Intermetallics 117 (2020) 106674

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Intermetallics
journal homepage: http://www.elsevier.com/locate/intermet

Oxide dispersion strengthened FeCoNi concentrated solid-solution alloys

synthesized by mechanical alloying
Yuanhang Guo a, Mingyang Li a, Cunguang Chen b, Pei Li b, Wuming Li a, Qingzhu Ji a,
Yanwen Zhang c, d, Yongqin Chang a, *
a
School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing, 100083, China
b
Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing, 100083, China
c
Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, 37831, USA
d
Department of Materials Science and Engineering, University of Tennessee, Knoxville, 37996, USA

A R T I C L E I N F O A B S T R A C T

Keywords: FeCoNi concentrated solid-solution alloys (CSAs) and its modified version strengthened by in-situ formed nano-
High-entropy alloys sized particles are successfully manufactured through mechanical alloying and spark plasma sintering method.
Alloy design Both the as-milled powders and the bulk materials are of single face-centered cubic structure. After sintering and
Dispersion strengthening
heat treatment, grains are refined by 68% with the addition of oxides. In oxide dispersion strengthened (ODS)
Mechanical properties
Mechanical alloying and milling
FeCoNi CSAs, the majority of nano-sized particles with diameter ranging from a few to ~ 40 nm are uniformly
Microstructure distributed in the matrix, and most of them are identified as Y2Ti2O7. Electron backscattered diffraction results
reveal that the recrystallization process is suppressed due to the existence of the nano-sized particles. The size
and distribution of oxide particles in the matrix can be controlled by adjusting experiment parameters of the
mechanical alloying process and annealing treatment. Refined grains and high-density nano-sized particles result
in enhanced compressive yield strength for ODS-FeCoNi CSAs at room temperature and 700 � C, which is 1295
MPa and 127 MPa, respectively.

1. Introduction the advantages of CSAs and ODS materials.

In recent years, concentrated solid-solution alloys (CSAs), including
high entropy alloys (HEAs), have attracted increasing interest because of
their excellent properties, such as high strength, high hardness, good
oxidation and corrosion resistance [1,2]. Moreover, CSAs are also
promising candidates as alternative structural materials with
outstanding irradiation-resistance because of their high atomic-level
stresses [3] and chemical complexity [4–8]. It was reported that grain
boundaries and interfaces in diluted alloys can act as sinks for
irradiation-induced defects, leading to improved irradiation resistance
[9,10]. Due to the extreme chemically complexity from reported work in
CSAs [4–8], grains in CSAs are expected to be stable, and the quantities
of the interfaces between the matrix and particles may be increased
accordingly [11]. It is therefore projected that, as nano-sized oxide
particles are introduced into CSAs, the resulting oxide dispersion
strengthened (ODS) concentrated solid-solution alloys (ODS-CSAs) may
exhibit substantial performance improvement in extreme environments.
Such ODS-CSAs may possess superior performance because it combines
For ODS-CSAs, two kinds of nano-sized oxide particles, Y2O3 and
Al2O3, were mainly used in previous research. H. Hadraba et al. [11]
reported that grain size of CoCrFeNiMn was refined 50% by adding 0.3
wt% oxide particles. For ODS-CoCrFeNiMn, the ultimate tensile strength
and the yield strength increased by 30% and 70% at room temperature
and 800 � C, respectively. S. Praveen et al. [12] reported that the hard­
ness of AlCoCrFe HEAs increased from 1050 � 20 HV1 to 1070 � 20 HV1
because of the addition of oxide particles, and it was suggested that the
contribution from solid solution strengthening effect overwhelmed the
effect of oxide dispersion on hardness in AlCoCrFe HEAs. B. Gwalani
et al. [13] reported that compressive yield strength increased from 979
MPa to 1759 MPa for Al0.3CoCrFeMnNi HEAs with the introduction of 3
vol% Y2O3. The significant increase in strength was ascribed to the
nano-dispersoid strengthening coupled with grain refinement. X.Y. Liu
et al. [14] found that the tensile strength of CrMnFeCoNi HEAs increased
from 868 MPa to 1001 MPa due to the addition of 0.25 wt% Y2O3, and
ODS-CrMnFeCoNi HEAs also showed excellent wear-resistance. B. Jia
et al. [15] reported that the yield strength increased from 654 MPa to

