Solid State Ionics 180 (2009) 5762

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Solid State Ionics

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / s s i

Investigation of electrical and mechanical properties of 3YSZ/8YSZ

composite electrolytes
M. Ghatee a, M.H. Shariat a, J.T.S. Irvine b,
a
Department of Materials Science and Engineering, School of Engineering, Shiraz, Iran
b
School of Chemistry, University of St. Andrews, Purdie Building, St Andrews, Fife KY16 9ST, Scotland, United Kingdom

a r t i c l e i n f o a b s t r a c t

Article history: The effects of addition of 3YSZ (3 mol% yttria stabilized zirconia) on electrical and mechanical properties of
Received 14 March 2008 8YSZ (8 mol% yttria stabilized zirconia) has been investigated. Three different composites of 3YSZ/8YSZ with
Received in revised form 30 September 2008 compositions of 10 wt.%, 25 wt.% and 35 wt.% of 3YSZ were prepared by conventional solid oxide mixing
Accepted 7 October 2008
followed by sintering. Microstructures were characterized by XRD and SEM. The electrical properties were
studied by impedance spectroscopy as a function of temperature. Biaxial exural strength and fracture
Keywords:
toughness of composite samples were measured by ring on ring and Vickers microhardness indentation
Zirconia
Electrolyte
methods respectively. Results of electrical conductivity measurement proved that by increasing the 3YSZ
Mechanical properties content of the composite samples, the electrical conductivity at high temperatures (T N 550 C) decreased
while at low temperatures (T b 550 C) the conductivity increased. In addition, composite electrolytes had
lower activation energy of conductivity at both low and high temperatures. It was shown that both toughness
and fracture strength of composite samples improved by the addition of 3YSZ particles.
2008 Elsevier B.V. All rights reserved.

1. Introduction zirconia (PSZ) [13]. If a signicant volume fraction of metastable

Yttria doped zirconia solid electrolytes are among the most im-
portant oxygen ion conducting solid electrolytes, owing to their
applications in technologically important devices, e.g. solid oxide fuel
cells [1,2]; oxygen sensor [3,4]; and oxygen pumps [5]. In most of
these applications, not only high ionic conductivity, but also better
mechanical properties (exural strength and fracture toughness) are
required. In this group of ionic conductors, 8 mol% yttria stabilized
zirconia (8YSZ) with cubic structure possesses highest ionic con-
ductivity and good chemical stability over wide temperature and
oxygen partial pressure range [6] but its low mechanical strength,
hinders the fabrication of self supported electrolyte plate for use in
planar solid oxide fuel cell systems [7]. Addition of second phase
particles like alumina [7,8], neodymium titanate [9], BaTiO3 [10] or
monoclinic zirconia [11] improve mechanical strength of 8YSZ but at
the same time can degrade electrical properties [2,7,8].
According to ZrO2Y2O3 phase diagram [12], at stabilizer concen-
tration of 37 mol% Y2O3, both cubic and tetragonal phases can be
retained in the microstructure. The microstructure of these ceramics
consists of a cubic phase matrix in which tetragonal phase is dispersed
This grade of ZrO2Y2O3 solid solution is termed partially stabilized
Corresponding author.
E-mail address: jtsi@st-and.ac.uk (J.T.S. Irvine).
tetragonal phase is present, these tetragonal precipitates give the
ceramic good mechanical properties (strength and toughness) by a
process known as transformation toughening [14]. So the presence of
tetragonal phase can improve mechanical properties of zirconia based
solid electrolyse. As the maximum conductivity in ZrO2Y2O3 occurs
at a concentration of around 8 mol% of yttria, the electrical con-
ductivity of PSZ is lower than 8YSZ [15]. The addition of ne particles
of partially stabilized zirconia enhanced the fracture toughness
without signicantly degrading the conductivity of 8YSZ ceramics
[13].
3 mol% yttria stabilized zirconia (3YSZ) with an excellent
combination of high exural strength (~1 GPa) and good fracture
toughness (~ 10 MPa m1/2) are usually used to prepare composite
materials with other engineering ceramics like alumina and TiB2 to
improve the mechanical properties of these ceramics [14,16]. The 3YSZ
ceramics which are ne grained material with tetragonal structure
(usually called tetragonal zirconia polycrystals, TZP) also show higher
electrical conductivity than 8YSZ at low temperatures (T b 550 C) [17].
Composite materials can improve the combination of electrical
and mechanical properties of materials to get the required performance
required for different applications. The electrical conduction and
mechanical properties of solid electrolytes is inuenced by the presence
of a second phase [18,19].
This study is part of a programme to prepare and evaluate different
zirconia composites formed by different fabrication methods. The
aim of the present research is to study the effects of addition of 3YSZ

