Journal of the European Ceramic Society 41 (2021) 2855–2860

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Journal of the European Ceramic Society

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Ultrafast densification of high-entropy oxide

(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7 by reactive flash sintering
Hai-Rong Mao a, Rui-Fen Guo a, Yue Cao a, Shen-Bao Jin b, Xiao-Ming Qiu a, Ping Shen a, *
a
Key Laboratory of Automobile Materials (Ministry of Education), School of Materials Science and Engineering, Jilin University, No. 5988 Renmin Street, Changchun,
130022, PR China
b
Herbert Gleiter Institute of Nanoscience, School of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing, 210094, China

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

Keywords: Pyrochlore-type high-entropy oxides (HEOs) are usually sintered at high temperatures for a long time to achieve
High-entropy pyrochlore oxide (HEPO) full density. Herein, we synthesized pyrochlore-structured (La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7 HEOs with den­
Reactive flash sintering (RFS) sities up to 99 % at a furnace temperature of 1200 ◦ C in seconds via reactive flash sintering (RFS). The resultant
Mechanical property
HEOs achieved compositional uniformity at the atomic level and exhibited superior modulus, hardness and
fracture toughness compared to the counterparts prepared by conventional solid-state sintering (at 1600 ◦ C for
6 h). The underlying mechanisms for the ultrafast densification of the RFSed-HEOs were addressed in view of the
roles of electric field, rapid heating, external pressure and internal reactions.

1. Introduction (Ti0.2Y0.2Zr0.2Sn0.2Hf0.2)O3-x and (Bi0.2Na0.2K0.2Ba0.2Ca0.2)TiO3 perov­

Since Rost et al. first prepared a high-entropy oxide (HEO),
Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O, via solid-state sintering in 2015 [1], a series
of HEOs with unique thermophysical, mechanical and optical/elec­
trical/magnetic properties have been developed [2–5]. Among them,
high-entropy pyrochlore oxides (HEPOs) have attracted great attention
due to their extremely low thermal conductivities, high melting points
and sluggish grain growth rates [6–9]. However, these unique properties
also make the sintering of the HEPOs to full density via conventional
techniques rather difficult. For instance, Li et al. synthesized a
(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7 HEPO at 1500 ◦ C for 3 h and ob­
tained only 71.4 % relative density [8]. In contrast, Teng et al. [9]
prepared a nearly fully dense (La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7 HEPO
after sintering at 1500 ◦ C for 40 h.
An alternative method to prepare high-density HEOs is reactive flash
sintering (RFS). In recent years, RFS has been applied to synthesize
single-phase compounds by dissolving and densifying oxide mixtures or
amorphous phase precursors at lower temperatures [10–12]. Recently,
Yoon et al. [13], Liu et al. [14] and Kumar et al. [15], respectively, re­
ported the RFS of a rocksalt Mg0.2Ni0.2Co0.2Cu0.2Zn0.2O HEO, which can
readily be sintered to a high density by conventional solid-state sintering
at low temperatures (≤ 1050 ◦ C) [16]. More recently, Wang et al. [17]
and Liu et al. [18] have prepared high entropy Sr
skite oxide ceramics using RFS. To our knowledge, there are no reports
on the synthesis of dense HEPOs by RFS. In addition, despite that RFS
has been demonstrated to be an effective method for the synthesis of
high-entropy oxides, the mechanisms for the rapid densification remain
largely unclear so far.
In this work, we prepared a (La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7
(hereafter abbreviated as 5RE2Zr2O7) HEPO with a 99 % relative density
via RFS at 1200 ◦ C in seconds. The mechanical properties of the RFSed-
5RE2Zr2O7 HEPOs were evaluated by nano-indentation tests and
compared with those of the counterparts that were conventionally sin­
tered at 1600 ◦ C for 6 h. Besides, the mechanisms for the ultrafast
densification during the RFS process were addressed.
2. Experimental
Commercially available La2O3, Nd2O3, Sm2O3, Eu2O3, Gd2O3 and
ZrO2 powders (all in 99.9 wt% purity, D50 = 30 nm) were used as raw
materials. Firstly, stoichiometric amounts of the respective oxides for
the synthesis of 5RE2Zr2O7 were ball-milled for 60 min in a high-speed
three-dimensional pendulum ball-mill machine. The powder mixtures
with 2 wt% polyvinyl alcohol (PVA) as binder were cold pressed into
cylindrical pellets with sizes of φ 6 mm × 3.5 mm under a uniaxial
pressure of 400 MPa. The pellets were then pre-sintered at 600 ◦ C for 1 h

