Scripta Materialia 191 (2021) 131–136

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Scripta Materialia
journal homepage: www.elsevier.com/locate/scriptamat

Designing Vx NbMoTa refractory high-entropy alloys with improved

properties for high-temperature applications
M. Wang a,b, Z.L. Ma a,b,∗, Z.Q. Xu a,b, X.W. Cheng a,b,∗
a
School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China
b
National Key Laboratory of Science and Technology on Materials Under Shock and Impact, Beijing 100081, China

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

Article history: Poor high/medium-temperature phase stability and/or low room-temperature ductility are currently bot-
Received 16 July 2020 tlenecks of refractory high-entropy alloys (RHEAs) that restrict their high-temperature applications. Here,
Revised 14 September 2020
we explored novel Vx NbMoTa RHEAs with vanadium concentrations of 0–25 at.%. Vx NbMoTa RHEAs ex-
Accepted 14 September 2020
hibit a single body-centered cubic (BCC) structure with unprecedented phase stability at a wide temper-
ature range from solidus down to 350°C. The grain structure of Vx NbMoTa can be substantially refined
Keywords: when increasing the V concentration since higher V contents induce stronger solutal effects which con-
Refractory high-entropy alloys tribute to higher growth restriction factors. Equimolar VNbMoTa exhibits the yield strength of 811 MPa
Grain Refinement at 10 0 0°C that is superior to most RHEAs reported by far, and this alloy also shows excellent room-
Phase stability
temperature ductility with the fracture strain > 25% and no strain-softening at high temperature, which
Mechanical properties
is rarely seen in many popular RHEAs. These exceptional performances of VNbMoTa enable it to be a very
promising material for high-temperature applications.
© 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

For a long time, conventional alloy designs are constrained to
the model of combining a/few principal component(s) with sev-
eral minor elements added to tailor properties. Since this strat-
egy only explores limited compositional space, the development
and application of alloys are largely restricted. Different from con-
ventional alloys, high-entropy alloys (HEAs) that consist of at least
four principal elements explore a wide composition space in the
interior regions of hyper-dimensional multicomponent phase di-
agrams and, therefore, open up a new dimension for the explo-
ration of new materials and new properties [1,2]. Inspired by this
novel alloy design strategy, refractory high-entropy alloys (RHEAs)
were also fabricated by employing refractory elements from Group
IV, V, and VI, and sometimes with non-refractory additions such
as Ni, Co, Al, or Si to tune the mechanical properties [3–6]. Since
alloy softening generally occurs at temperatures higher than 0.5-
0.6Tm , RHEAs featuring high melting points can exhibit higher
strength at elevated temperatures (> 800°C) compared with widely
used Nickel-based superalloys such as Inconel 718 and Haynes 230
[7–10], which enables RHEAs to be very promising alternatives
for high-temperature applications. Nevertheless, most RHEAs ex-
hibit lower ductility at room temperature (RT) and/or poor phase
stability at high temperatures [7,11–14]. One approach to tackle
∗
Corresponding authors.
E-mail addresses: z.l.ma@bit.edu.cn (Z.L. Ma), chengxw@bit.edu.cn (X.W. Cheng).
this bottleneck is to design basket-weave nano-scale microstruc-
tures analogous to Nickel-based superalloys. As recently reviewed
by Miracle et al. [15], this type of RHEA is named as refractory
high entropy superalloys (RSAs) which exhibit disordered A2 + or-
dered B2 basket-weave nano-structure and can show compressive
yield strengths up to 935 MPa at 10 0 0°C and high RT compres-
sive ductility (>50%). However, some RSAs suffer from the dis-
solution of B2 phases during heat treatment above 600°C, which
degrades their high-temperature strength [15]. Another approach
to maintain both RT ductility and high-temperature strength is
to design single-phase disordered solid solution RHEAs and adjust
their properties via alloying. This is focused in this study. Single-
phase RHEAs are usually more ductile than multi-phase RHEAs
and can exhibit good high-temperature phase stability [16], and
therefore high strength. However, it is still challenging to simul-
taneously achieve good RT ductility and high strength and good
phase stability at high temperatures. For example, WNbMoTa al-
loy which is one of the most classical RHEAs initially developed
by Senkov et al. exhibits a single-phase structure and the ex-
ceptionally high yield strength (405 MPa) at 1600°C, but it only
has 2.1% fracture strain at RT [7]. Until now, only TiZrHf alloyed
with Ta, Nb, and Nb-Ta reveal single-phase structures at RT and
tensile fracture strains ~15–30% that are comparable to Ni-based
superalloys, but these alloys are relatively weak above 10 0 0 °C
and show poor phase stabilities at high/medium temperature
[16,17].

