Ceramics International 45 (2019) 17675–17680

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Ceramics International
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Microwave sintering and fracture behavior of zirconia ceramics T

a,∗ a,b,∗∗∗ a b b a,b,∗∗
Yongqiang Chen , Bingbing Fan , Bingquan Yang , Weikui Ma , Guoqi Liu , Hongxia Li
a
School of Materials Science and Engineering, Zhengzhou University, Henan, 450001, China
b
Sinosteel Luoyang Institute of Refractories Research Co., Ltd., Luoyang, 471039, China

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

Keywords: Yttria and Lanthana co-stabilized zirconia ceramics were successfully prepared by microwave hybrid sintering
Zirconia ceramics with a multi-mode cavity at 2.45 GHz. Microhardness, bending strength, fracture toughness, and relative density
La2O3 addition were tested. The fracture behavior of 3Y–ZrO2 ceramics was studied after sintering. The results showed the
Intergranular fractures average toughness values of 1550 °C microwave sintered and conventional sintered samples were 7.68 MPa m1/2
Grain boundaries
and 4.31 MPa m1/2 respectively. The average grain size of microwave sintered samples was 500 nm which was
Microwave sintering
smaller than that (700 nm) of conventional sintered samples. The microstructure of fracture samples showed that
the intergra1nular fractures were main features for microwave sintered samples, whereas the numerous trans-
granular fractures were observed in conventional sintered samples. The XRD results revealed that content of
monoclinic phase gradually increase with the increasing of microwave sintering temperature in 3Y–ZrO2 sam-
ples. It was proposed that the grain boundary diffusion and induced phase transformation worked together
weakening the grain boundary bonding strength under the effect of microwave field.

1. Introduction pollution, all-solid structure and wide fuel adaptability. The electrolytes
need to operate at high temperatures (600 °C-1000 °C) for a long time.
Zirconia (ZrO2) ceramics have attracted huge attention due to their So, 3Y-TZP is often used as an electrolyte in SOFCs due to good me-
unique properties, such as stable chemical properties, excellent me- chanical properties [11]. In addition, more than 8 mol% Y2O3 can be
chanical properties, low thermal conductivity, and good biocompat- added to matrix to get high oxygen ion conductivity [12]. Matsumoto
ibility [1–3]. Numerous advantages make it widely used in production, et al. [13,14] studied the high temperature phase stability and thermal
life, and scientific research [2–4]. In general, ZrO2 has three different conductivity of 4 mol% Y2O3–ZrO2 (YSZ) with (0–5 mol%) La2O3
crystalline states [5]: monoclinic (m), tetragonal (t), and cubic (c). Due doping. They found that 1 mol% La2O3 addition can significantly im-
to the lower thermal conductivity and toughness, applications of the prove the PSZ coating phase stability, and effectively reduce the
monoclinic ZrO2 were limited to some extent, while the tetragonal can thermal conductivity. Viazzi C. et al. [15] doped La2O3 in Y2O3–ZrO2
make up for the lack of monoclinic phase properties. Therefore, the via a mechanical milling method, and the results showed that when the
stable tetragonal zirconia at room temperature can broaden its appli- amount of additives was appropriate, the thermal conductivity of the
cation areas. However, cracks always appear when the ZrO2 transforms coating was reduced by 30% compared to the YSZ coating. Liu Y et al.
from monoclinic phase to tetragonal phase due to the volume changes. [16] found incorporation of La2O3 not only reduced the thermal con-
Therefore, various rare earth additives were added to ZrO2 ceramics to ductivity of the YSZ material, but also could make the coating grain size
prepare stabled ZrO2, such as [6–10], CaO, MgO, Y2O3, CeO2, and smaller and improve the material's sintering ability. Therefore, La2O3
La2O3. Over the past several decades, most literature have reported plays an important role in improving properties of PSZ. The defect re-
zirconia ceramics doped with single or multiphase doping oxides. To a action equation of Zr4+ replaced by La3+ is as follows:
certain extent, multiphase cooperation can make up for the deficiency ZrO2
of single doping, such as improving the sintering properties of the ′ + Vo·· + 3Oo
La2 O3 → 2LaZr
material and improving the mechanical properties. Solid oxide fuel cells
It has been known that microwave sintering can enhance ceramics
(SOFCs) is a new type power generation device with high efficiency, no
sintering rate, meanwhile, microwave can refine the grain and increase