* Corresponding author.
E-mail address: chang@ustb.edu.cn (Y. Chang).

https://doi.org/10.1016/j.intermet.2019.106674
Received 17 December 2018; Received in revised form 9 May 2019; Accepted 3 December 2019
Available online 9 December 2019
0966-9795/© 2019 Elsevier Ltd. All rights reserved.
Y. Guo et al.
Fig. 1. SEM images of FeCoNi CSAs, (a) raw powders, (b) as-milled powders, (c) bulk materials and the corresponding images of ODS-FeCoNi CSAs, (d), (e), and (f).
1754 MPa for FeCrCoNi HEAs strengthened by 5 wt% Y2O3 particles.
Analyses on the synergic effects of grain size hardening and particle
strengthening indicate that the addition of nano-scaled oxides is an
effective and suitable way to design HEAs with superior mechanical
properties.
Ł. Rogal et al. [16] found that compressive yield strength increased
from 1180 MPa to 1600 MPa with 5 wt% additions of α-Al2O3
nano-particles into CoCrFeMnNi composites. S.F. Yang et al. [17] re­
ported that Al0.4FeCrCo1.5NiTi0.3 HEAs reinforced with 8 wt% nano-­
Al2O3 particles showed excellent compressive properties. The yield
strength, fracture strength and compressive ratio were 2.05 � 0.01 GPa,
2.14 � 0.01 GPa and 13.98 � 0.25%, respectively. H. Prasad et al. [18]
studied FeNiCoCrAlMn HEAs dispersed with 2 wt% alumina. They found
that AlNi and CrFeMn rich phase increased after sintering and less
thermal expansion coefficient and better oxidation resistance in
ODS-FeNiCoCrAlMn HEAs.
In the previous studies, the ODS-CSAs of interests were usually
focused on the quaternary or quinary alloys [11–18] and researches on
ODS ternary alloys have not been carried out yet. High-temperature and
high-fluence irradiation experiments suggested that the improved radi­
ation resistance depends critically on the type alloying elements, and
some HEAs containing 4 or more elements may not intrinsically better
than some medium entropy alloys (MEAs), e.g., ternary CSAs [19–22]. It
is therefore highly desirable to investigate the radiation perform of
ODS-MEAs or in a more general term ODS-CSAs. Up to now, several
groups have reported CSAs strengthened by Y2O3 particle or its modified
version [11–15]. For ODS-CoCrFeNiMn, yttrium oxide dispersoids were
introduced into the matrix by adding of O2 gas, Y and Ti powders during
mechanical alloying (MA) process [11]. For ODS-AlCoCrFe, Ti and Y2O3
were synthesized separately and blended together with as-milled
AlCoCrFe HEA powders to produce oxide dispersed HEA powders
[12]. Furthermore, Electron backscattered diffraction (EBSD) technique
was used in ODS-CoCrFeNiMn to observe the grain morphology and
determine the average grain size [11]. But the characteristic of grain
boundaries has not been investigated. As one of the main sources for
high strength in ODS-CSAs, crystal structure and particle size distribu­
tion of nano-sized oxide particles in the matrix also have not been fully
analyzed [11–15]. In this work, nano-sized oxide particles were intro­
duced into FeCoNi based ternary alloys by mechanical alloying. Y2O3, Ti
and other raw powders were blended simultaneously and then
nano-sized Y–Ti–O particles precipitated from the matrix during spark
plasma sintering (SPS) and annealing process, as such the average
diameter, stoichiometry and distribution of oxide particles could be
controlled by adjusting experiment parameters. The characteristic of
grain boundaries were observed using EBSD technique to investigate the
grain growth process. Chemical compositions and crystal structures of
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Intermetallics 117 (2020) 106674
the nano-sized oxide particles were also systematically analyzed. In this
work, ODS-FeCoNi CSAs were designed as the candidate structural
materials serving in generation Ⅳ fission systems or nuclear fusion re­
actors, so compression test were conducted at room temperature and
700 � C [23] to evaluate the mechanical properties at surveying
temperature.
2. Materials and methods
High purity Fe, Co, Ni, Ti and Y2O3 powders were blended with the
nominal chemical composition FeCoNi (FCN) and FeCoNi–2Ti–2Y2O3
(ODS-FCN) in a planetary ball-miller (MITR-YXQM-2L) for 80 h at 350
rpm in argon atmosphere. Stainless steel vials and balls were used as
milling media with the ball-to-powder mass ratio of 15:1. N-heptane was
introduced as processing controlling agent (PCA) to prevent cold
welding and metal oxidation. The as-milled powders were consolidated
by SPS at 1100 � C for 8 min under 50 MPa in vacuum, and then annealed
at 850 � C for 48 h in argon atmosphere.
Average particle size of the as-milled powders was measured by laser
particle size distribution analyzer (LPSDA, LMS-30). Phase structure of
the as-milled powders and bulk materials was analyzed using X-ray
diffraction equipment (XRD, Rigaku D/max-Rb) with CuKα radiation (λ
¼ 0.15406 nm). The metallographic analysis was observed using scan­
ning electron microscopy (SEM, ZEISS-EVO 18). Grain size and bound­
ary observation were carried out by auger electron spectrometer (AES,
ULVAC-PHI 710). Microstructures and nano-sized oxide particles were
analyzed by using transmission electron microscopy (TEM, FEI Tecnai
F20 and JEOL JEM-2010F) with energy dispersive spectrometer (EDS)
system. The TEM samples were prepared by ion-beam thinning. Density
of the bulk materials was examined using Archimedes’ principle. The
compression tests were performed at room temperature (RT) and at 700
�
C using cylindrical samples with nominal dimensions of 8 � 12 mm (d
� h) and strain rate of 1 � 10 3 s 1. Compression test at RT was carried
out using an electromechanical testing system CMT4305. Compression
test at 700 � C was employed using a high temperature testing system
MTS Landmark6 with a heating furnace. Hardness measurements were
conducted using a Vickers hardness tester (401MVD Wolpert Wilson
Instruments™) at a load of 1.96 N for a loading time of 15 s and twenty
indentations were performed and averaged.
3. Results and discussion
Typical SEM images of the raw powders, as-milled powders, and bulk
materials of FCN and ODS-FCN CSAs are shown in Fig. 1. Fig. 1a and
d shows the raw powders with different morphologies. The as-milled
powders are in spherical or ellipsoidal shape with the average
Y. Guo et al. Intermetallics 117 (2020) 106674