https://doi.org/10.1016/j.scriptamat.2020.09.027
1359-6462/© 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
132 M. Wang, Z.L. Ma, Z.Q. Xu et al. / Scripta Materialia 191 (2021) 131–136
Fig. 1. (a) Pseudo-binary phase diagram of V-NbMoTa [24]. (b) XRD patterns. (c) Microstructure and (d) EDS mappings of V1.0 RHEA. (e) Segregation ratios K. (f) TEM-SAED
patterns of Vx NbMoTa (x = 0.25, 0.5, 0.75, and 1.0) RHEAs.
Based on the classical WNbMoTa, this study will further adjust
the composition to explore novel single-phase RHEAs with good
RT ductility and high strength and good phase stability at high
temperatures. It is suggested that Mo and W contribute to the im-
proved high-temperature performance of WNbMoTa RHEA but are
also responsible for the room temperature brittleness [13, 18–21].
Yao et al. [22] replaced W in WNbMoTa with V and found that
VNbMoTa RHEA can exhibit the yield strength of 1.5 GPa and the
compressive fracture strain of 21% at RT, which are both higher
than those of WNbMoTa (σ y = 1.1 GPa, ε f = 2.1%). Binglun Yin
et al. [23] proposed that V can be the prime element for strength-
ening HEAs, and HEAs containing V have higher strengths com-
pared with their counterparts without V. Besides, the pseudo-
binary phase diagram of V-NbMoTa (calculated in the current
study with the Thermo-Calc and the TCHEA1 database [24]) in
Fig. 1(a) indicates that alloys containing 0–30 at.% V have a wide
temperature range (from 2300 to 500°C) exhibiting only a single
BCC phase, which implies that alloys in this composition range
would have good phase stabilities (i.e. only a single phase) at
high temperatures. Therefore, based on these benefits of vanadium,
Vx NbMoTa RHEAs with different V concentrations are fabricated
and explored in this study. Influences of the V contents on mi-
crostructures and phase stabilities of Vx NbMoTa are studied, and
mechanical properties at different temperatures are compared with
RHEAs reported by far.
Vx NbMoTa (x = 0.25, 0.5, 0.75, 1.0) RHEAs, hereinafter referred
to as V0.25, V0.5, V0.75, and V1.0, were prepared with high pu-
rity (>99.9 at. %) V, Nb, Mo, and Ta using vacuum arc melting in
water-cooled copper crucible under argon atmosphere. Alloys were
remelted at least eight times to ensure the compositional homo-
geneity. Crystal structures were examined with a Rigaku Ultima III
X-ray diffractometer using Cu-Kα radiation and the scanning rate
of 5°/min from 20° to 100°. Microstructures of as-cast alloys were
studied using a scanning electron microscope (SEM, Hitachi S4800)
equipped with an Oxford Instruments INCA Energy-dispersive X-
Table 1
Lattice constants of Vx NbMoTa measured by XRD
and TEM.
Alloys V0.25 V0.5 V0.75 V1.0
aXRD (Å) 3.241 3.227 3.214 3.204
aTEM (Å) 3.266 3.244 3.228 3.194
ray spectroscopy (EDS), and an Oxford HKL Nordlys II Electron
Backscattered Diffraction (EBSD). TEM samples were prepared by
mechanical milling and ion thinning and tested with a transmis-
sion electron microscope (TEM, FEI Tecnai G2 F20). RT and high-
temperature (800°C and 1000°C) mechanical properties of V1.0 al-
loy were measured at a constant strain rate of 10−3 s−1 using
an Instron 5569 universal testing machine and a dynamic ther-
mal simulation testing machine (Gleeble-3500) respectively. CAL-
culation of PHAse Diagrams (CALPHAD) was performed using the
Thermo-Calc and the TCHEA1 database to model the required ther-
modynamic properties of the alloy.
Typical XRD patterns in Fig. 1(b) show that all as-cast
Vx NbMoTa RHEAs exhibit the BCC crystal structure. But the XRD
pattern moves slightly to higher 2θ when increasing the V con-
centration, as typically shown by the enlarged (110) peaks at the
upper right corner of Fig. 1(b). This peak movement indicates the
decreased lattice constant (Table 1) as estimated by the Bragg’s
Law (2dsinθ = λ), which should essentially attribute to the smaller
atomic radius of V (rv =1. 346 Å) compared with the other three
elements (rTa = 1.467 Å, rNb = 1.468 Å, rMo = 1.4 Å) [25], which
leads to lattice shrinkage.
Vx NbMoTa RHEAs exhibit dendritic microstructures as typically
shown by V1.0 in Fig. 1(c). Fig. 1(d) shows the EDS map of the red
rectangle area is in Fig. 1(c). Compositions of the dendrite and in-
terdendrite regions of Vx NbMoTa RHEAs are specified in Table 2.
The segregation ratio of the element in dendritic and interden-
 M. Wang, Z.L. Ma, Z.Q. Xu et al. / Scripta Materialia 191 (2021) 131–136 133