∗
Corresponding author.
∗∗
Corresponding author. School of Materials Science and Engineering, Zhengzhou University, Henan, 450001, China.
∗∗∗
Corresponding author. School of Materials Science and Engineering, Zhengzhou University, Henan, 450001, China.
E-mail addresses: [email protected] (Y. Chen), [email protected] (B. Fan), [email protected] (H. Li).

https://doi.org/10.1016/j.ceramint.2019.05.334
Received 2 April 2019; Received in revised form 3 May 2019; Accepted 30 May 2019
Available online 01 June 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Y. Chen, et al. Ceramics International 45 (2019) 17675–17680

the strength and toughness of ceramics [17]. There are mainly two conventional precursor pyrolysis. The precursor was dried in a vacuum
modes about the interaction of microwave and ceramics materials: oven at 80 °C for 48 h, then calcined at 650 °C for 30 min.
energy dissipation and coupling with dipoles [18]. The energy dis-
sipation is connected with microwave frequency and materials tem- 2.2. Microwave sintering process
perature. The coupling with dipoles is related to dielectric loss of
ceramics materials. Meanwhile, the dielectric loss relies on materials The samples were formed by die pressing and cold isostatic pressing
composition and temperature with a certain microwave frequency [19]. process. Then, the green bodies were sintered in a multimode
The grain growth can be retarded under the effect of microwave field Microwave sintering furnace (SL-10 kW, San le) with auxiliary-heating
due to the existing of grain boundary energy. A local high temperature insulation device. The microwave frequency was 2.45 GHz with a
in grain boundary can cause a potential well that impedes the migration maximum input power of 10 kW. Microwave heating rate was con-
of atoms from grain boundary to low temperature adjacent matrix trolled by adjusting the input power. Meanwhile, the temperature was
[20,21]. Of course, the potential well is counterbalanced by high grain monitored using a monochromatic optical fiber infrared thermometer
boundary diffusivity with the increasing of sintering time. It is clearly (OI-T6I2–B-1-type, GOIDSUN, USA) and calibrated by Ferro (PTCR)
that microwave field always lowers sintering temperature and enhances Process Temperature Control Rings. For comparison purposes, the
sintering rate of ceramics materials. However, there is lacking attention conventional sintering was also used. The selected sintering systems
on grain boundary bonding under the especial interaction of grain were 1400 °C, 1450 °C, 1500 °C, 1550 °C and 1600 °C for 30 min.
boundary and electromagnetic field. Besides, the influence of micro-
wave field on phase transformation of ceramics materials also has been 2.3. Characterization
rarely researched. Zirconia is a typical phase transition material which
has been plenty researched [22]. The high temperature tetragonal The phase compositions of sintered samples were measured using
phase usually is stabilized with yttria. The transition of tetragonal phase the X-ray diffraction analysis (XD-3). The morphological features of
to monoclinic phase can absorb part fracture energy, thereby improving fracture surface of zirconia ceramics were examined by scanning elec-
fracture toughness of metastable zirconia ceramics. It has been de- tron microscopy (SEM, JEOL, JSM-7001F). The relative density is
monstrated that a traction applied to an interface can develop an gained by bulk density divided by theoretical density. The bulk density
electrical potential [23]. According to that, it could be assumed that of the sintered samples was measured by the Archimedes’ method.
microwave field can create stress in grain boundary or lattice which Single edge notched bending test was used to study fracture toughness.
may induce the phase transforming of zirconia in sintering process. The four adjacent sides of standard samples (2 mm × 4 mm x 22 mm)
Precursor powders strongly affect the properties of sintered ZrO2, were polished until no obvious scratches, then the chamfer dimension
and in our study a co-precipitation method was used to prepare the of the test strips was grinded to less than 1/10 of the thickness.
starting Y2O3 and La2O3 co-doped ZrO2 powders. The zirconia ceramics Subsequently, the middle of single side of the samples was cut out a
samples were prepared by microwave sintering and conventional sin- groove with a width of 0.2–0.22 mm and a depth of 0.8–1 mm by a wire
tering. The flexural strength, fracture toughness, density and Vickers cutting machine (DK7740, Taizhou chuang yuan machine tool co. LTD,
hardness of samples were measured. The aim of this work was to study China). The fracture load P was determined by three-point bending
the influence of microwave field and La2O3 on performance of 3Y–ZrO2 method (with a span of 16 mm and cross-head speed of 0.5 mm/min)
ceramics by analyzing physical properties, microstructure and XRD. using Universal Testing Machines (WD-P4504). The fracture strength
and toughness values were gained by the average of five measurements.
2. Experimental procedures The sample was polished to 5 μm with SiC abrasive cloth. Then, the
Vickers hardness (HV) was measured using a diamond indenter by a
2.1. Raw materials Vickers Hardness Tester (TH700, China Beijing, TIME) with a loading of
5 kgf and holding time of 15 s. Ten HV measurements were used to
The ZrOCl2·8H2O (99%, Zibo huan tuo chemical co. LTD, China) and obtain an average value.
Y(NO3)·6H2O, (Analytical reagent, Tianjin kai tong chemical reagent
co.,ltd, China) were used as raw materials. 3 mol% Y2O3 and n mol% 3. Results and discussion
La2O3 (n = 0, 1, 3, 5) co-doped partially stabilized ZrO2 (3Y-nLa-PSZ)
powders were prepared by chemical co-precipitation and conventional 3.1. Characterization of raw materials
pyrolysis method, using LaCl3·7H2O (chemical pure, ≥ 99%). The
ammonia water was used as precipitator. The NH3·H2O was added into The SEM and XRD of pyrolyzed ZrO2 (3Y–1La-PSZ) powder are
solution dropwise under rigorous stirring until pH = 10. The 3 mol% shown in Fig. 1. It could be seen that the particle size of as-synthesized
Y2O3 partially stabilized ZrO2 (3Y–ZrO2) powders were prepared by 3Y–1La-PSZ powders was approximate 30 nm with good dispersion

