Ceramics International 47 (2021) 21618–21624

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Microstructure evaluation of 3YSZ sintered by Two-Step Flash Sintering

Isabela R. Lavagnini a, *, João V. Campos a, Eliria M.J.A. Pallone a, b
a
Postgraduate Programme in Materials Science and Engineering, University of São Paulo, USP/FZEA, Av. Duque de Caxias Norte, 225, 13635-900, Pirassununga, SP,
Brazil
b
Department of Biosystem Engineering, Faculty of Animal Science and Food Engineering (FZEA), University of São Paulo (USP), 13635-900, Pirassununga, SP, Brazil

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

Keywords: Flash Sintering (FS) is an energy-efficient sintering technique, which allows a considerable reduction in pro­
Zirconia cessing time and temperature. However, a recurring problem of flash sintered samples is the microstructural
Yttria-stabilized zirconia heterogeneity, which occurs mostly on samples with a high surface-to-volume ratio (e.g., cylindrical samples).
Flash sintering
Thus, aiming to obtain homogeneous microstructures and smaller grain sizes, this work evaluated the application
Two step sintering
of Two-Step Flash Sintering (TSFS) in 3YSZ and compared them with samples sintered by FS. The TSFS exper­
iments consisted of applying a first step of current density with greater magnitude (100 mA mm-2 and 200 mA
mm-2) followed by the second step with smaller magnitude (50 mA mm-2 and 75 mA mm-2). In the FS experi­
ments, a single step of current density was used (100 mA mm-2 and 200 mA mm-2). The Results showed that TSFS
significantly reduced the microstructural heterogeneity compared to FS, promoting smaller and more homoge­
neous grain sizes in different regions of the samples.

1. Introduction energy savings when compared to conventional sintering [15,17,18].

Refined microstructures (smaller grain sizes) result in properties
changes in material, such as increased fracture toughness, increased
hardness, among others [1–6]. The microstructural control of ceramic
materials, and, consequently, of their final properties, can be performed
during the material processing stages [6–9]. Among these stages, sin­
tering is one of the most critical in obtaining a dense material with a
refined microstructure, due to the inherent grain growth of the process
[10–12]. Thus, several unconventional sintering techniques have been
studied to obtain materials with high densification and refined micro­
structure [13–16].
Flash Sintering (FS) is an unconventional sintering technique pre­
sented for the first time in 2010 [15]. This technique consists of applying
an electric field in a ceramic sample, concomitant to the furnace heating
up. At a critical temperature, the electric current flowing through the
sample rises abruptly due to the thermal runaway (cycle of increase in
temperature and electrical conductivity caused by the Joule heating in
materials with negative temperature coefficient), leading to rapid
densification of the sample. The furnace temperature in which the
thermal runaway occurs is usually much lower than the temperature
used in conventional sintering [15]. Thus, FS increases the processing
speed, reduces the processing temperature, and consequently promotes
Despite these advantages, some studies have reported microstruc­
tural heterogeneity within flash sintered materials, i.e., regions with
different grain sizes in the same sample. Some studies presented het­
erogeneities related to the interior and surface of the sample [19–23].
Others reported heterogeneities between the regions close to the elec­
trodes (cathode and anode) [24–26]. Anyway, this is a challenge that
must be overcome to achieve better properties of the final material.
Thus, several studies are looking for ways to improve the FS to obtain
materials with homogeneous microstructure [19,21,27–33].
Steil et al. [19] presented a variation of FS, the Double Flash Sin­
tering. This technique consists of applying two steps of current density:
the first one for a short time; and then, after an interval without current
density, a second step for a longer time. With this methodology, the
authors sintered 8YSZ to full density. Nie et al. [27] proposed another
variation of FS, the Two-Step Flash Sintering (TSFS). In this variation,
two steps of electric current density were applied: one of greater
magnitude (for a few seconds), only to activate the densification
mechanisms; and another one of lower magnitude to densify the mate­
rial without too much grain growth. Nie et al. sintered ZnO by TSFS and
obtained smaller grain sizes (up to three times) compared to those sin­
tered by FS.
Thus, the present work aims to evaluate the effect of two steps of