* Corresponding author.
E-mail address: shenping@jlu.edu.cn (P. Shen).

https://doi.org/10.1016/j.jeurceramsoc.2020.11.052
Received 13 August 2020; Received in revised form 24 November 2020; Accepted 29 November 2020
Available online 10 December 2020
0955-2219/© 2020 Elsevier Ltd. All rights reserved.
H.-R. Mao et al.
in air to remove the PVA binder. The relative density of the pre-sintered
samples was ~50 %. For the RFS, the pellet was placed between two
graphite electrodes in a boron nitride tube inside a graphite mold, as
schematically shown in Fig. 1(a). The furnace was evacuated to approx.
5 Pa and then heated to 1200 ◦ C at 10 ◦ C/min. After isothermal dwelling
for 15 min, an AC power (100 Hz) with a preset electric field strength (E,
9 V/mm) and a current density (I, within 60–200 mA/mm2) was applied
to the pellet. Once the flash was initiated, the AC power automatically
switched from voltage control to current control. A pressure of 10 MPa
was applied during the RFS process to ensure that the electrodes closely
contacted the sample. Finally, the sample was cooled at 20 ◦ C/min to
600 ◦ C and subsequently furnace-cooled to room temperature.
The densities of the sintered samples were determined by the
Archimedes method. The crystal structures of the polished RFSed sam­
ples (to remove the pollution from graphite) were identified by X-ray
diffraction (XRD, D/Max 2500PC, Rigaku, Japan). The microstructures
were observed by using a field emission electron microscope (FE-SEM,
JSM-6700 F, JEOL, Japan) and a transmission electron microscope
(TEM, JEM-2100 F, JEOL, Japan) equipped with an energy dispersive
spectrometer (EDS). The specimens for TEM were firstly mechanically
ground to a thickness of approx. 50 μm, and then ion-beam milled
(EMRES101, Leica, Germany) with a beam energy of 5 kV and an angle
of 10◦ . Furthermore, an atom probe tomography (APT) measurement
was performed with a local electrode atom probe instrument (LEAP
4000X Si, Cameca, USA) at a target specimen temperature of 40 K under
a pulsing UV laser with a pulsing energy of 60 pJ, a pulse rate of
200 kHz, and a detector efficiency of ~55 %. Needle-shaped APT sam­
ples were prepared by using a focused ion beam (FIB, Zeiss Auriga SEM/
FIB, Germany). Nano-indentation tests were carried out on a nano
indenter system (G200, KLA-Tencor, USA) with a Berkovich diamond
Fig. 1. (a) Schematic diagram of RFS device; (b) typical variations in electric field strength (E), current density (I) and power density (P) with time during RFS
process; (c) XRD patterns and (d) relative densities of the RFSed samples sintered under different current densities and the CSSed samples sintered at 1600 ◦ C for 3 h
and 6 h (The insert in (d) shows an image of the RFSed sample).
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Journal of the European Ceramic Society 41 (2021) 2855–2860
indenter at room temperature. The average of five measurements was
presented.
3. Results and discussion
Fig. 1(b) shows the typical variations in electric field, current and
power with time during the RFS process. After a short incubation period
(stage I), the current rapidly increased and the AC power changed from
voltage control to current control. Accordingly, the power showed a
sharp peak (stage II) and then rapidly decreased to a stable value (stage
III). At a current density of 120 mA/mm2, the peak power in stage II
reached 1115 mW/mm3. Such an instantaneous high peak power caused
rapid heating and cooling in the sample, which was beneficial to the
formation and stabilization of a high-entropy phase [13]. Note that the
electric resistance (E/I) of the sample was fairly stable in stage III,
implying that the primary densification might have been finished in