Fig. 1. SEM image (a) and XRD pattern (b) of synthesized ZrO2 (3Y–1La-PSZ) powders.

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Fig. 2. Practical microwave heating profile and corresponding input changes

and reflected power for 3Y–1La-PSZ compacts.

(Fig. 1(a)). Fig. 1(b) shows the X-ray diffraction pattern of 3Y–1La-PSZ
powders. It indicates that the main phase is t-ZrO2, and the reason is
Fig. 3. XRD patterns of 3Y-nLa-PSZ ceramics sintered at 1550 °C.
that the t-ZrO2 can be stably present when the content of yttrium oxide
is 3 mol% [24]. As well as, La2O3 or Y2O3 was not detected in powders
indicating La3+ and Y3+ dispersing well in gel after co-precipitation.
The morphologies and phase composition of the other 3Y-nLa-PSZ
powders are similar.

3.2. Microwave sintering process

It is well known that microwave heating exhibits selective and rapid

heating characteristics [25,26]. Thus, a two-stage heating method
(Fig. 2) was employed in our study. At the first sintering stage, a rapid
heating speed (∼30 °C/min) was controlled by tailoring the input
power and continued for 30 min. At this stage, it is clear that the re-
flected power increases synchronously with input power. The phe-
nomenon was interpreted that the coupling ability of ZrO2 and micro-
wave was weak at low temperature (below 600 °C) [27]. So, aided SiC
heaters absorbed microwave generating heat to sinter ZrO2 ceramics at
this stage by thermal radiation [27,28]. Fig. 4. Relative density of 3Y-nLa-PSZ sintered simples at different sintering
temperatures.
Immediately, the initial stage ended after the second phase begun
with a heating speed (∼15 °C/min). It could be seen that the reflected
power slightly decreased after the initial stage, and input power in- density decreased due to over-sintering causing abnormal grain growth
creased gradually in order to maintain the heating rate. The heating (Fig. 8(e)). The rare earth element (La2O3) has a special electron layer
rate was lower than that of the original stage. This was because ZrO2 structure which is a surface-active element of materials. So, it can im-
instead of SiC became the main absorption phase of microwave at prove the wetting performance of PSZ ceramics. Generally speaking, the
higher temperature, [26]. rare earth La2O3 is generally distributed in the surface of PSZ particles,
and it can reduce the melting point of the PSZ materials. Therefore, the
low melting point liquid phase can easily be formed. So, the porosity of
3.3. Characteristic of zirconia ceramics fabricated by microwave sintering
zirconia ceramics decreased due to the combined action of capillary
force and liquid phase. But, if the content of doped La2O3 is excess, the
Fig. 3 illustrates the XRD patterns of 3Y-nLa-PSZ ceramics sintered
mechanical properties of ceramics will decrease because of the new
at 1550 °C. The PDF numbers of tetragonal zirconia, monoclinic zir-
phase (La2Zr2O7), as we could see from Fig. 3. So, the hardness also
conia and La2Zr2O7 are 50–1089, 37–1484 and 49–1642 respectively. It
reached peak (14.3 GPa) for 3Y–1La-PSZ after 1550 °C sintering
shows that the fraction of t-ZrO2 increases with La2O3 content in-
(Fig. 5).
creasing. La2Zr2O7 and c-ZrO2 were detected when La2O3 content ex-
The bending strength and fracture toughness of the different sin-
ceeded 1 mol%. That was because the soluble of La2O3 in ZrO2 was
tered ceramics are the function of the La2O3 content which are sum-
lower (< 1 mol%), when La2O3 content exceeded 1 mol%, inter-
marized in Fig. 6 and Fig. 7 respectively. From the pictures, we can
granular phase (La2Zr2O7) was formed. Fig. 4 illustrates the relative
know that the bending strength of samples with different sintered
density and micro hardness of 3Y-nLa-PSZ with different sintering
temperatures has the same principle, all samples reached its maximum
temperatures. As we can see, the two items showed a parabolic varia-
in 3 mol% Y2O3 and 1 mol% La2O3 co-stabilized ceramics. So, the peak
tion tendency followed by the increased percentage of La2O3. The re-
of bending strength (192 MPa) was located in 3Y–1La-PSZ at 1500 °C,
lative density and microhardness reached peaks (99% and 14.3 GPa)
and decreased to 188.9 MPa at 1550 °C. we can see that the maximum
with the addition of 1 mol% La2O3 (3Y–1La-PSZ). Fig. 4 told us that the
of toughness was 7.68 MPa∙m1/2 for 3Y–1La-PSZ at 1550 °C. We also
maximum relative density of 3Y-nLa-PSZ appeared at 1550 °C. Mea-
found that the bending strength and toughness were all increased with
while, the relative density increased with temperature increasing before
the increasing sintered temperature before dropped at 1600 °C. The
1550 °C. However, when temperature reached 1600 °C, the relative

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Fig. 5. Microhardness of 3Y-nLa-PSZ sintered simples at different sintering

temperatures.

Fig. 8. Fracture surface of 3Y-nLa-PSZ compacts sintered by microwave at

different temperatures: (a) 3Y–1La-PSZ, 1400 °C (b) 3Y–1La-PSZ, 1450 °C (c)
3Y–1La-PSZ, 1500 °C (d) 3Y–1La-PSZ, 1550 °C and (e) 3Y–1La-PSZ, 1600 °C. (f)
3Y–0La-PSZ, 1550 °C (h) 3Y–3La-PSZ, 1550 °C (i) 3Y–5La-PSZ, 1550 °C.