Fig. 2. XRD patterns of the raw powders, as-milled powders and bulk materials of (a) FeCoNi and (b) ODS-FeCoNi CSAs.

Fig. 3. EBSD diagrams of FeCoNi CSAs, (a) inverse pole figure map, (b) grain boundary misorientation map, (c) grain size distribution and the corresponding di­
agrams of ODS-FeCoNi CSAs, (d), (e), and (f).

diameter of 15.20 � 0.12 and 14.12 � 0.29 μm, respectively (Fig. 1b and
e). The bulk materials shown in Fig. 1c and f reveal that the powders are
successfully solidified, and only a few holes are detected. The bulk
density is around 94.4% and 92.7% of the theoretical value for FCN and
ODS-FCN CSAs, respectively.
Fig. 2 represents the XRD spectra of the raw powders, as-milled
powders and bulk materials for FCN and ODS-FCN CSAs. Selected
metals are detected in the raw powders for both materials. After milling
for 80 h, all the diffraction peaks belong to an face-centered cubic (FCC)
structure, and the diffraction peaks of the pure metal disappear for both
materials, indicating the raw powders are fully alloyed during the MA
process. For as-milled powders of FCN CSAs, broad diffraction peaks and
weak diffraction intensity are detected, which means large amount of
internal stress and defects are introduced in the lattice during the MA
process. Similar phenomenon was observed in ODS-FCN CSAs (Fig. 2b),
but the strongest diffraction peak of the as-milled powders for ODS-FCN
CSAs (2θ ¼ 43.541� ) is smaller than that of FCN CSAs (2θ ¼ 43.680� ),
which means larger interplanar spacing and greater lattice distortion
exist in ODS-FCN powders. The increasing interplanar spacing and lat­
tice distortion may result from the addition of titanium and yttrium
atoms because the radius of Ti and Y is larger than that of Fe, Co and Ni.
After sintering and annealing processes, all the diffraction peaks belong

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Y. Guo et al. Intermetallics 117 (2020) 106674

Fig. 4. (a) TEM image of FeCoNi CSAs, (b) the corresponding SAED patterns.