0167-2738/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.ssi.2008.10.006
58 M. Ghatee et al. / Solid State Ionics 180 (2009) 5762

Table 1 The cubic phase fraction, Xc, and cubic volume fraction, Vc, were
Nomenclature, composition, density and grain size of specimens calculated from Eqs. (2) and (3) respectively [21]
Specimen Composition Density Th. density % of Th. Grain size (m)
description (g cm 3) (g cm 3) density Cubic Tetragonal I400c
Xc = 2
I400c + I400t + I004t
8YSZ 13 wt.% Yttria 5.6 5.90 95 5
(TZ-8Y, stabilized zirconia
TOSOH) 1:34Xc
C1 10 wt.% 3YSZ 5.6 5.29 96 4 0.3
Vc = 3
1 + 0:34Xc
90 wt.% 8YSZ
C2 25 wt.% 3YSZ 5.8 5.95 97 4 0.3 where Ic and It represent the integrated intensity of cubic (400) and
75 wt.% 8YSZ
tetragonal (400) and (004) peaks after correcting for background.
C3 35 wt.% 3YSZ 5.7 5.97 95 4 0.3
65 wt.% 8YSZ The phase fraction of monoclinic phase was also investigated by the
Pure 3YSZ 5 wt.% Yttria 5.9 6.10 96 0.2 method of Garvie and Nicholson [22]:
(TZ-3Y-E, stabilized zirconia  
TOSOH) I 111 + I111m
Xm = m  4
Th. means theoretical density.
I111m + I 111 + I 111t
m

in which It and Im represent the integrated intensity of tetragonal

particles on electrical and mechanical properties of a 8YSZ matrix. The (101) and monoclinic (111) and (111) peaks. The monoclinic volume
electrical properties of the resultant composites have been compared fraction, Vm, was calculated from Eq. (5)
with existing models of electrical conductivity of composite materials.
1:34Xc
Vm = 5
2. Experimental 1 + 0:34Xc

Pseudo-Voigt function was used to t peak shape and calculating

High purity 8YSZ (TZ-8Y, Tosoh Corporation, Tokyo, Japan) and related parameters.
3YSZ (TZ-3Y-E, Tosoh Corporation, Tokyo, Japan) were used as raw
materials. Three different compositions of 3YSZ/8YSZ mixture with
10, 25, and 35 wt.% of 3YSZ were produced by conventional solid
oxide mixing, hereafter referred to as C1, C2 and C3 respectively (see
Table 1). Appropriates amounts of 3YSZ and 8YSZ powders were
weighed and then mixed by ball milling for 12 h in acetone, using
zirconia grinding media and polyethylene container to produce a
more homogeneous distribution of particles. Particle size of resulting
mixture was studied by Laser particle analysis (Horiba LB550, USA).
The resulting mixtures were then dried. Cylindrical pellets were pre-
pared by uniaxial pressing (P = 40 MPa) followed by isostatic pressing
(P = 200 MPa). Pellets were sintered at 1350 C for 5 h. This sintering
temperature was chosen because the dilatometry results for various
compositions of composite electrolytes showed signicant shrinkage
at temperatures around 1350 C and use of a much higher temper-
atures would have moved phase assembly much closer to equilibrium
distribution than in starting mixture.
Density of samples was measured by Archimedes procedure in
distilled water. The theoretical densities of pure 3YSZ and 8YSZ were
taken 6.1 and 5.9 g/cm3 respectively. These theoretical densities were
used to calculate theoretical density of composite samples (C1, C2 and
C3) by simple mixing rule by the following equation