* Corresponding author.
E-mail address: isabela.lavagnini@usp.br (I.R. Lavagnini).

https://doi.org/10.1016/j.ceramint.2021.04.174
Received 29 March 2021; Received in revised form 15 April 2021; Accepted 18 April 2021
Available online 21 April 2021
0272-8842/© 2021 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
I.R. Lavagnini et al.
electric current density (TSFS) on the densification and microstructure
of 3YSZ using an alternate electric field.
2. Material and methods
The commercial 3 mol% yttria-stabilized zirconia powder from
Tosoh (TZ-3Y-E, particle size 40 nm, 6.05 g cm− 3 theoretical density)
was prepared as described in a previous work [21]. The cylindrical
samples (6 mm in diameter and 5 mm in height) were formed using
uniaxial pressing followed by isostatic pressing at 200 MPa, then
calcined at 600◦ C for 1 h using a heating rate of 5◦ C.min-1.
The sintering was carried out in an automated vertical tubular
furnace [26] using platinum disks as electrodes. Those disks were placed
on the flat surfaces of the cylindrical sample (top and bottom). A uni­
axial mechanical pressure (3 bar) was applied to maintain contact be­
tween the sample and the electrodes since no conductive paste was used.
An alternate electric field of 120 V cm-1 (RMS), frequency of 1000 Hz,
was applied since the beginning of the furnace heating (heating rate of
20◦ C.min-1). A displacement sensor (LVDT type) recorded the specific
linear shrinkage of the samples in situ during the sintering procedure.
For the TSFS experiments, the first step of a higher electric current
density (100 and 200 mA mm-2) was applied for 5 s. Then, in the second
step, a lower current density (75 and 50 mA mm-2) was applied for 55 s.
The experiments in FS were performed with the maximum current
density limits (100 and 200 mA mm-2) applied for 60 s. All the current
densities described above were RMS values. The different conditions
studied are represented and labelled in Table 1. J1, J2, Δt1 and Δt2 are,
respectively, the electric current densities of the first and second steps
and the time of those steps. Each condition was performed in triplicate.
The apparent densities of the samples were determined using the
Archimedes’ principle according to ASTM C373-8826; the averages of
the relative densities were expressed as a function of the theoretical
density of 3YSZ. The Black Body Radiation model (BBR) was used to
estimate the temperature on the samples surfaces during the first and
second step, using equation (1) [34]. The samples surface temperatures
for each step were calculated by the average temperature of the last 3 s
for each step.
( )
dTs
mCp = VI − σεA Ts4 − Tf4 (1)
dt
In equation (1) m is the sample mass (kg), Cp is the sample heat ca­
pacity (600 J kg-1 K-1 [35]), Ts is the sample temperature (K), t is time
(s), V is the voltage (V), I is the current (A), σ is Stefan’s Boltzmann
constant (5.67 10-8 W m-2 K-4), ε is the sample emissivity (assumed 0.8
[36]), A is the sample surface area (m2), and Tf is the furnace temper­
ature (K). The numerical solution of equation (1) is presented in terms of
iterations (i) in equation (2). Worth noting that the acquisition rate of
the setup was three points per second.
t(i + 1) − t(i) [ ( )]
Ts (i + 1) = Ts (i) + V(i)I(i) − σεA(i) Ts (i)4 − Tf (i)4
mCp
Carvalho et al. [37] reported that 3YSZ samples under alternate
electric field with 1000 Hz presented similar linear shrinkage as samples
under a direct electric field. It indicates that the capacitive effects have a
minor influence on the I and V when using this frequency. Thus, for the
Table 1
Experimental conditions of TSFS and FS using different step times and maximum
electric current densities.
Condition Label J1(mA.mm-2) Δt1 (s) J2 (mA.mm-2)
