) in Al0.3Ti0.2 and to
(γ + β) in Al0.5 PH-HEAs (Figure 2b, right).
Through a comparison of the phase diagrams
of Ni33Co17Fe17Cr17Cu8Al8 (at.%) and Ni34.8Co17
Fe17Cr14Cu8Al8Ti1Mo0.1W0.1 (at.%) (Figure 2c),
it was found that the curve for the γ′ phase was
shifted upward, which implied a higher γ′ vol-
ume fraction in the Ni34.8Co17Fe17Cr14Cu8Al8
Ti1Mo0.1W0.1 (at.%) PH-HEA than the
Ni33Co17Fe17Cr17Cu8Al8 (at.%) PH-HEA.50 It is
Figure 2. Intermediate temperature embrittlement of precipitation-hardened high-entropy of interest to point out that small additions of
alloys (PH-HEAs) and computational-aided alloy design. (a) (Left) Ductility loss at 800°C in refractory elements Mo, W, and Ti can raise the
Ni1.5Co1.5FeCrAl0.2Ti0.3 PH-HEAs.37 (Right) Strength and ductility of Ni27.27Co27.27Fe18.18Cr18.18 volume fraction of the γ′ phase considerably,
Al3.31Ti5.78 (at.%) PH-HEAs at different temperatures; cellular precipitation caused sharp
ductility loss at around 750°C.36 (b) CALculation of PHase Diagrams (CALPHAD) results of resulting in the suppression of the NiAl.50
(left) (NiCoCr)97–xAlxTi3 (at.%) PH-HEAs and (right) Ni1.5Co1.5FeCrAlxTiy (x + y = 0.5) PH-HEAs.
21 35
However, some discrepancies still exist
(c) Phase diagram predictions of (left) Ni33Co17Fe17Cr17Cu8Al8 PH-HEA and (right) Ni34.8Co17 between the experimental results and the
Fe17Cr14Cu8Al8Ti1Mo0.1W0.1 (at.%) PH-HEA.50 Arrows in the left panel indicate the expansion
of γ′ phase region through small alloy additions of Ti, Mo, and W. CALPHAD predictions13,51 in terms of detri-
mental phases, volume fractions of γ′, and γ′

