Journal of the European Ceramic Society 40 (2020) 2504–2508

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Journal of the European Ceramic Society

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Short communication

Ultrafast synthesis of entropy-stabilized oxide at room temperature T

a a b,c, b,c d e
Dianguang Liu , Xinyu Peng , Jinling Liu *, Liying Chen , Yong Yang , Linan An
a
School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu, Sichuan 610031, China
b
State Key Laboratory of Traction Power & School of Mechanics and Engineering, Southwest Jiaotong University, Chengdu, Sichuan 610031, China
c
Applied Mechanics and Structure Safety Key Laboratory of Sichuan Province, Southwest Jiaotong University, Chengdu, Sichuan 610031, China
d
Department of Mechanical Engineering, City University of Hong Kong, Tat Chee Avenue, Kowloon Tong, Kowloon, Hong Kong Special Administrative Region
e
Department of Materials Science and Engineering, University of Central Florida, Orlando, FL 32816, USA

A R T I C LE I N FO A B S T R A C T

Keywords: Five-component entropy-stabilized oxide ceramic (Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O) has been successfully synthesized
Entropy-stabilized oxides by reaction assisted flash sintering at room temperature. Compared to the conventional sintering technique, the
Flash sintering starting materials have been completely transformed to a single rocksalt phase in just a few seconds. Analysis
Phase transformation suggests that the electric field significantly accelerated the rate of phase transition. These results clearly de-
Rocksalt
monstrate the feasibility of employing the reaction assisted flash sintering technique to fabricate entropy-sta-
bilized oxides with new chemistries and attractive properties.

Entropy-stabilized oxides (ESOs) are homogeneous single-phase
solid solutions, where four or more metallic atoms, in equimolar
amounts, are randomly arranged on crystalline lattice [1]. Similar to
the idea of high entropy alloys (HEAs) [2–5], the ESOs are believed to
be stabilized due to a relatively high configurational entropy of mixing,
which can be maximized by mixing a number of diverse elements. In
2015, Rost et al. synthesized the first ESO, which is a single phase
rocksalt-structured Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O [1]. Since then, various
ESOs with different structures and compositions have been developed
[6–12]. It has been demonstrated that ESOs presented notable lattice
distortion [13,14], and produced the attractive properties, such as the
colossal dielectric constant [15], lithium superionic conductivity [16],
reversible lithium storage [17], and magnetic properties [18].
In the prior works, solid-state diffusion processes were employed to
synthesize ESOs, where starting binary oxide powders were mixed and
sintered at high furnace temperature [1,6–12]. However, several to tens
of hours are required to synthesize single-phase ESOs by conventional
sintering with high furnace temperature [1,6–12]. Other techniques,
such as nebulized spray pyrolysis (NSP), flame spray pyrolysis (FSP),
and reverse co-precipitation (RCP), have also been employed to syn-
thesize ESOs [19]. NSP and FSP offer faster processing due to short
precursor/particle residence time and rapid quenching. However, these
techniques can only produce nanopowders, but bulk entropy-stabilized
oxide ceramics cannot be made by these processes.
Recently, it has been demonstrated that a critical electric field ac-
celerated phase transition during flash sintering, and also lead to
densification at low furnace temperatures [20–29]. Herein, we first
report the bulk entropy-stabilized Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O was syn-
thesized in ultrashort time by the method of reaction assisted flash
sintering at room temperature.
The NiO (Shanghai Naiou Nanotechnology Co., Ltd, 99.9 %), CuO
(Shanghai Naiou Nanotechnology Co., Ltd, 99.9 %), Co3O4 (Shanghai
Naiou Nanotechnology Co., Ltd., 99.9 %), MgO (Xuan Cheng Jing Rui
New Materials Co., Ltd, 99.9 %) and ZnO (Xuan Cheng Jing Rui New
Materials Co., Ltd, 99.9 %) nanopowders were used as raw materials in
this study. The received nanopowders with the molar ratio of NiO : CuO
: MgO : ZnO : Co3O4 = 3 : 3 : 3 : 3 : 1 were uniformly mixed in distilled
water by planetary ball milling (ND8−4 L, Nanjing Nanda Tianzun
electronic Co., Ltd., China) at 150 rpm for 12 h using ball to powder
weight ratio of 12.8 : 1. The slurry was baked at 95 °C in the oven. Then,
the powder mixture was ground in an agate mortar, and subsequently
was pressed into dog bone-shaped compacts by uniaxial pressing at 25
MPa, followed by cold isostatic pressing at 290 MPa. The compacts
were pre-sintered at 500 °C for 2 h in the air with the heating rate of 2
°C/min from room temperate using box furnace (KSL-1200X, KJ Group,
Anhui, China), to remove the binder and improve the mechanical
strength of green bodies, and then the samples were cooled down to 300
°C with the rate of 5 °C/min before turning off the furnace. Finally, a
hole, with a diameter of 1.6 ± 0.1 mm, was drilled on each end of the
pre-sintered pellets for electrical connections. The measured relative
density of the pre-sintered green bodies is around 55 %.
The pre-sintered sample was connected to platinum wires via the