possible reason was that La2O3 refined the ceramic grains (Fig. 8), and
the finer the grain, the greater the proportion of grain boundaries. So,
Fig. 6. Bending strength of 3Y-nLa-PSZ sintered simples at different sintering
when the grain boundaries are destroyed, samples with smaller size
temperatures.
grains will have a longer crack growth journey shortening the dis-
location glide. As a result, the strain difference between the inside grain
and the grain boundaries will be smaller. Finally, there is a smaller
chance of cracking, and a high toughness. But when the temperature
reached 1600 °C, the grains abnormal grew causing the dropped me-
chanical properties.
SEM images of fracture surfaces of 3Y-nLa-PSZ samples prepared by
microwave sintering at different temperatures were shown in Fig. 8.
Fig. 8 (a) showed that the samples merely had less dense and in-
homogeneous microstructure at a lower temperature (1400 °C). This
was mainly because the low level of input power resulted in low elec-
tromagnetic field energy. With the input power increasing, the sintering
temperature increased and more microwave energy was absorbed in-
side the sample which would provide more driving force for densifi-
cation, as shown in Fig. 8(b–d). The 3Y–1La-PSZ materials sintered at
1550 °C (Fig. 8 (d)) exhibited homogeneous microstructure with an
average grain size of about 500 nm. But when the sintering temperature
was further increased to 1600 °C, the grain size increased greatly
(∼1 μm), as shown in Fig. 8 (e). However, below 1550 °C, the grain
growth was limited by the limited energy due to the low input power.
When the temperature was over 1550 °C, the increase of input power
Fig. 7. Indentation fracture toughness of 3Y-nLa-PSZ sintered simples at dif- led to the large quantity of heat and high electromagnetic field in-
ferent sintering temperatures. tensity, which greatly promoted the diffusion of atoms resulting in the
existence of grains with size of about 1 μm at 1600 °C. Intergranular