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 Precipitation-hardened high-entropy alloys for high-temperature applications: A critical review
solvus temperatures. It appears that more thermodynamic data
for CALPHAD calculations are needed for PH-HEAs design.
Summary
The microstructural evolution of PH-HEAs has been reviewed in
this article. A dual high-entropy nanostructure consisting of high-
entropy γ′ precipitates and a high-entropy γ matrix is analogous
to that of conventional superalloys. Due to severe lattice distor-
tion, sluggish diffusion, and the high-entropy effect, PH-HEAs
have the potential to replace conventional Ni-based superalloys
and to be used in high-temperature environments. Some critical
issues remain, suggesting future directions for research:
1. Phase control should be given higher priority. Hard and
brittle deleterious phases need to be eliminated by care-
fully tuning chemical compositions and heat treatments. The
CALPHAD method makes it easier to obtain a target micro-
structure without time-consuming experiments. Retaining
a stable γ′/γ dual-phase structure at higher temperatures is
a presumption for the design of high-temperature struc-
tural materials. Phase stability evaluation is an important
consideration in selecting structural materials under
elevated-temperature environments. Besides, a high-volume
fraction of the γ′ strengthener is preferred in order to develop
high-performance structural materials. The preferential size,
morphological shape, and composition of the precipitates, as
well as lattice misfit between the matrix and the precipitates
in PH-HEAs for high-temperature applications, remain open
questions for researchers.
2. The high-temperature strength of PH-HEAs decreased
rapidly when the temperature approached 1000°C because
of the rapid dissolution of hardening precipitates. The yield
strength of the Ni36Co25Fe15Cr8Al10Ti6 PH-HEA remained
at 672 MPa at 800°C, but dropped to just 148 MPa at
1000°C.32 Similarly, the hardnesses of Ni40.7Co20.6Fe11.5Cr12.2
Al 7.8Ti 7.2 (at.%) and Ni 48.6Co 17.0Fe 9.0Cr 7.5Al 10.3Ti 5.8Ta 0.6
Mo0.8W0.4 (at.%) PH-HEAs were superior to that of Ni-based
superalloy CM247LC (Ni-10Co-8.4Cr-5.5Al-1.0Ti-3.0
Ta-0.7Mo-10.0W-0.15C-0.015B-0.05Zr-1.5Hf wt%) at
room temperature, but softened quickly when the temperature
increased above 600°C.24 The stabilization of the L12 pre-
cipitate at high temperatures is a key issue for alloy design.
3. There is limited data on creep resistance30 and thermal
fatigue behavior of PH-HEAs at the present time. Also,
the mechanical performance of directionally solidified
(DS) and single-crystal (SC) PH-HEAs have been scarcely
reported.30,52 There are three main reasons for the enhance-
ment of elevated-temperature properties in DS- and SC
PH-HEAs. The elimination of grain boundaries normal to the
stress axis improves creep resistance and high-temperature
ductility because of the lack of failure initiation sites. The
second is that a preferred low-modulus [001] orientation in
the solidification direction improves thermal fatigue resis-
tance. Third, due to the removal of grain boundaries along
the stress axis in the DS PH-HEAs and the complete removal
of grain boundaries in the SC PH-HEAs, incipient melting
858
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temperatures for such PH-HEAs are higher than their poly-
crystal counterparts, implying a better high-temperature
performance. More importantly, we need to compare the
high-temperature strength and creep resistance of DS- and
SC PH-HEAs with that of Ni-based superalloys.
4. High-temperature oxidation resistance is another key issue
to be characterized. Hot corrosion, as a form of degradation,
should also be considered. PH-HEAs mainly count on Al
and Cr content to form alumina and chromia, respectively,
for surface protection and oxidation resistance. As a result,
the alloying additions of Al and Cr should be quantitively
studied in order to improve the PH-HEA oxidation and cor-
rosion resistance.
Acknowledgment
The research is supported by the Hong Kong Government
GRF (Grant No. CityU 11202718).
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(Basel) 20, 646 (2018).  He was also a distinguished professor at Auburn
Boxuan Cao is a doctoral candidate in the Depart-
ment of Materials Science and Engineering at
the City University of Hong Kong, Hong Kong.
He obtained his bachelor’s degree in 2018
from Shandong University, China. His current
research focuses on the applications of high-
entropy alloys in elevated temperature envi-
ronments. Cao can be reached by email at
bocao4-c@my.cityu.edu.hk.
Wei-hong Liu is an associate professor at the
Harbin Institute of Technology (Shenzhen),
China. She obtained her PhD degree from the
City University of Hong Kong, Hong Kong, in 2016.
Her research focuses on the development and
mechanical behavior of advanced materials,
including high-entropy alloys and metallic glasses.
She has more than 10 papers published, and
two of them were rated as highly cited papers by
the Clarivate Web of Science. Liu can be reached
by email at weihonliu2@gmail.com.
C.T. Liu is a university distinguished professor
at the City University of Hong Kong, Hong Kong.
He received his PhD degree in materials science
and engineering at Brown University in 1967.
He was previously at Oak Ridge National Labo-
ratory as group leader of the Alloying Behavior
and Design Group, and The University of Ten-
nessee as a distinguished research professor.
University, and a chair professor at The Hong
Kong Polytechnic University. His research inter-
ests include physical metallurgy and mechanical
behavior of alloys, nanostructured materials,
intermetallic compounds and bulk amorphous
alloys, microstructure and phase transformation, alloy design of high-temperature
structural materials, precious metals, Ti-based alloys, metal-matrix compos-
ites, and innovative materials processing. Liu can be reached by email at
chainliu@cityu.edu.hk.

Tao Yang is a postdoctoral fellow at the City

CALL FOR
University of Hong Kong, China. He received his
master’s degree in materials science and engineer-
ing from Xiamen University, Hong Kong, in 2014,
PAPERS
and his PhD degree in mechanical engineering
from the City University of Hong Kong in 2018. Submission Deadline—
He has published more than 10 peer-reviewed June 1, 2020
articles on innovative design and microstructural
characterization of advanced structural materi-
als, including high-entropy alloys, superalloys, JANUARY 2021
steels, and titanium alloys. Yang can be reached
by email at taoyang6-c@my.cityu.edu.hk. Early Career Scholars
in Materials Science 2021
Novel materials discovery
Electronic, photonic and magnetic materials
Energy conversion and storage materials
New thermal and structural materials
Soft materials
Biomaterials and related topics
Nanoscale science and technology
Advances in materials characterization methods
and techniques
Computational materials science, modeling and theory

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