Theoretical density of composite samples = m1 1 + m2 2 1

where 1 and 2 are volume fractions of each component with

theoretical densities of 1 and 2 respectively.
The polished and chemically etched samples (using hot sulfuric
acid) were investigated by means of scanning electron microscopy
(SEM, JEOL, JSM-56000) to reveal the microstructure. The average
grain sizes were measured by the linear intercept length method [20].
Phase analysis was carried out on sintered samples by X-ray pow-
der diffraction (XRD) using a STOE Stadi P transmission diffractometer
(Cu K1 = 1.5406 ). At rst, XRD measurements were performed over
2 range of 2090 with a step width of 0.05 and 40 s of exposure
time per position. Because of structural similarity of cubic and te-
tragonal phases, some of the XRD diffraction peaks of these two
structures usually overlap. To conrm the presence of both cubic
and tetragonal phases and to calculate the amount of each phase,
XRD measurements were also performed in a narrower 2 range from Fig. 1. XRD pattern of composite electrolytes after sintering at 1350 C for 5 h, see Table 1
70 to 80 with a step size of 0.05 and 50 s of exposure time per step. for compositions.
 M. Ghatee et al. / Solid State Ionics 180 (2009) 5762
Electrical conductivity was measured by two terminal a.c.
impedance measurements using a Hewlett Packard 4192A impedance
analyzer over the frequency range 5 Hz13MHz. Measurements were
made using platinum electrodes, in air, over the temperature range
300900 C. Temperature was controlled by Keithley nanovoltmeter
and collected data were analysed by electrochemical impedance
software Zplot.
Hardness and toughness were measured by Vickers micro
indentation method on surfaces polished down to 1 m diamond
paste by hardness tester (Matsuzawa, model MHT2, Yamamoto, Japan)
under load of 98 N. The formula of Anstis [23] was used to calculate
fracture toughness, using an elastic modulus (E) of 200 GPa [24].
Biaxial exural strength of disc type specimens was measured
by ring on ring test method according to the ISO 6474 standard test
method [25]. A universal testing machine ZWICK (Model 1496-2D,
Germany) with cross head speed of 0.1 mm/min, was used to perform
Fig. 2. XRD pattern of composite electrolytes after sintering, over limited 2 range.
59
Fig. 3. Typical SEM images of composite electrolytes (C3 at different magnications).
the ring on ring test on specimens with diameter of 20 mm and
thickness of at least 2 mm. Measurement of hardness, toughness and
strength was performed on at least 5 different samples and data were
reported as an average.
3. Results and discussions
3.1. Phase assemblages and microstructure
Table 1 presents nomenclature and densities of sintered samples.
In addition, densities of pure 3YSZ and 8YSZ prepared under same
sintering condition are also presented. All the samples showed 96% of
theoretical density, which is acceptable for electrical and mechanical
measurements. Laser particle analysis showed that particle size has
not changed drastically after ball milling. The mean particle size re-
duced from 150 nm to 140 nm after ball milling.
The XRD patterns of the various composite electrolytes in the
range of 2 from 20 to 90 are shown in Fig. 1. According to JCPDS card
42-1164 and 27-0997, diffraction proles of both cubic and tetragonal
zirconia are seen to be present in all composite grades. As shown in
Fig. 2, the measured XRD patterns over the 70 to 80 show the pre-
sence of (400)t and (004)t peaks of tetragonal phase(JCPDS card 27-
0997) and the (400)c of cubic phase(JCPDS card 42-1164), which
is used to distinguish the cubic from tetragonal structure. Calculated
amount of tetragonal phase does not show a signicant deviation
from initial values. In addition, the amount of monoclinic phase is
not noticeable. It should be added that the calculation of tetragonal
60 M. Ghatee et al. / Solid State Ionics 180 (2009) 5762