stage II, since the electrical resistance was closely related to sintering
density and temperature [11,19]. In addition, according to the feedback
from pressure sensor during the RFS process (Fig. S1), the sample un­
derwent rapid shrinkage during the peak power stage (stage II), con­
firming that the densification mainly occurred during this period (within
5 s).
XRD examinations (Fig. 1(c)) show that there was no significant
difference in peak patterns between the RFSed samples obtained under
different current densities and the conventionally solid-state sintered
(hereafter abbreviated as CSSed) samples, indicating that the crystal­
lographic phases formed in both cases were similar. According to liter­
ature [8], the 5RE2Zr2O7 HEPO product has a pyrochlore structure with
a lattice parameter of 10.625 Å. Here, the lattice parameters of the
as-prepared 5RE2Zr2O7 HEPOs were calculated to be in the range of
H.-R. Mao et al.
10.615–10.628 Å, consisting with the reported result.
Fig. 1(d) shows the sintered densities of the RFSed-5RE2Zr2O7 HEPOs
under different current densities together with those of the CSSed-
5RE2Zr2O7 HEPOs prepared at 1600 ◦ C for 3 h and 6 h (the theoretical
density of 5RE2Zr2O7 was reported to be 6.554 g⋅ cm− 3 [8]). The relative
density of the RFSed samples increased noticeably with increasing cur­
rent density, reaching 99 % when the current density was 200 mA/mm2.
For comparison, the relative density of the samples sintered in the same
furnace at 1200 ◦ C for 15 min but without the application of the AC
power was 62 % (the porous structure is shown in Fig. S2(a)). Never­
theless, a high-entropy pyrochlore phase had also formed (Fig. S2(b)),
suggesting that the formation of the HEPO phase is much easier than the
achievement of the high density. In contrast, the relative densities of the
CSSed samples reached 94 % and 97 % after sintering at 1600 ◦ C for 3 h
and 6 h, respectively. In comparison, the RFSed samples show only
uniformly dispersed micropores (Fig. 2(a–f)), while the CSSed samples
have scattered larger pores (Fig. 2(g, h)), which was related to the
long-period high-temperature diffusion and merging of micropores. In
addition, it is worth mentioning that the final diameters of the RFSed
samples were equivalent to the inner diameter (6.1 mm) of the boron
nitride protective tube in the graphite mold, suggesting that the HEPO
samples underwent plastic rheology under 10 MPa axial pressure during
the flash sintering process. Without the application of pressure, the
HEPO samples sintered at a current density of 150 mA/mm2 reached a
relative density of ~94 % and their diameters shrank to ~4.95 mm.
The fracture morphologies of all RFSed-5RE2Zr2O7 samples and
CSSed-5RE2Zr2O7 sample (1600 ◦ C–6 h) show a flat transgranular frac­
ture mode (Fig. 3(a–f)), indicating that they have relatively high
strength at grain boundaries. As the current density increased from
60 mA/mm2 to 200 mA/mm2, the porosity in the RFSed samples grad­
ually decreased, and the average grain size increased from 0.6 μm to
2.4 μm. Note that the average grain size of the CSSed sample was much
larger, reaching 5.2 μm. The smaller grain sizes in the RFSed samples
were mainly attributed to the ultrafast densification under rapid heating
and external pressure. Fig. 3(g) shows the SEM image of the polished
surface of the RFSed-5RE2Zr2O7 sample (under 200 mA/mm2) together
with the corresponding EDS mapping graphs. All the components were
homogeneously distributed over a wide range without noticeable
segregation or clustering.
Fig. 4(a) shows a TEM image of the RFSed-5RE2Zr2O7 sample (under
120 mA/mm2) at a triangular boundary junction. Each grain was ho­