⁎
Corresponding author at: State Key Laboratory of Traction Power & School of Mechanics and Engineering, Southwest Jiaotong University, Chengdu, Sichuan
610031, China.
E-mail address: liujinling@swjtu.edu.cn (J. Liu).

https://doi.org/10.1016/j.jeurceramsoc.2020.01.018
Received 28 November 2019; Received in revised form 7 January 2020; Accepted 8 January 2020
Available online 10 January 2020
0955-2219/ © 2020 Elsevier Ltd. All rights reserved.
D. Liu, et al. Journal of the European Ceramic Society 40 (2020) 2504–2508

holes, platinum paste was applied between the platinum wires and the
holes to minimize contact resistance. Then, the pre-sintered sample
placed onto a heating plate (CHPS 250DN, ASSRE, Japan), keeping the
specimen surface parallel to the heating plate. The temperature of the
heating plate was set to 30 °C, which gives the temperature of the
specimen to be ∼ 25 °C. After stabilizing at 30 °C for 20 min, the
electric field was applied on the specimen by a DC power source (APS
DCP1200V-1A, Adaptive Power System, CA). The sample was held for
60 s after the current density reached the maximum value. The power
to the sample was then disconnected, and the sample was directly
quenched in ice water. The temperature of the specimen surface was
measured using a thermal imaging camera with spectral range 7.5–13.0
μm (A600, FLIR system Inc., Sweden). To calibrate the camera, the
surface temperature of the heated sample without electric field applied
had been measured by the camera and a thermocouple that was at-
tached the sample surface. The result gives the reflection coefficient of
the specimen to be 0.98 and the accuracy of the temperature mea-
surement to be ± 2 °C. Fig. 2. The temperature evolution along the gauge length as a function of time.
Then, a fast firing method has also been employed to investigate the The flash sintering is conducted at room temperature with the electric field of
phase transformation [30]. The experiments were carried out in a tube 250 V/cm and current density limit of 80 mA/mm2.
furnace in air with a steady state temperature of 875 °C, same as the
previous flash sintering. To obtain the highest heating rates possible in
high as 3530 V/cm [33]. In addition, the onset temperature was re-
the experiments (the estimate heating rate is about 65 °C/s below 900
duced when increasing the conductivity of the sample by changing the
°C), the pre-sintered sample, which was connected to a platinum wire
atmosphere [32,34]. Here, we first discovered the mixed ZnO with
via one of the hole, was inserted into the center of the tube furnace from
other powders can be flash sintered at room temperature with the
outside rapidly. After sintering for 180 s or 300 s at the steady state
electric field as low as 240 V/cm, about one fifteenth compared to
temperature, the sample was directly quenched in ice water.
previous report [33]. We believe that the onset of flash event is arising
The crystal structure of the center of resulting samples were ana-
from the increased electronic conductivity of the sample [35]. It seems
lyzed by X-ray diffractometer (XRD, PANalytical Empyrean,
the mixed p-type semiconductor (NiO, CuO and CoO) powders in-
Netherlands), which equipped with Cu Kα source. The polished surface
creased the conductivity of the samples with applied electric field at
was characterized by scanning electron microscopy (SEM, JSM-7800F