3.2. Electrical properties

Total conductivity and contribution of bulk and grain boundary

Fig. 4. Impedance plots of pure 8YSZ and C3 samples measured at 380 C.
Fig. 5. Arrhenius plot of total conductivity for samples C1, C2, C3 and pure 8YSZ.
phase in C1 sample with 10 wt.% 3YSZ is not accurate due to low
concentration of this phase and lower detection limit of XRD
technique.
The SEM micrograph of a typical composite sample is shown in
Fig. 3. In all composite samples, a clear bimodal grain size distribution
is present that is composed of ne tetragonal and larger cubic grains
[6]. Grain sizes of tetragonal and cubic grains are presented in Table 1.
The lower grain size of cubic phase in composite electrolytes with
respect to pure 8YSZ grain size (prepared under the same conditions)
can be related to grain growth inhabitation of cubic grain by ne grain
tetragonal particles.
conductivities to the total conductivity of each ceramic sample were
estimated using impedance spectroscopy. Fig. 4 compares impedance
plot of pure 8YSZ and C3 sample in which the effect of second phase on
impedance plot is more obvious. The geometrical factor (the ratio of
area to thickness) of pure 8YSZ and C3 samples were 8.1 and 4.7 cm 1
respectively. In the low temperature range (280450 C) two semi
circles are observed in the impedance plot. The high frequency arc
is the bulk component and low frequency arc correspond to grain
boundary contribution. As can be seen the impedance spectra of C2-B
sample show depressed grain boundary arc with lower contribution of
grain boundary resistance to total conductivity. The impedance spectra
can be modeled with a series of three electrical circuits, having
resistance and constant phase element coupled in parallel. Because of
depression of the arcs in some cases, the use of simple capacitor is not
sufcient to model the electrical response of the materials so more
complex equivalent circuit with frequency-dependent elements such
as constant phase elements is used to t results.
Arrhenius plots of total conductivity for various composite
electrolytes are shown in Fig. 5. The activation energy can be obtained
from the slope of the Arrhenius line.
A change in activation energy occurs at ~ 550 C which has been
attributed to the associationdissociation of defect clusters [6]. The
values of specic conductivity at 900 C for different composites are
shown in Table 2. The conductivity of composite electrolytes at this
temperature decreases with increasing 3YSZ content. This can be due
to the lower conductivity of 3YSZ with respect to 8YSZ at high
temperatures. The conductivity of 3YSZ phase is lower than the 8YSZ
by a factor of two at high temperatures (T N 550 C) [26].
The values of apparent total activation energy of samples at high
and low temperatures are shown in Table 2. The activation energies of
composite electrolytes decreased at high and low temperatures with
respect to pure 8YSZ prepared under the same conditions. This can be
related to the fact that activation energy of electrical conductivity for
3YSZ is lower than 8YSZ at all temperatures [26]. In order to have a
better insight of the effect of addition of second phase on electrical
properties of composite electrolytes, the Arrhenius plot of both bulk
and grain-boundary of samples at low temperatures (T b 550 C) along
with the corresponding plot of pure 8YSZ are shown in Fig. 6 and 7
respectively. The conductivity of composite samples at low tempera-
tures increases due to increase in 3YSZ content. This can be due to the
higher conductivity of 3YSZ than 8YSZ at low temperatures. As can be
seen, addition of 3YSZ decreases slightly both bulk and grain boundary
activation energy with respect to pure 8YSZ at low temperatures
(Table 3).
The presence of a second phase (generally nely dispersed and
insulating) can induce space charge near the grain boundary
interfaces, leading to an increase the in the electrical conductivity.
This effect is called the composite effect and it occurs mainly at low
temperatures [27,28].
Various models have been proposed to account for the overall
composite electrical properties. A good review of these models and

Table 2
Activation energy at low and high temperatures and conductivity at 900 C of the composite electrolyte and pure 8YSZ, bulk and grain boundary components considered together

Specimen Activation energy (eV) Conductivity Theoretical conductivity of

Low temperatures High temperatures at T = 900 C (S/cm) composite samples, calculated
(T b 550 C) Ea 0.03 eV (T N 550 C) Ea 0.04 eV using GEM model (S/cm)

8YSZ (TZ-8Y, TOSOSH) 0.95 1.08 0.10

C1 0.95 1.08 0.094 0.10
C2 0.90 1.00 0.090 0.094
C3 0.89 1.01 0.088 0.086
 M. Ghatee et al. / Solid State Ionics 180 (2009) 5762 61