mogeneous without containing a secondary phase. Selected area elec­
tron diffraction (SAED) pattern (Fig. 4(b)) and HRTEM image (Fig. 4(c))
confirmed that the RFSed-5RE2Zr2O7 sample had a single-phase pyro­
chlore structure. EDS analysis (Fig. S3) demonstrated that the
Fig. 2. Optical micrographs of (a–f) the RFSed-5RE2Zr2O7 samples sintered under different current densities and (g–h) the CSSed-5RE2Zr2O7 samples sintered at
1600 ◦ C for 3 h and 6 h.
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Journal of the European Ceramic Society 41 (2021) 2855–2860
5RE2Zr2O7 HEPO had no elemental segregation at the grain boundaries.
Furthermore, atom probe tomography was also used to characterize the
compositional homogeneity of the RFSed-5RE2Zr2O7 HEPO. The three-
dimensional (3D) reconstructions of the atomic maps (Fig. 4(d)) for
the RFSed-5RE2Zr2O7 HEPO (under 120 mA/mm2) strongly confirmed
the homogenous distribution of the compositions at the atomic scale.
As we have mentioned before, the mechanisms for ultrafast densifi­
cation in reactive flash sintering have not yet been clarified so far. Here,
we suppose that the ultrafast densification of the RFSed-5RE2Zr2O7
HEPOs is presumably attributed to the following aspects: (1) The com­
bination of transient high temperature (caused by Joule heat effect)
during the peak power stage (stage II) and external pressure (10 MPa)
should be responsible for the rapid densification, as demonstrated by the
fact that the diameter of the RFSed samples was equivalent to the inner
diameter of the boron nitride protective tube in the graphite mold. (2)
The presence of lattice defects in the RFSed sample promoted the rapid
diffusion of ions. It is believed that a large number of Frenkel-pair de­
fects such as positively charged oxygen vacancies and interstitial oxygen
ions can be generated in the oxide powders under the application of an
electric field [14,20,21]. These high-energy charged lattice defects can
greatly reduce the diffusion activation energy of the ions, thereby pro­
moting the rapid homogenization and densification of the high-entropy
oxides; (3) Rapid heating provided high sintering activity in the nano­
particles. During the peak power stage (~650–1550 mW/mm3) in the
RFS process, the samples underwent rapid heating (~103–104 ◦ C/min)
and dramatic shrinkage. The rapid heating and short duration at the
maximum temperature avoided grain coarsening and neck growth
encountered in traditional solid-state sintering process [22]; (4) Internal
reactions provided additional chemical driving force. The RFS process
was accompanied with phase transformations and solid solution re­
actions, which might provide additional impetus for the sintering.
The mechanical properties of the RFSed- and CSSed-5RE2Zr2O7
(1600 ◦ C-6 h) HEPOs were evaluated by using nano-indentation. Fig. 5
(b) shows the loading-unloading curves of the RFSed- and CSSed-
5RE2Zr2O7 HEPOs. The nano-hardness and Young’s modulus of the
RFSed HEPOs increased with increasing current density during sintering
(Fig. 5(c)). The RFSed sample sintered at 200 mA/mm2 showed a slight
decrease in hardness, presumably owing to the grain coarsening in its
microstructure (Fig. 3(e)). Similarly, the CSSed sample showed an even
lower hardness than the RFSed sample (under 200 mA/mm2) due to its
larger grain size (Fig. 3(f)). It is noteworthy that the modulus of the
CSSed sample was much lower than that of the RFSed samples. Jia et al.
observed a similar phenomenon but did not explain the mechanism
[23]. We speculate that this phenomenon may be related to the different
pore structures in the RFSed samples and the CSSed samples (Fig. 2), or
H.-R. Mao et al. Journal of the European Ceramic Society 41 (2021) 2855–2860