Fig. 5. TEM images of ODS-FeCoNi CSAs, (a) grain morphology, (b) SADP of position 1, (c) SADP of position 3, (d) HAADF-STEM image of the matrix, (e) size
distribution of the particles in the matrix.

to FCC structure for both materials, and the peak intensity increases
dramatically. The reason may be that defects introduced during MA
process decreases, grain coarsens and internal stress releases after so­
lidification and heat treatment. Full width at half maxima (FWHM) of
diffraction peaks decrease, indicating that the crystalline of these ma­
terials increases. After SPS and annealing treatment, the strongest
diffraction peak shifts to higher Bragg angle for both materials.
Compared with FCN CSAs, the value of Bragg angle for ODS-FCN CSAs is
still smaller, which indicates that the interplanar spacing and lattice
distortion still exists.
The inverse pole figure (IPF) map, grain boundary misorientation
map and grain-size distribution of FCN and ODS-FCN CSAs are shown in
Fig. 3. In Fig. 3a, grains with random orientation exist in FCN CSAs with
the average size of 735 � 405 nm. In Fig. 3b, high angle grain
boundaries (HAGBs) (misorientation >15� ) are represented by dark
lines and low angle grain boundaries (LAGBs) (15� > misorientation
>2� ) are marked by red lines. The fractions of HAGBs and LAGBs are
61.4% and 38.6%, respectively. LAGBs are usually observed in small
grains, and these subgrains annex adjacent grains to grow up by
reducing the area of small angle interface and lowering the stored en­
ergy (Position 1). HAGBs are mainly detected in the coarse grains along
with twin structures (Position 2). Fig. 3d shows that the grains are highly
refined in ODS-FCN CSAs, and the average grain size is 237 � 99 nm. A
large number of LAGBs is observed in ODS-FCN CSAs with the number
fraction of 45.8%, which is higher than that in FCN CSAs (38.6%).
During the annealing process, grains coarsen and LAGBs transform to
HAGBs (Fig. 3b), but the movement of grain boundaries is effectively
hindered by these nano-sized oxides, which causes high number fraction

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Y. Guo et al. Intermetallics 117 (2020) 106674

Fig. 6. (a) HAADF-STEM image of the nano-sized particles in ODS-FeCoNi CSAs and five typical points were chosen to quantitatively analyze the content and
ingredient of different elements, EDS elemental maps of (b) Fe, (c) Co, (d) Ni, (e) Y, (f) Ti, (g) O, (h) C, (i) Ti þ Y, (j) all elements.

Table 1
Chemical composition (in wt.%) of the different particles in ODS-FeCoNi CSAs.
wt.% Fe Co Ni Y Ti O

Base metal Point. 1 33.8 34.1 31.4 0.0 0.2 0.4

Type I Point. 2 33.6 32.8 19.1 3.5 4.5 6.5
Point. 3 1.4 1.4 1.1 18.9 33.9 37.3
Point. 4 29.6 29.6 29.0 2.5 2.6 6.7
Type II Point. 5 1.3 1.3 1.2 – 49.2 42.3
Point. 6 12.0 12.5 11.4 4.7 33.7 25.8