room temperature, and resulted in the flash sintering was initiated at
Prime, JEOL, Japan), and the selected area was analyzed using energy
lower conditions. After the power surge, the power density immediately
dispersive spectroscopy (EDS,OXFORD X-Max 80, England) to identify
decreased, and then it kept at a relative stable level, which is similar to
the compositional uniformity. The crushed powders from the center
the flash sintering of other materials [20–28].
part of the flash sintered sample were analyzed by transmission electron
One should note that the sample temperature should be higher than
microscopy (TEM, JEOL 2100 F, Japan) with energy dispersive spec-
room temperature due to Joule heating after the incubation stage.
troscopy (EDS).
Hence, the temperature evolution along the gauge length as a function
Fig. 1 shows the plots of applied field, current density, power dis-
of time was monitored by thermal imaging camera during flash sin-
sipation, as a function of time. Apparently, flash sintering occurred
tering (see Fig. 2, the full video was uploaded as Supplementary in-
even at room temperature, as indicated by the existence of a power
formation). It is seen from Fig. 2 that the temperature in the gauge
dissipation surge. Pure ZnO was flash sintered above 650 °C with
length showed rapid temperature rise, which concurs with the power
electric field of 80 V/cm in air [31]. When the electric field increased to
surge. After the power dissipation reached steady stage, the tempera-
300 V/cm, the initial furnace temperature decreased to 600 °C in air
tures are also stabilized. As shown in Fig. 2, the temperature distribu-
[32]. Although the flash event of ZnO was observed at room tempera-
tion at steady stage is nonuniform on the surface of the sample. It in-
ture in air recently, the applied alternating current (AC) field was as
dicates the highest temperature is located near the cathode of the
sample at the beginning of steady state. Then, the high temperature
zone occurs at the center of the sample, which is different from the
asymmetric temperature distribution on 8YSZ [36]. The measured
temperature at the center of the sample at the steady stage is about 875
°C, which is lower than the value (991 °C) estimated by black body
radiation model [37], when using the emissivity of 1. In addition, the
low temperature zone is observed between the anode and the middle
point of the sample, as well as between the cathode and the middle
point of the sample. Now, the mechanism of the nonuniform tempera-
ture distribution is mystery, especially during synthesis the high en-
tropy oxides, but the internal reactions have been proposed to explain
the phenomenon in flash sintering [36,38,39], such as the forming of
oxygen vacancies under high electric field, the absorbing of electrons by
the vacancies, and the combining of electrons and holes at the steady
stage.
The phase transition during flash sintering and fast firing is studied
using XRD (Fig. 3). The current density limit has exhibited a significant
influence on the phase transition during flash sintering. The XRD pat-
Fig. 1. Plots of applied field, current density, and power dissipation as a
function of time for flash sintering at room temperature with the electric field of
tern of the sample, which is sintered at RT with current density of 70
250 V/cm and current density limit of 80 mA/mm2. mA/mm2, is similar to the pre-sintered sample with mixed rocksalt (R),