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defects were observed inside the exaggerated grain due to rapid growth,
which could decrease the apparent density of samples, but the particles
were packed tightly and showed no apparent pores. The samples still
exhibited higher relative density under the circumstances. Comparing
Fig. 8(d–i), it told us that the grain size of un-doped lanthanum oxide
simple (3Y–0La-PSZ, 1550 °C) was significantly larger than that of
doped lanthanum oxide simple. Thus, the grain size reduced due to the
increasing content of La2O3. Unfortunately, when the percentage of
La2O3 exceeded 1 mol%, for example, 3 mol% and 5 mol%, the grain
size decreased as expect, while the inhomogeneous grains also ap-
peared. It could be explained that the La2Zr2O7 destroyed the densifi-
cation process. In general, the rare earth lanthanum aggregated at the
grain boundaries of the material in the form of tiny oxides, and the
concentration distribution was non-equilibrium thermodynamic beha-
vior with a kind of uphill diffusion [29,30]. La3+has a larger ionic ra-
dius and can reduce the thermal diffusion in the grain boundaries,
lattice and ceramic surface [31]. Furthermore, to a certain extent, the
grain growth was inhibited resulting in grains with smaller size.
Therefore, the addition of rare earth lanthanum played a significant
role in promoting the sintering process and leading to the grain re- Fig. 9. SEM of 3Y–ZrO2 ceramics fracture surface after sintering at 1550 °C, (a,
finement. But the content can not be surpassed 1 mol% in order to avoid c-microwave sintering, b, d-conventional sintering).
local accumulation of La2O3 and generating La2Zr2O7.
caused transgranular fracture. According to above analysis, it could be
3.4. Fracture behavior analysis concluded that grain boundary cohesion of MS samples was weaker
than that of CS samples. The lower Vickers hardness value of MS
Table 1 shows the sintering time and physical properties of 1550 °C samples also further confirmed this conclusion. It was interesting that
3Y–1La-PSZ samples. The average grain size of 1550 °C MS (microwave microwave sintering weakened the grain boundary strength of zirconia
sintering) sample is 500 nm, which is smaller than that (700 nm) of ceramics. It was deemed that the grain boundary firstly became high
1550 °C CS (conventional sintering) sample. It is noteworthy that the energy region due to the selective heating of microwave field. Then, the
MS time (140min) was obviously shorter than CS time (600 min). In atoms speedily diffused to adjacent matrix due to extremely energy that
other words, the microwave field actually promoted the grain growth of caused weak grain boundary. In contrast, the conventional sintering
zirconia ceramics. This phenomenon seemingly contradicted the feature can't cause local energy accumulation.
of microwave sintering retarding grain growth. In fact, the 140 min is a Fig. 10 shows the XRD patterns of 3Y–1La-PSZ samples of conven-
long process for microwave sintering. Although the grain boundary tional sintering at 1550 °C and microwave sintered at different tem-
energy could retard the grain growth within a short time, the energy peratures (1400°C-1600 °C). Both m-ZrO2 and t-ZrO2 phases were de-
fast decreased due to excessively accumulating that promoted the grain tected in all samples. However, with the sintering temperature