FS100 100 60 – –
TSFS100/50 100 5 50
TSFS100/75 100 5 75
FS200 200 60 – –
TSFS200/50 200 5 50
TSFS200/75 200 5 75
Ceramics International 47 (2021) 21618–21624
sake of simplicity, we did not take the capacitive response of the sample
into account in the BBR model. Therefore, assuming that I and V were in
phase, we used their RMS values in equation (2).
Cylindrical samples used here presented larger dimensions when
compared to dog-bone samples. Thus, in our experiments, the heat
exchanged between the sample flat surfaces and the electrodes cannot be
neglected at the BBR model. To consider the electrodes as heat sinks, the
area (A), used in equation (2), was the total surface area of the sample
(radial + flat surfaces). With that, we assumed that conduction heat flux
between the flat surfaces and the electrodes was similar to radiation heat
flux between the furnace and samples radial surfaces.
After sintering, the samples were cut in their radial centres in the
longitudinal direction. The cut surfaces were polished and thermally
etched at 1450◦ C for 10 min with a heating rate of 10◦ C.min-1. The
microstructural analysis was performed using a scanning electron mi­
croscope (SEM, FEG-XL 30). Different regions of the cut surface were
analysed: core, radial surface (located at half height of the cylindrical
samples), and the flat surface (region close to the electrodes). Fig. 1
shows the longitudinal radial section of the cylindrical sample and the
regions where the micrographs were obtained from the polished
surfaces.
The ImageJ software (National Institutes of Health) was used to
calculate the grain size in each analysed region. The homogeneity
evaluation, according to the average grain sizes in each region of the
same sample, was made by analysis of variance according to the Tukey
test, with a significance level of 5%.
3. Results and discussion
Fig. 2 shows the curves of electric current density (J), electric field
(E), power density (P), and linear shrinkage (dL/Lo) of all studied con­
ditions. It is observed that the curves presented are in accordance with
the standard curves of the FS, in which the increase in the electric cur­
rent density provides a drop in the value of the applied electric field as
well as the instantaneous shrinkage of the material [15]. For TSFS
samples, the current density curves presented two steps regarding the
magnitude of the current. The power density curves showed a high
power peak in the samples sintered by FS and only in the first step of the
samples sintered by TSFS. The power density is related to the samples’
temperature.
Fig. 2 also shows that the behaviour of the electric field was different
between the experiments. It is noted that the electric field of the samples
in TSFS presented two well-defined steps. In the case of TSFS200/75 and
TSFS200/50, the transition between the first and second step reached
lower values of electric field than the transitions of TSFS100/75 and
TSFS100/50. This behaviour indicates that the samples’ conductivity
changes during the steps transitions due to change in the samples’
temperature. This effect was more evident in TSFS200/50 because there
was a greater difference between the current density of the steps.
(2) However, despite the curves of current density, electric field, and
power density of the samples in TSFS present two well-defined steps, this
is not observed in the linear shrinkage curves. This is because most of the
linear shrinkage of the sample takes place at the first step, regardless of
Δt2 (s)
55
55
55
Fig. 1. Radial longitudinal section of a cylindrical sample and its polished
55
surface, with emphasis on regions where the microstructure was analysed.
21619
I.R. Lavagnini et al. Ceramics International 47 (2021) 21618–21624