Table 2
EDS measured compositions in dendritic and interdendritic regions in Vx NbMoTa RHEAs. Mean values and standard deviations are given
based on at least 5 measurements for each case. Segregation ratios (K) are calculated using mean values.

Alloys V Nb Mo Ta

V0.25 Nominal composition (at. %) 7.69 30.77 30.77 30.77

Dendrite (at. %) 5.32 ± 0.79 32.62 ± 1.19 30.22 ± 1.40 31.84 ± 1.60
Interdendrite (at. %) 12.99 ± 1.53 37.35 ± 1.23 26.62 ± 0.98 23.04 ± 1.91
K = cdr /cid 0.41 0.87 1.14 1.38
V0.5 Nominal composition (at. %) 14.29 28.57 28.57 28.57
Dendrite (at. %) 10.12 ± 1.37 29.70 ± 1.05 27.31 ± 2.13 32.87 ± 2.71
Interdendrite (at. %) 20.14 ± 1.96 30.54 ± 2.24 25.13 ± 1.57 24.19 ± 1.47
K = cdr /cid 0.50 0.97 1.09 1.36
V0.75 Nominal composition (at. %) 20 26.67 26.67 26.67
Dendrite (at. %) 14.45 ± 1.71 27.84 ± 0.54 26.51 ± 1.75 31.20 ± 1.58
Interdendrite (at. %) 30.28 ± 2.28 28.59 ± 1.73 21.16 ± 2.19 19.97 ± 1.13
K = cdr /cid 0.48 0.97 1.25 1.56
V1.0 Nominal composition (at. %) 25 25 25 25
Dendrite (at. %) 18.53 ± 1.92 25.83 ± 0.44 25.24 ± 0.85 30.40 ± 1.67
Interdendrite (at. %) 36.51 ± 3.05 27.18 ± 1.43 17.39 ± 1.96 18.92 ± 2.02
K = cdr /cid 0.51 0.95 1.45 1.61