growth after a certain time. It is well known the reduction of grain size increasing, the t-ZrO2 diffraction peaks gradually became weak while
normally reduces the fracture toughness of zirconia ceramics. Never- the m-ZrO2 diffraction peaks became stronger as seen in Fig. 10 (a). As
theless, the MS sample with an average grain size of 500 nm has the comparing, the m-ZrO2 diffraction peak is very weak in the conven-
toughness value of 7.68 MPa m1/2 which was higher than tional sintering sample. The reason is that long microwave sintering
(4.31 MPa m1/2) that of the CS sample with an average grain size of process has caused phase transition (t → m) among the sintering sam-
700 nm. The improving of fracture toughness usually is related to in- ples [26]. According to the results, it could be proposed that microwave
creased crack propagating path. That is to say that the crack propa- filed induced the formation of monoclinic 3Y–ZrO2. In addition, two
gating energy can be effectively absorbed by the increasing of propa- Zr4+ were replaced by two La3+ or two Y3+ in the crystal lattice of 3Y-
gation path in 1550 °C MS samples. By contrast, the lower toughness nLa-PSZ, then an oxygen vacancy arose. As a result, the lattice was
value of CS samples was correlated to higher stress concentration due to distorted and induced pinning effect due to the presence of oxygen
the strong grain boundary bonding. vacancies around Zr4+, so the t-ZrO2 can still exist at room temperature
Fig. 9 shows SEM of 3Y–1La-PSZ ceramics fracture surface after [31]. Note that if the dense 3Y–ZrO2 was monoclinic phase under the
sintering at 1550 °C, (a,c-microwave sintering, b, d-conventional sin- action of microwave filed at high temperature, the transforming of
tering). It can be seen from Fig. 9 that the fracture of MS sample mainly monoclinic phase to tetragonal phase was inevitable after removing
happens at grain boundary. It is noticeable that the actual area of microwave field. Therefore, the phase transforming of m-3Y–ZrO2 to t-
fracture region of MS sample is larger than that of CS sample. This 3Y–ZrO2 broke the grain boundary bonding after turning off microwave
result certified that the more fracture energy was absorbed by the in- power. It also can be seen from Table 1 that the flexural strength of MS
creasing of fracture region. The transgranular fracture can be obviously samples is lower that of CS samples due to weak grain boundary
observed from Fig. 9(b) and (d). It was believed that the stress con- bonding. There are two possible reasons for the formation of monoclinic
tinuously accumulated in the process of crack propagating which 3Y–ZrO2 ceramics. The first, the interaction of external field and space

Table 1
The sintering time and physical properties of 1550 °C samples.
ST min GS nm FS MPa FT MPa.m1/2 H GPa BD g/cm3

1550 °C MS 140 500 ± 75 189 ± 23 7.68 ± 0.81 14.3 ± 1.8 5.84

1550 °C CS 600 700 ± 100 326 ± 34 4.31 ± 0.68 15.6 ± 2.1 6.01

ST: Sintering time; GS: Grain size; FS: Flexural strength; FT: Fracture toughness; H: Hardness.
MS: Microwave sintering; CS: Conventional sintering; BD: Bulk density.

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Fig. 10. 3Y–1La-PSZ samples sintered at different temperatures.

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