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D. Liu, et al.
Fig. 3. Typical XRD patterns of pre-sintered, flash sintered (FS), and fast fired
(FF) samples. Only the flash sintered sample shows single rocksalt (R) phase,
which is conducted at room temperature with the electric filed of 250 V/cm and
current density limit of 80 mA/mm2.
tenorite (T), and wurtzite (W) phases. However, the two peaks at 2θ =
75° and 78° is more obviously, as well as the intensity increasing of
other peaks belong to rocksalt phase, which indicates that the sample
was partially transformed to rocksalt structure from tenorite and
wurtzite phases. Further increase the current density to 80 mA/mm2, it
resulted in the oxide mixture completely transformed to the single-
phase rocksalt structure, all the peaks belong to tenorite and wurtzite
phases have been disappeared.
The sample, which was fast fired at 875 °C for 3 min, exhibits mixed
rocksalt (R), tenorite (T), and wurtzite (W) phases, but the intensity of
rocksalt (R) phase has increased compared to the pre-sintered sample. It
means the tenorite (T) and wurtzite (W) phases had transformed to the
rocksalt (R) phase partially, however, the phase transformation can’t
finish within 3 min due to the lower diffusion rate of cation at 875 °C.
When extending the holding time of fast firing experiment to 5 min at
875 °C, it seems the peaks belong to tenorite (T) and wurtzite (W)
Fig. 4. EDS elemental maps of Co, Zn, Cu, Mg, Ni for flash sintered samples at room temperature with the electric field of 250 V/cm and current density limit of 80
mA/mm2.
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Journal of the European Ceramic Society 40 (2020) 2504–2508
phases are not obvious. Almost all the tenorite (T) and wurtzite (W)
phases have transformed to the rocksalt (R) phase. Hence, only obvious
rocksalt (R) phase can be identified from the XRD patterns.
Although the highest temperature at the current density of 80 mA/
mm2 is slightly higher than the temperature range (850−900 °C) for
phase transition of Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O [1], the temperature at
the center of the sample is close to the phase transformation tempera-
ture. To be noticed, compared to the conventional sintering technique
[1], the time for full conversion to Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O by re-
action assisted flash sintering was in just a few seconds, which was two
orders of magnitude lower than the conventional sintering. The full
conversion time for flash sintering is also at least five times shorter than
fast firing.
It indicates that the phase transformation process, especially cation
diffusion, has been significantly accelerated due to the applied electric
field, which is in good agreement with previously published reports
[20–29]. It demonstrates the rapid heating rate during flash sintering
contribute to the accelerated mass transport partially [30]. However,
the detailed mechanism for this process is not uncovered fully. It be-
lieved the internal reactions and high concentration of oxygen va-
cancies under the applied electric field make contribution to this pro-
cess [36,38].
The surface morphology and compositional uniformity of the
sample sintered at room temperature has been characterized by SEM
with EDS maps, the results have been shown in Fig. 4. As can be seen,
the sample surface exhibits porous microstructure after flash sintering
at room temperature. It means the densification has not been finished
within 60 s. Hence, the density of the sample after flash sintering for 60
s is low in our experiments. The measured relative density is about 62
%. A uniform dispersion of the metal signals was observed in Fig. 4,
which indicates the homogeneity of element in the sintered samples.
Here, the formation of high entropy oxide is dominated by the cation
diffusion, it seems this process has finished at the early stage of den-
sification.
Furthermore, the crystalline structure and compositional uniformity
of the sample sintered at room temperature has been verified by se-
lected area electron diffraction (SAED) and EDS compositional maps
shown in Fig. 5. The insert image in Fig. 5a indicates the grains of the
flash sintered sample is belongs to rocksalt (R) phase, which is con-
sistent with the XRD pattern. The tenorite (T) and wurtzite (W) phases
have not been found in the test. As can be seen, a uniform dispersion of
these metal signals is observed, which indicated the homogeneity of the
D. Liu, et al.
Fig. 5. (a) The darke phase image of the grains from the center part of the flash sintered sample at room temperature with the electric field of 250 V/cm and current
density limit of 80 mA/mm2. The insert image shows the selected area electron diffraction (SAED) pattern of the grain edge, which is consistent with the rocksalt (R)
phase. EDS elemental maps of (b) Mg, (c) Co, (d) Ni, (e) Cu, (f) Zn for the grain of flash sintered sample.
sintered samples again. Therefore, a single solid solution phase, with
rocksalt structure, has been obtained by flash sintering in just a few
seconds at room temperature. It means the mixing of atoms is ac-
celerated by the applied electric field before fully densification.
We have demonstrated the ultrafast synthesis of five-component
entropy-stabilized oxide ceramic by flash sintering at room tempera-
ture. Under the current density of 80 mA/mm2, a single solid solution
phase, with rocksalt structure, has been obtained by flash sintering in
just a few seconds. The measured temperature by thermal imaging
camera is close to the temperature range for phase transition of
Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O by conventional sintering technology. The
ultrafast synthesis process indicates that the applied electric field ac-
celerated the cation diffusion. This work clearly demonstrates that re-
action assisted flash sintering is a very promising technique to synthesis
entropy-stabilized oxide ceramics.
Declaration of Competing Interests
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
This work was financially supported by the National Natural Science
Foundation of China [Grant Nos. 51672227, 51732009 and 51802271],
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Journal of the European Ceramic Society 40 (2020) 2504–2508
and the Fundamental Research Fund for the Central Universities [Grant
Nos. 2682018CX51 and 2682019LK04]. The research of YY is sup-
ported by the City University of Hong Kong [Grant Nos. 9610366 and
9610391].
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in the
online version, at https://doi.org/10.1016/j.jeurceramsoc.2020.01.
018.
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