of LAGBs (Fig. 3e). Xu et al. [24] observed the similar phenomena in

ODS steel annealed at 900 � C.
Typical TEM image of FCN CSAs is shown in Fig. 4. Coarse grains and
low dislocation density are observed in FCN CSAs. Twin structures are
detected in the matrix (marked by green circles), which may be formed
during the blending and annealing process. The corresponding selected
area electron diffraction (SAED) patterns of Position 1 are shown in
Fig. 4b. Diffraction patterns belonging to the matrix are indicated by
white dashed lines, and the patterns of twin structures are marked by
green solid lines. Plane (111) is identified as the twinning plane in FCN
CSAs.
Fig. 5 shows a typical TEM image and the corresponding high-angle
annular dark field (HAADF) image of ODS-FCN CSAs. Refined grains are
detected in Fig. 5a. White particles marked by blue arrows are uniformly
distributed in the matrix. Twin structures marked by red circles (position
1 and position 2) are also observed. The corresponding SAED patterns of
position 1 are shown in Fig. 5b. Diffraction patterns assigning to matrix
are indicated by white dashed lines, and the patterns of twin structures
are marked by red solid lines. Plane (111) is also identified as the
twinning plane in ODS-FCN CSAs. The SADP of position 3 is shown in
Fig. 5c, and two sets of diffraction patterns are observed. One set is
confirmed as the matrix, marked by white solid lines. The other set is
identified as Y2Ti2O7 and marked by yellow solid line. The STEM image
of the matrix is shown in Fig. 5d, and the nano-sized particles with
different sizes are uniformly distributed in the matrix, which correspond
to the white particles in Fig. 5a. The histogram of particle size distri­
bution is shown in Fig. 5e. The diameter of these particles ranges from Fig. 7. HRTEM micrograph of the Y2Ti2O7 particles with diameters of (a) ~6
several nanometers to more than one hundred nanometer with an nm, (c) ~40 nm, (e) ~100 nm, and their corresponding FFT diagram (b), (d)
average value is 34.0 � 27.9 nm, but the majority is smaller than 40 nm. and (f).
Chemical compositions of the particles in selected area of the matrix
are analyzed by EDS mapping. Fig. 6a shows the HAADF image of the been fully decomposed during the SPS process. Fig. 6i shows that par­
matrix. The EDS maps shown in Fig. 6b–g indicate that the particles are ticles in the matrix are divided to two types: most of them are type I
enriched with the elements of Y, Ti, O and depleted of Fe, Co, Ni. Trace composed of Ti and Y, but a few type II are enriched with Ti. Fig. 6j
carbon observed in Fig. 6h indicates that carbon induced by PCA has contains all elements in the bulk materials. In order to quantitatively