Fig. 2. Electric current density (J), electric field (E), power density (P), and linear shrinkage (dL/Lo) curves as a function of time for samples during FS and TSFS.

the magnitude of the electric current density applied, in the same way as
Table 2
the shrinkage of the samples in FS. However, it is observed that the
Power density peak, average power density, and temperature estimated by BBR
samples in TSFS that received 75 mA mm-2 (regardless of the current
for samples during FS and TSFS followed by the standard deviation for all
density limit applied in the first step) showed higher values of linear conditions studied.
shrinkage, indicating that there was some shrinkage at the second step
Condition Power Peak Average Power (mW. Temperature BBR (◦ C)
as well.
Label (mW.mm-3) mm-3)
Table 2 shows the power density peak, the average power density,
1◦ step 1◦ step 2◦ step 1◦ step 2◦ step
and the calculated temperature using the BBR model for FS and for each
step of TSFS samples. It is observed that the sample temperature is FS100 1469.8 ± 528.4 ± – 1662.7 ± –
proportional to the current density applied, i.e., higher current densities 25.3 52.2 14.1
TSFS100/50 1325.5 649.1 ± 261.1 ± 1731.9 1416.4 ±
lead to higher temperatures [36]. Worth noting that the temperatures
± ±
53.0 16.5 5.4 12.2 10.3
estimated by BBR for FS and the first steps of TSFS samples using the TSFS100/75 1394.4 ± 643.7 ± 406.4 ± 1737.3 ± 1558.9 ±
same current density were slightly different. It happened because the 67.8 17.0 5.1 9.6 9.7
first steps of TSFS were too short (5 s). In this short time, the samples FS200 2782.5 ± 1189.3 ± – 2035.0 ± –
224.4 49.7 15.2
were still densifying. Thus, their electrical resistivity was still changing
TSFS200/50 2714.2 ± 1431.7 ± 242.8 ± 2087.4 ± 1401.1 ±
and consequently their temperature. In FS, the temperature estimated by 179.4 45.5 19.9 13.6 11.7
BBR was lower because the step was long enough (60 s) to densify and TSFS200/75 2830.5 ± 1455.7 ± 395.5 ± 2111.8 ± 1560.3 ±
stabilize the samples’ electrical resistivity. 201.7 48.3 21.7 15.7 8.1
The temperatures showed in Table 2 suggest that the samples
TSFS200/75, TSFS200/50, and FS200 reached temperatures higher than the
platinum melting point. However, no evidence of molten platinum was
observed on the electrodes, suggesting that the BBR model

21620
I.R. Lavagnini et al. Ceramics International 47 (2021) 21618–21624

overestimated the samples’ temperatures, up to 350◦ C as already re­
ported by Charalambous et al. [38].
The furnace temperature at the moment of the flash was 995◦ C
(±5◦ C) for all the studied conditions. The variation in the onset tem­
perature of flash between all the conditions was slight because the same
electric field limit (120 V cm-1) [39] was used in all cases, and all the
samples presented the same size [20].
Fig. 3 shows the micrographs in different regions (core, radial sur­
face, and flat surface) of the samples under different conditions in FS and
TSFS. Table 3 shows the relative densities and the average grain size
measured for these regions. It is observed that the samples in FS showed
larger grains in its core than in the other regions, regardless of the

Fig. 3. SEM micrographs of the different regions analysed for each condition studied.

21621
I.R. Lavagnini et al. Ceramics International 47 (2021) 21618–21624

current density limit used. Also, the sintered samples with a current
density limit of 200 mA mm-2 showed larger grains for all regions,
accompanied by the presence of pores. Dong and Chen [40] also
observed the presence of pores at flash sintered 8YSZ in severe condi­
tions of current density. These pores were attributed to the cavitation
effect, due to reduction-generated voids by condensation of supersatu­
rated oxygen vacancies [21,40].
The samples in TSFS with a limit of 100 mA mm-2 presented grains
with similar sizes for all analysed regions. In contrast, samples with a
limit of 200 mA mm-2, in the first step, showed much bigger grains in
their core than the other regions (radial and flat surfaces). Regarding the
current densities applied at the second step (50 or 75 mA mm-2), no
significant differences were observed.
The exaggerated growth in grain size inside samples in FS and TSFS,
when using a current density limit of 200 mA mm-2, happens due to the
thermal gradient formed in cylindrical samples during FS. This thermal
gradient is caused by the difference between the heat gain rate (due to
Joule heating) and the heat loss rate of the material [21,33,40,41]. In
the case of TSFS samples with a limit of 100 mA mm-2, it was possible to
control the thermal gradient.
Regarding the relative density of the samples, it can be seen in
Table 3 that the samples with a current density limit of 100 mA mm-2
showed higher densities than the samples with 200 mA mm-2. This
behaviour was counterintuitive if one thinks that higher temperature
should lead to higher densification. Although, as observed in Fig. 3, the
samples submitted to 200 mA mm-2 presented higher coarsening and
cavitation, leading to lower densification, as reported previously [21].
Besides that, in Fig. 1, the final linear shrinkage of the samples was
higher for conditions using 200 mA mm-2. However, the relative den­
sities showed the opposite behaviour. It can be happening because the
linear shrinkage was measured only on the vertical axis (height of the
cylinders). Thus, considering the superplasticity effect during flash
presented by the material [42–44], it is expected that the samples may
have deformed during these severe current density conditions. There­
fore, the linear shrinkage measured by the LVDT took into account the
shrinkage (caused by sintering) and deformation of the sample (caused
by the 3-bar mechanical pressure).
Fig. 4 shows the evaluation of microstructural homogeneity for all
conditions studied according to the Tukey’s mean difference. The
comparison between two regions of the same sample shows an average
difference value, and how close to zero this value indicates if the regions
have statistically similar grain sizes.
In Fig. 4, TSFS100/75 and TSFS100/50 presented a homogeneous
microstructure for all regions analysed. However, FS100 presented ho­
mogeneity only between the radial and flat surfaces. All samples that
received a current density limit of 200 mA mm-2, both in FS and TSFS,
presented heterogeneous microstructures in all regions. Although, in the
case of TSFS samples, the heterogeneity was slighter than those sintered