dritic regions is given by K = cdr /cid . K > 1 or K < 1 indicates
that the element is segregated into the dendritic or interdendritic
region, and the more the K value deviates from 1, the more se-
vere the segregation of the element. As shown in Fig. 1(e), it is
clear that high melting-point elements Ta and Mo are prone to
segregate in the dendritic region, and the lower melting-point ele-
ment V is segregated into the interdendritic region. Nb is nearly
evenly distributed in the alloy. This phenomenon highlights the
influence of melting points on segregations and it is typical in
casted alloys. Segregations of these elements in the alloy should
also attribute to their different mutual solid solubilities. The bi-
nary phase diagrams [26] of these four elements indicate that i)
V cannot form complete solid solutions with Ta and Mo but it is
completely soluble in Nb above 300 K, ii) Nb forms complete solid
solutions with the other three elements at room temperature, and
iii) Ta and Mo show complete solid solubility. These are consistent
with the nearly zero segregation ratio of Nb and mutual segrega-
tions of Ta and Mo in the dendritic region, and also indicate that
the pseudo-binary V-NbMoTa can be comparable to the pseudo-
binary V-MoTa. Therefore, it is anticipated that increasing the V
content would expand the mushy zone (e.g. Fig. 1(a)) and thus in-
duce increased segregations of Ta and Mo as evidenced by Fig. 1(e).
The increased degree of element segregation with the expansion
of the mushy zone is also commonly found in other RHEAs (e.g.
WNbMoTa and WNbMoTaV [27]). Although dendritic and interden-
dritic regions show different compositions, they have the same
crystal structure and approximate lattice constants as indicated by
the XRD results. Fig. 1(f) shows the selected area electron diffrac-
tion (SAED) patterns of Vx NbMoTa RHEAs which confirm that they
are all single-phase BCC structures. The lattice constants calculated
from SAED (Table 1) also show a decreasing trend as increasing the
V content, which is consistent with the XRD results.
Fig. 2(a) summarizes the grain sizes of as-cast Vx NbMoTa
RHEAs. It is clear that as increasing the V content from V0.25
to V1.0, the grain size of the alloy continuously decreases from
~830 μm to ~250 μm, indicating that increasing the V content
can significantly refine grains. Similarly, Senkov et al. have also re-
ported that adding V into WNbMoTa can reduce the grain size from
200 μm to 80 μm [27].
Two theoretical paradigms, i.e. nucleant catalyst and solutal ef-
fect, account for the grain refinement in alloys [28]. It is believed
that both nucleation and the effect of the solute on the growth of
dendrites and the constitutionally undercooled zone in front of the
liquid-solid interface are important for grain refinement [29,30].
Solute restricts crystal growth by requiring an interface to cool as
it grows [31]. It also causes a region of constitutional undercooling
to develop in the liquid ahead of growing crystals in which fur-
ther nucleation events can be triggered [32–33]. A measure of how
rapidly constitutional undercooling develops in the early stages of
growth is the growth restriction factor Q, which is defined as
   
∂ (TCS ) ∂T
Q= =− (1)
∂ fS f →0
∂ fS
f S →0
S
where TCS is the constitutional undercooling and defined by
TCS = TL − TA . TL is the liquidus temperature and TA is the ac-
tual temperature. fS is the mass fraction of solid. For Vx NbMoTa
RHEAs, TL , TA , and fS can be calculated with the Thermo-Calc
and the TCHEA1 database [24]. Fig. 2(b) shows the TCS - fS
curves of Vx NbMoTa RHEAs. The initial slope of each curve is ob-
tained by fitting 5-10 closely spaced sampling points in the range
0 < fS < 0.01 using a parabolic function (TCS = a + b · fS + c · fS2 ),
and the growth restriction factor Q equals the value b [34]. Fig. 2(c)
shows the result of the calculation using V0.25 as an example. The
calculated Q values of Vx NbMoTa RHEAs are shown in Fig. 2(d). It
can be seen that values of Q increase significantly as the V content
increases, which means that V can be considered to be the solute
in the pseudo-binary system V-NbMoTa that effectively limits the
growth of grains. The solutal effect of V is also supported by the
segregation of V shown in Table 2 and Fig. 1(e), i.e. V is rejected
into the liquid as the solid grows, corresponding to its higher con-
tent in the interdendritic region. Schematics in Fig. 2(e) illustrate
the mechanism of the grain refinement induced by V. In the al-
loy of higher V concentration, a shorter growth distance (Rg ) of
the solid would generate a steeper concentration profile of V in
the liquid ahead of the interface, which induces a higher constitu-
tional undercooling and therefore, triggers more nucleation events.
Meanwhile, the distance (w∗ ) from the dendrite tip (i.e. the solid-
liquid interface) to where the free growth of other nuclei could oc-
cur (i.e. reaching the critical undercooling Tfg ) is much shorter for
the alloy of higher V concentration, which suppresses the growth
of the grain and contributes to the grain refinement.
It was found that the grain size can be related to the solute
content by a semi-empirical relationship d = a + b/Q [35], where
d is the grain size and a and b are constants. Using the measured
mean grain sizes and calculated Q, a and b can be calculated as -
100 and 24750 respectively. The relationship between Q and the V
content c in mass fraction (as shown in Fig. 2(d)) can be described
by a parabolic function Q = 15.77 + 277c + 850c2 if we extend the
data to higher and lower V concentrations, as shown in the Supple-
mentary Information. Therefore, combing these two equations, the
relationship between the V content and the grain size of Vx NbMoTa
134 M. Wang, Z.L. Ma, Z.Q. Xu et al. / Scripta Materialia 191 (2021) 131–136