Fig. 3. Fracture morphologies of (a–e) the RFSed-5RE2Zr2O7 samples under different current densities and (f) the CSSed-5RE2Zr2O7 sample (the insets show the
statistic diagrams of average grain size (AGS) obtained by using Nano Measurer software); (g) SEM image of the polished surface of the RFSed-5RE2Zr2O7 sample
(under 200 mA/mm2) together with the corresponding EDS mappings of Zr, La, Nd, O, Sm, Eu and Gd elements.

to the influence of internal crystal defects or stress. However, the
detailed mechanism for this result needs to be further explored. The
indentation toughness Kc of the 5RE2Zr2O7 HEPOs was calculated ac­
cording to the following equation [24]:
( / )
KC = 0.015(a/l)1/2 (E/Hv )2/3 P c3/2 (1)
where E is the Young’s modulus (GPa), Hv is the hardness (GPa), P is the
load (N), l is the crack length (m), and a is the half-diagonal of the
indentation impression (c = l + a, as shown in Fig. 5(a)). The calculation
results (Fig. 5(d)) indicate that the fracture toughness of the RFSed-
5RE2Zr2O7 samples noticeably decreased with increasing current den­
sity and kept a plateau after the current density exceeded 120 mA/mm2.
However, it is worth mentioning that the calculated toughness values for
the low-density RFSed samples (sintered at 60 and 80 mA/mm2, marked
by brown dots in Fig. 5(d)) could have a large error since the cracks at
the indentation corners were inconspicuous. Surprisingly, the fracture
toughness of the nearly fully dense RFSed-5RE2Zr2O7 HEPO sintered at
200 mA/mm2 was as high as 2.8 ± 0.2 MPa⋅m1/2, more than twice that
of the single-component rare-earth zirconate RE2Zr2O7 (RE = La, Nd,
Sm, Eu, or Gd) [2,25]. In comparison, the fracture toughness of the
CCSed samples was much lower (1.1 ± 0.1 MPa⋅m1/2), which was
ascribed to the presence of relatively large pores (Fig. 2(h)). We suggest
that the superior mechanical properties of the RFSed-5RE2Zr2O7 HEPOs
are related to the current effect, rapid heating/cooling and uniform
distribution of micropores, but the specific mechanism needs to be
further explored.
4. Conclusions
Nearly fully dense (La0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7 HEPOs were
synthesized at a low furnace temperature in a short time by reactive
flash sintering. The application of electric field, rapid heating, external
pressure and internal reactions should play important roles in the rapid

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Fig. 4. (a) TEM image, (b) SAED pattern, (c) HRTEM image, and (d) 3D atomic distribution maps of the RFSed-5RE2Zr2O7 sample (under 120 mA/mm2).

Fig. 5. (a) Nano-indentation morphology of the RFSed-5RE2Zr2O7 HEPO (under 200 mA/mm2); (b) loading-unloading curves, (c) Young’s modulus, hardness and (d)
fracture toughness of the RFSed- and CSSed-5RE2Zr2O7 HEPOs (error bar represents standard deviation).

densification of the 5RE2Zr2O7 HEPOs. The resultant HEPOs had a Declaration of Competing Interest
uniform composition at the atomic scale and superior modulus, hardness
and fracture toughness to the CCSed counterparts. This work demon­ The authors declare that they have no known competing financial
strates that the RFS is a potentially advanced technique for the prepa­ interests or personal relationships that could have appeared to influence
ration of HEOs, especially for those with difficulty in achieving high the work reported in this paper.
densification.
Acknowledgments

We are grateful to Drs. Yu-Hua Liu, Liang Zhao and Gui-Xun Sun at

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H.-R. Mao et al.
Key Laboratory of Automobile Materials, Jilin University, for their helps
in characterization and testing. This work is supported by the National
Natural Science Foundation of China (Nos. 51871110 and 51604156)
and the Changbai Mountain Scholars Program of Jilin Province (No.
2015011).
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