Table 3
Relative density and average grain size in the core, radial surface, and flat surface followed by the standard deviation for all conditions.
Condition Relative Densities (%TD) Average grain size (μm)

Core Radial Surface Flat Surface

FS100 92.1 ± 1.4 1.1 ± 0.2 0.5 ± 0.2 0.4 ± 0.2

TSFS100/50 92.9 ± 0.6 0.6 ± 0.2 0.5 ± 0.1 0.4 ± 0.2
TSFS100/75 93.9 ± 0.5 0.6 ± 0.3 0.5 ± 0.2 0.4 ± 0.2
FS200 90.9 ± 1.3 7.1 ± 1.8 0.8 ± 0.4 0.5 ± 0.2
TSFS200/50 90.1 ± 0.2 3.8 ± 1.6 0.6 ± 0.3 0.5 ± 0.2
TSFS200/75 89.3 ± 0.6 6.1 ± 1.8 0.6 ± 0.2 0.5 ± 0.2

Fig. 4. Tukey’s mean difference between the average grain size of each region was analysed for the same condition.

21622
I.R. Lavagnini et al.
by FS, indicating that the second step minimizes this heterogeneity.
4. Conclusions
The application of two steps of different electric current density
promoted greater microstructural control and homogeneity in the grain
size of 3YSZ cylindrical samples, showing the potential of the TSFS
technique to improve the results of FS even more.
However, the current density limit is an important parameter, as it
has a great influence on the final microstructure. The samples sintered in
TSFS with 200 mA mm-2 continued to exhibit microstructural hetero­
geneity between the regions studied, in addition to greater grain growth.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
This work was supported by the Coordenação de Aperfeiçoamento de
Pessoal de Nível Superior – Brasil (CAPES) – Finance Code 001 and the
São Paulo Research Foundation (FAPESP) [2015/07319-8, and 2018/
04331-5].
References
[1] H.L. Yao, C. Yang, Q. Yang, X.Z. Hu, M.X. Zhang, X.B. Bai, H.T. Wang, Q.Y. Chen,
Structure, mechanical and bioactive properties of nanostructured hydroxyapatite/
titania composites prepared by microwave sintering, Mater. Chem. Phys. 241
(2020) 122340, https://doi.org/10.1016/j.matchemphys.2019.122340.
[2] S. Balaji, B.K. Mandal, S. Ranjan, N. Dasgupta, R. Chidambaram, Nano-zirconia –
evaluation of its antioxidant and anticancer activity, J. Photochem. Photobiol. B
Biol. 170 (2017) 125–133, https://doi.org/10.1016/j.jphotobiol.2017.04.004.
[3] A. Kusior, J. Banas, A. Trenczek-Zajac, P. Zubrzycka, A. Micek-Ilnicka, M. Radecka,
Structural properties of TiO2 nanomaterials, J. Mol. Struct. 1157 (2018) 327–336,
https://doi.org/10.1016/j.molstruc.2017.12.064.
[4] Z. Yin, J. Yuan, Z. Wang, H. Hu, Y. Cheng, X. Hu, Preparation and properties of an
Al2O3/Ti(C,N) micro-nano-composite ceramic tool material by microwave
sintering, Ceram. Int. 42 (2016) 4099–4106, https://doi.org/10.1016/j.
ceramint.2015.11.082.
[5] P. fei Liu, Z. Li, P. Xiao, H. Luo, T. hui Jiang, Microstructure and mechanical
properties of in-situ grown mullite toughened 3Y-TZP zirconia ceramics fabricated
by gelcasting, Ceram. Int. 44 (2018) 1394–1403, https://doi.org/10.1016/j.
ceramint.2017.09.151.
[6] R.H.L. Garcia, V. Ussui, N.B. de Lima, E.N.S. Muccillo, D.R.R. Lazar, Physical