Fig. 2. (a) Grain sizes and (b) TCS -fS curves of Vx NbMoTa (x = 0.25, 0.5, 0.75, 1.0) RHEAs. (c) Calculation of the growth restriction factor Q using V0.25 RHEA as an example.
(d) Q in Vx NbMoTa as a function of V contents. (e) Schematic diagrams show how constitutional undercooling (Tcs ) influences the nucleation and grain growth in alloys
of high and low V contents. The blue, green, and orange curves correspond to profiles of the V concentration, liquidus temperature (TL ), and actual temperatures (TA ) in the
liquid in front of the solid-liquid interface (i.e. the dendrite tip) respectively. The dashed circle indicates the envelope beyond which the constitutional undercooling exceeds
the critical undercooling Tfg . Therefore, the nucleants within the envelope (red particles) are inactivated and only those out of the envelope can be triggered.

RHEAs can be described by the Eq. 2:
d = −100 + 24750/(15.77 + 277c + 850c ) 2
(2)
Maintaining the phase stability in a broad temperature range
during a prolonged service time is crucial for applications of RHEAs
at high temperatures [16]. Some RHEAs have a single-phase struc-
ture at the as-cast condition but phase transformation can occur
during heat treatment [5,13,36]. For instance, HfNbTaTiZr has a sin-
gle BCC structure at the as-cast condition and after heat treatments
(10 0 0°C~140 0°C), but it decomposes into two phases (BCC matrix
and BCC Ta-Nb rich precipitates) or three phases (BCC matrix, BCC
Ta-Nb rich precipitates, and HCP Zr-Hf rich precipitates) after an-
nealing at 50 0–90 0°C [16,36–40]. After annealing above 1400°C,
this alloy was also reported to decompose into three phases (BCC)
matrix, FCC1 Zr-Hf-Ti rich precipitates, and FCC2 Zr-Hf-Ti rich pre-
cipitates) [41]. Fig. 1(a) shows that V-NbMoTa (0–30 at %) alloys
can exhibit a single BCC phase at a wide temperature range (2300–
500°C), which indicates that this alloy should possess good phase
stability. To test this anticipation, V1.0, which has the highest V
contents and the highest predicted secondary-phase precipitation
temperature (451°C as shown in Fig. 3 (a)) among the four stud-
ied alloys was heat-treated at 1250°C and 350°C (i.e. ~100°C lower
than the predicted precipitation temperature). The heat-treatment
profiles are shown in Fig. 3 (b). For the 1250°C case, samples were
held at 1250°C for 1 day and quenched to room temperature. For
the 350°C heat treatment, samples were first soaked at 1250°C for
3 days, then cooled (10°C/min) to 800°C and held for 7days, and fi-
nally cooled to 350°C and held for 30 days. The previous two steps
at higher temperature are to promote atomic motion to facilitate
the phase transformation (if there is any), since it would be ki-
netically inert for the alloy to undergo phase transformation if it
was directly held at 350°C. Fig. 3(c) shows XRD patterns of V1.0
at different conditions, indicating that as-cast and heat-treated al-
loys all exhibit the same single BCC phase structure without phase
transformations, though the secondary phase is predicted to form
at 350°C (Fig. 3(a)). The absence of the phase transformation at
350°C is probably due to i) the low diffusivities of refractory el-
ements in RHEAs that are commonly reported [8] and also evi-
denced by segregations in dendrites as shown in Fig. 3(d)–(f), and
ii) the inaccuracy of the CALPHAD simulation for the incomplete
thermodynamic description (full assessment) of all binary and, es-
pecially, ternary systems that essential for building higher-order
systems [42]. Microstructures of V1.0 alloy after heat treatments