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Y. Guo et al.
Table 2
Measured and calculated inter-planar distances of the nano-sized oxide particles
in Fig. 7a, c and e.
d(Å) d1{222} d2{400} d3{440}
Calculated 2.914 2.523 1.785
Particle in Fig. 7a 2.917 2.527 – boundary strengthening as well as dispersion strengthening.
Particle in Fig. 7c – 2.531 1.756
Particle in Fig. 7e 2.901 2.522 – movement during the plastic deformation as well as twin structures.
analyze the content and ingredient of different elements in the matrix
and particles, several typical particles from these two types (labeled in
Fig. 6a) are chosen, and the EDS results are listed in Table 1. It is found
that the matrix (Point 1) composes of Fe, Co and Ni. For the type I
particles, the concentration of Y is close to that of Ti (Points 2 and 4), or
Ti and Y are highly enriched (Point 3) compared with the base metal.
These particles are referred as Y–Ti–O particles. For the type II particles,
no any yttrium is detected (Point 5) or its concentration is much lower
than that of titanium (Point 6). These particles are supposed to be tita­
nium oxide.
In order to identify the stoichiometric ratio and crystal structure of
the Y–Ti–O particles in the matrix, around 30 particles with different
diameters are analyzed using high-resolution transmission electron mi­
croscopy (HRTEM). According to the particle size distribution histogram
in Fig. 5e, three representative particles with different diameters (~6
nm, ~40 nm and ~100 nm) are selected, and their corresponding fast
Fourier transformation (FFT) diagrams are shown in Fig. 7. Table 2
shows the measured and calculated inter-planar distances of these par­
ticles. The interplanar spacing and FFT results indicate that all these
particles are of Y2Ti2O7 with pyrochlore structure, which agrees with the
SAED results in Fig. 5c. The Y2Ti2O7 particle shown in Fig. 7a and e are
oriented with [011] zone axis to the electron beam, and the particle in
Fig. 7c is oriented with [001] zone axis. Fig. 7 shows that nano-sized
oxide particles with diameters from several nanometers to more than
one hundred nanometers have the same crystal structure and similar
chemical composition, which indicates that most of the yttrium and ti­
tanium precipitate from the matrix and form Y2Ti2O7 particles in the
ODS-FCN CSAs.
For conventional FCN CSAs fabricated by vacuum arc melting
(VAM), the average grain size is several tens of micrometers, and
hardness (HV) is 141.1 � 4.3 [25]. In this work, hardness is increased to
223.2 � 7.6 and 422.2 � 14.1 for FCN and ODS-FCN CSAs, respectively.
The increasing hardness for FCN CSAs mainly results from the refined
grains due to the MA method. For ODS-FCN CSAs, the grain sizes are
further refined with the addition of nano-sized oxides. Grain boundary
strengthening and dispersion strengthening result in enhanced hardness
Fig. 8. Compression stress-strain curves of FeCoNi and ODS-FeCoNi CSAs tested at (a) room temperature and (b) 700 C.
6
Intermetallics 117 (2020) 106674
in ODS-FCN CSAs. Compression stress-strain curves of FCN and
ODS-FCN CSAs, tested at RT and at 700 � C, are presented in Fig. 8. In
Fig. 8a, high yield strength with the value of 824 � 3 MPa is achieved for
the FCN CSAs. For ODS-FCN CSAs, the yield strength increase 57%. The
enhanced strength for ODS-FCN CSAs is mainly attributed to grain
High-density grain boundaries can effectively hinder the dislocation
Interaction between dislocations and nano-sized particles also contrib­
utes to the high strength of the ODS-FCN CSAs. In Fig. 8b, the
compressive yield strength for FCN and ODS-FCN CSAs at 700 � C is 104
and 127 MPa, respectively. This positive effect of in-situ formed oxide
particles reduced at evaluated temperature, explaining the shrinking
strength gap between FCN and ODS-FCN CSAs with increasing temper­
ature (from 57% at RT to 22% at 700 � C).
In this work, high energy introduced by collision among stainless
balls, tank wall and powders during the MA process results in mixing
and alloying of Fe, Co, Ni and Ti powders, and the simultaneously
decomposing of Y2O3 powders (Fig. 2b). During the sintering and
annealing processes, nano-sized oxide particles precipitate from the
matrix and most of them are in the form of Y2Ti2O7 (Figs. 6 and 7). It
means that the yttrium oxide particles are dissolved during the MA
process and then precipitate during the following consolidation process.
This kind of “dissolution-re-precipitation mechanism” has also been
observed in other ODS materials synthesized by MA methods [26,27].
4. Conclusion
In this paper, FCN and ODS-FCN CSAs are prepared by MA and SPS
method. Single FCC phase in both materials are obtained after MA
process. After sintering and annealing treatment, high-purity and high-
density bulk materials with FCC structure are achieved. EBSD results
reveal that the bulk materials compose of fine and equixed grains with
the average diameter around 237 nm in ODS-FCN CSAs, and its growth
are prevented by the nano-sized oxide particles, which hinder the
movement of the grain boundaries. In ODS-FCN CSAs, uniformly
distributed nano-sized oxide particles with diameter around 34 nm are
mainly composed of Y2Ti2O7. The extra titanium exists in the matrix in
the form of titanium oxide. Submicron grains and nano-sized particles
result in high compressive strength for ODS-FCN CSAs both at room
temperature and 700 � C, which is 1295 and 127 MPa, respectively.
Statement
The authors are requested to state that all authors have participated
sufficiently in this work to take public responsibility for it. All authors
�
Y. Guo et al.
have reviewed the final version of the manuscript and approve it for
publication. Neither this manuscript nor one with substantially similar
content under my (our) authorship has been published or is being
considered for publication elsewhere.
Acknowledgements
This work was supported by the National Natural Science Foundation
of China (No. 11775017, 11175014), the Fundamental Research Funds
for the Central Universities (FRF-GF-17-B5) and Beijing Municipal
Natural Science Foundation (No. 2162023). Prof. Y. Zhang was sup­
ported as part of the Energy Dissipation to Defect Evolution (EDDE), an
Energy Frontier Research Center funded by the US Department of En­
ergy, Office of Science, Basic Energy Sciences under contract number
DE-AC05-00OR22725.
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