properties of alumina/yttria-stabilized zirconia composites with improved
microstructure, J. Alloys Compd. 486 (2009) 747–753, https://doi.org/10.1016/j.
jallcom.2009.06.204.
[7] P.J. Thomas, P. O’Brien, Nanomaterials Chemistry, WILEY-VCH Verlag GmbH &
Co, Weinheim, 2007, https://doi.org/10.1002/9783527611362.
[8] A. Shafeiey, M.H. Enayati, A. Al-Haji, The effect of slip casting parameters on the
green density of MgAl2O4 spinel, Ceram. Int. 43 (2017) 6069–6074, https://doi.
org/10.1016/j.ceramint.2017.01.151.
[9] F.A.T. Guimarães, K.L. Silva, V. Trombini, J.J. Pierri, J.A. Rodrigues, R. Tomasi, E.
M.J.A. Pallone, Correlation between microstructure and mechanical properties of
Al2O3/ZrO2 nanocomposites, Ceram. Int. 35 (2009) 741–745, https://doi.org/
10.1016/j.ceramint.2008.02.002.
[10] D.S.B. Heidary, M. Lanagan, C.A. Randall, Contrasting energy efficiency in various
ceramic sintering processes, J. Eur. Ceram. Soc. 38 (2018) 1018–1029, https://doi.
org/10.1016/j.jeurceramsoc.2017.10.015.
[11] M.N. Rahaman, Ceramic Processing and Sintering, 1996, https://doi.org/10.1179/
095066096790151286.
[12] N.J. Lóh, L. Simão, C.A. Faller, A. De Noni, O.R.K. Montedo, A review of two-step
sintering for ceramics, Ceram. Int. 42 (2016) 12556–12572, https://doi.org/
10.1016/j.ceramint.2016.05.065.
[13] A. Fregeac, F. Ansart, S. Selezneff, C. Estournès, Relationship between mechanical
properties and microstructure of yttria stabilized zirconia ceramics densified by
spark plasma sintering, Ceram. Int. 45 (2019) 23740–23749, https://doi.org/
10.1016/j.ceramint.2019.08.090.
21623
Ceramics International 47 (2021) 21618–21624
[14] Y. Chen, B. Fan, B. Yang, W. Ma, G. Liu, H. Li, Microwave sintering and fracture
behavior of zirconia ceramics, Ceram. Int. 45 (2019) 17675–17680, https://doi.
org/10.1016/j.ceramint.2019.05.334.
[15] M. Cologna, B. Rashkova, R. Raj, Flash sintering of nanograin zirconia in <5 s at
850◦ C, J. Am. Ceram. Soc. 93 (2010) 3556–3559, https://doi.org/10.1111/j.1551-
2916.2010.04089.x.
[16] M. Biesuz, R. Sedlák, T. Saunders, A. Kovalčíková, J. Dusza, M. Reece, D. Zhu,
C. Hu, S. Grasso, Flash spark plasma sintering of 3YSZ, J. Eur. Ceram. Soc. 39
(2019) 1932–1937, https://doi.org/10.1016/j.jeurceramsoc.2019.01.017.
[17] C.E.J. Dancer, Flash sintering of ceramic materials, Mater. Res. Express 3 (2016)
102001, https://doi.org/10.1088/2053-1591/3/10/102001.
[18] F. Trombin, R. Raj, Developing processing maps for implementing flash sintering
into manufacture of whiteware ceramics, Am. Ceram. Soc. Bull. 93 (2014) 32–35.
[19] M.C. Steil, D. Marinha, Y. Aman, J.R.C. Gomes, M. Kleitz, From conventional ac
flash-sintering of YSZ to hyper-flash and double flash, J. Eur. Ceram. Soc. 33
(2013) 2093–2101, https://doi.org/10.1016/j.jeurceramsoc.2013.03.019.
[20] J.V. Campos, I.R. Lavagnini, J.G. Pereira da Silva, J.A. Ferreira, R.V. Sousa,