still exhibit dendrites (Fig. 3(d) and (e)) similar to Fig. 1(c), and
Fig. 3(f) shows the segregation ratios of all elements are weakened
but not eliminated, which could all attribute to the sluggish diffu-
sion featured by this alloy.
Fig. 4(a) compares yield strengths of 67 RHEAs reported by
far [9,43,44]. V1.0 alloy in this study is represented by the red
dot symbol. It can be seen that the yield strength of V1.0 at
RT (1256 MPa) is not outstanding compared with other RHEAs.
However, as the temperature increases, the yield stress of V1.0
exceeds those of most other RHEAs, indicating that V1.0 al-
loy has stronger resistance to high-temperature softening com-
pared with other RHEAs. At 10 0 0°C, the yield strength of V1.0
(811 MPa) is only lower than four RHEAs (in the blue rectan-
gle), i.e. MoNbTaVW [7], HfMoTaTiZr [13], HfMoNbTaZr [44], and
AlMo0.5 NbTa0.5 TiZr0.5 [45]. Nevertheless, Fig. 4(b) (at the upper
right corner of (a)) shows that V1.0 alloy has the RT fracture strain
>25% that is superior to other four RHEAs, especially MoNbTaVW
and AlMo0.5 NbTa0.5 TiZr0.5 (fracture strains ~2%), indicating V1.0
possesses much better RT ductility/workability. Fig. 4(c) further
compares the stress-strain curves of the five alloys at 10 0 0°C.
MoNbTaVW exhibits the highest yield stress and flow stress but
much lower ductility. AlMo0.5 NbTa0.5 TiZr0.5 , HfMoTaTiZr, and Hf-
MoNbTaZr show high yield strength and good ductility but ex-
hibit significant strain-softening after yielding (or as increasing the
strain), which is obviously inferior compared with V1.0 that fea-
tures the ultimate strength as high as ~1.4 GPa and no strain soft-
ening.
In summary, novel Vx NbMoTa RHEAs with varied V concen-
trations were explored in this study. Vx NbMoTa alloys exhibit a
single-phase BCC structure and possess unprecedented phase sta-
bility in a wide temperature range from 350°C to the solidus
 M. Wang, Z.L. Ma, Z.Q. Xu et al. / Scripta Materialia 191 (2021) 131–136 135

Fig. 3. (a) Solidification path of V1.0 RHEA. (b) Heat treatment profiles. (c) XRD patterns and (f) segregation ratios of V1.0 RHEA at different conditions. SEM images of V1.0
RHEA after heat treatments at (d) 1250°C and (e) 350°C.

Fig. 4. (a) Yield strengths of V1.0 RHEA and 67 RHEAs reported by far at different temperatures. Data are from references [9,43,44]. (b) Yield strengths at 10 0 0°C versus
fracture strains at RT of alloys in the blue rectangle in (a). Stress-strain curves (10 0 0°C and 10−3 s−1 ) of the five alloys are further compared in (c).

temperature. The grain structure of the alloy can be signif- Acknowledgments

icantly refined as increasing the V concentration due to the
strong solutal effect of V that contributes to higher growth
restriction factors at higher V contents. Compared with most
RHEAs reported by far, equimolar VNbMoTa exhibit superior high-
temperature strength and excellent room-temperature ductility,
and it even shows no stain-softening (at high temperature up to
10 0 0°C) that is rarely seen in other popular RHEAs, highlight-
ing that this alloy could be very promising for high-temperature
applications.
We acknowledge National Natural Science Foundation of China
(NSFC) grant number 51804032 and China Postdoctoral Science
Foundation grant number 2018M640076 for financial supports.
Supplementary materials
Supplementary material associated with this article can be
found, in the online version, at doi:10.1016/j.scriptamat.2020.09.
027.

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