R. Mücke, O. Guillon, E.M. Pallone, Flash sintering scaling-up challenges: influence
of the sample size on the microstructure and onset temperature of the flash event,
Scripta Mater. 186 (2020) 1–5, https://doi.org/10.1016/j.scriptamat.2020.04.022.
[21] I.R. Lavagnini, J.V. Campos, J.A. Ferreira, E.M.J.A. Pallone, Microstructural
evolution of 3YSZ flash-sintered with current ramp control, J. Am. Ceram. Soc.
(2020) 1–7, https://doi.org/10.1111/jace.17037.
[22] Y. Du, A.J. Stevenson, D. Vernat, M. Diaz, D. Marinha, Estimating Joule heating
and ionic conductivity during flash sintering of 8YSZ, J. Eur. Ceram. Soc. 36 (2016)
749–759, https://doi.org/10.1016/j.jeurceramsoc.2015.10.037.
[23] S. Carvalho, E. Muccillo, R. Muccillo, Electrical behavior and microstructural
features of electric field-assisted and conventionally sintered 3 mol% yttria-
stabilized zirconia, Ceramics 1 (2018) 1–10, https://doi.org/10.3390/
ceramics1010002.
[24] K. Ren, J. Xia, Y. Wang, Grain growth kinetics of 3 mol. % yttria-stabilized zirconia
during flash sintering, J. Eur. Ceram. Soc. 39 (2019) 1366–1373, https://doi.org/
10.1016/j.jeurceramsoc.2018.11.032.
[25] M. Biesuz, L. Pinter, T. Saunders, M. Reece, J. Binner, V.M. Sglavo, S. Grasso,
Investigation of electrochemical, optical and thermal effects during flash sintering
of 8YSZ, Materials 11 (2018), https://doi.org/10.3390/ma11071214.
[26] J.V. Campos, I.R. Lavagnini, R.V. Sousa, J.A. Ferreira, E.M.J.A Pallone,
Development of an instrumented and automated flash sintering setup for enhanced
process monitoring and parameter control, J. Eur. Ceram. Soc. 39 (2019) 531–538,
https://doi.org/10.1016/j.jeurceramsoc.2018.09.002.
[27] J. Nie, Y. Zhang, J.M. Chan, S. Jiang, R. Huang, J. Luo, Two-step flash sintering of
ZnO: fast densification with suppressed grain growth, Scripta Mater. 141 (2017)
6–9, https://doi.org/10.1016/j.scriptamat.2017.07.015.
[28] M. Biesuz, J. Dong, S. Fu, Y. Liu, H. Zhang, D. Zhu, C. Hu, S. Grasso, Thermally-
insulated flash sintering, Scripta Mater. 162 (2019) 99–102, https://doi.org/
10.1016/j.scriptamat.2018.10.042.
[29] A.G. Storion, J.A. Ferreira, S.C. Maestrelli, E.M.J.A. Pallone, Influence of the
forming method on flash sintering of ZnO ceramics, Ceram. Int. (2020), https://
doi.org/10.1016/j.ceramint.2020.08.210.
[30] R.R. Ingraci Neto, K.J. McClellan, D.D. Byler, E. Kardoulaki, Controlled current-
rate AC flash sintering of uranium dioxide, J. Nucl. Mater. 547 (2021) 152780,
https://doi.org/10.1016/j.jnucmat.2021.152780.
[31] G.M. Jones, M. Biesuz, W. Ji, S.F. John, C. Grimley, C. Manière, C.E.J. Dancer,
Promoting microstructural homogeneity during flash sintering of ceramics through
thermal management, MRS Bull. 46 (2021) 59–66, https://doi.org/10.1557/
s43577-020-00010-2.
[32] T.P. Mishra, R.R.I. Neto, R. Raj, O. Guillon, M. Bram, Current-rate flash sintering of
gadolinium doped ceria: microstructure and defect generation, Acta Mater. 189
(2020) 145–153, https://doi.org/10.1016/j.actamat.2020.02.036.
[33] C.A. Grimley, S. Funni, C. Green, E.C. Dickey, A thermal perspective of flash
sintering: the effect of AC current ramp rate on microstructure evolution, J. Eur.
Ceram. Soc. (2020), https://doi.org/10.1016/j.jeurceramsoc.2020.11.040.
[34] M.O. Prado, M. Biesuz, M. Frasnelli, F.E. Benedetto, V.M. Sglavo, Viscous flow flash
sintering of porous silica glass, J. Non-Cryst. Solids 476 (2017) 60–66, https://doi.
org/10.1016/j.jnoncrysol.2017.09.024.
[35] W. Ji, B. Parker, S. Falco, J.Y. Zhang, Z.Y. Fu, R.I. Todd, Ultra-fast firing: effect of
heating rate on sintering of 3YSZ, with and without an electric field, J. Eur. Ceram.
Soc. 37 (2017) 2547–2551, https://doi.org/10.1016/j.jeurceramsoc.2017.01.033.
[36] R. Raj, Joule heating during flash-sintering, J. Eur. Ceram. Soc. 32 (2012)
2293–2301, https://doi.org/10.1016/j.jeurceramsoc.2012.02.030.
[37] S.G.M. Carvalho, E.N.S. Muccillo, R. Muccillo, AC electric field assisted
pressureless sintering zirconia: 3 mol% yttria solid electrolyte, Phys. Status Solidi
Appl. Mater. Sci. 215 (2018) 1–5, https://doi.org/10.1002/pssa.201700647.
[38] H. Charalambous, S.K. Jha, R.T. Lay, A. Cabales, J. Okasinski, T. Tsakalakos,
Investigation of temperature approximation methods during flash sintering of ZnO,
Ceram. Int. 44 (2018) 6162–6169, https://doi.org/10.1016/j.
ceramint.2017.12.250.
[39] J.S.C. Francis, R. Raj, Influence of the field and the current limit on flash sintering
at isothermal furnace temperatures, J. Am. Ceram. Soc. 96 (2013) 2754–2758,
https://doi.org/10.1111/jace.12472.
I.R. Lavagnini et al.
[40] Y. Dong, I.W. Chen, Electrical and hydrogen reduction enhances kinetics in doped
zirconia and ceria: II. Mapping electrode polarization and vacancy condensation in
YSZ, J. Am. Ceram. Soc. 101 (2018) 1058–1073, https://doi.org/10.1111/
jace.15274.
[41] J. Park, I.W. Chen, In situ thermometry measuring temperature flashes exceeding
1,700◦ C in 8 mol% Y2O3-stablized zirconia under constant-voltage heating, J. Am.
Ceram. Soc. 96 (2013) 697–700, https://doi.org/10.1111/jace.12176.
[42] J.S.C. Francis, R. Raj, Flash-sinterforging of nanograin zirconia: field assisted
sintering and superplasticity, J. Am. Ceram. Soc. 95 (2012) 138–146, https://doi.
org/10.1111/j.1551-2916.2011.04855.x.
21624
Ceramics International 47 (2021) 21618–21624
[43] R. Raj, M. Cologna, J.S.C. Francis, Influence of externally imposed and internally
generated electrical fields on grain growth, diffusional creep, sintering and related
phenomena in ceramics, J. Am. Ceram. Soc. 94 (2011) 1941–1965, https://doi.
org/10.1111/j.1551-2916.2011.04652.x.
[44] J. Cho, Q. Li, H. Wang, Z. Fan, J. Li, S. Xue, K.S.N. Vikrant, H. Wang, T.B. Holland,
A.K. Mukherjee, R.E. García, X. Zhang, High temperature deformability of ductile
flash-sintered ceramics via in-situ compression, Nat. Commun. 9 (2018) 1–9,
https://doi.org/10.1038/s41467-018-04333-2.