Table 4
Vickers hardness and Indentation fracture of samples

Specimen Vickers hardness (GPa) Indentation fracture toughness (MPa m1/2)

Pure 8YSZ 11.8 1.7
C1 11.9 2.6
C2 12.5 3.7
C3 12.7 4.3
Pure 3YSZ 12.7 5.8

Use of the general effective media model (GEM) [29] or Wiener's

rule [29] results in nearly the same theoretical values for composite
system described here which can be due to comparable electrical
conductivity of the components of these composites.
Fig. 6. Arrhenius plot of bulk conductivity of samples at low temperatures (T b 550 C).
3.3. Mechanical properties

The Vickers hardness and indentation fracture toughness of the

different composite grades are summarised in Table 4. The hardness of
composite samples does not change signicantly.
The indentation fracture toughness of various composite electro-
lytes also increase with increasing 3YSZ content. The toughness of C3
sample is 4.3 MPa m1/2,which is the highest value among the different
composite samples. The increase in toughness of composite electro-
lytes can be attributed to transformation toughening mechanism.
Transformation of metastable tetragonal to monoclinic phase at crack
tip, improves toughness of 3YSZ and 3YSZ containing ceramics [14,30].
In addition, toughness of pure 8YSZ and 3YSZ raw materials pre-
pared under the same condition are 1.7 MPa m1/2 and 5.8 MPa m1/2
respectively [31]. The reported fracture toughness of 8YSZ ceramics
vary over a range of 0.93 MPa m1/2, depending on test method
and form of the material (pressed bar or thin foil) [9]. Measured
toughness values of pure 3YSZ are different, being primarily
dependent on parameters like starting powder, sintering parameter,
microstructure variables and testing technique [32]. It is well
Fig. 7. Arrhenius plot of grain-boundary conductivity of samples at low temperatures
established that grain size strongly inuences the toughness of 3YSZ
(T b 550 C).
ceramic specimens [33]. The reported fracture toughness of 3YSZ
samples (TZ-3Y, Tosoh, Tokyo, Japan) with an average grain size of
~0.5 m is about 6 MPa m1/2 [34].
range of applicability presented by McLachlan, can be found in
Fig. 8 illustrates the fracture strength of composite samples.
Ref. [29]. One of the most commonly used approach for investigating
Addition of 3YSZ particles to 8YSZ matrix has increased the strength of
transport properties in inhomogeneous media is Bruggeman's sym-
composite samples. As previously has been stated, fracture strength of
metric Effective Medium Theory (EMT) [30]. According to this model,
3YSZ and 3YSZ containing ceramics can be increased due to stress-
the individual conductivities of the composite components and the
total composite conductivity satises an equation of the type:

m1 1 = 1 + 2  + m2 2 = 2 + 2  = 0 6

where 1, 2 and are the conductivity of the individual phases and

the conductivity of composite respectively, and i denotes the volume
fraction of the phases, so that i = 1.
The values of electrical conductivity of composite samples with
different composition at temperature of 900 C are shown in Table 2. For
sake of comparison, the conductivity data of composite samples obtained
from application of symmetric Effective medium Theory (EMT) using the
values of 1 (8YSZ)= 0.12 ( cm 1) and 2 (3YSZ) =0.038 ( cm 1) are
also presented in Table 2.

Table 3
Bulk and grain-boundary activation energies at low temperatures

Specimen Bulk activation energy Grain-boundary activation

(eV) EBulk
a 0.03 energy (eV) EGain
a
boundary
0.04
Pure 8YSZ(8Y-TZ,TOSOH) 0.96 1.12
C1 0.96 1.1
C2 0.93 1.08
C3 0.90 1.08
Fig. 8. Variation of fracture strength of samples with 3YSZ content.
62 M. Ghatee et al. / Solid State Ionics 180 (2009) 5762
induced phase transformation phenomena [35]. The fracture strength
of brittle ceramics is generally lowered by defects such as aws,
cracks or inclusions, existing in sintered body. In uniaxial strength
measurements such as 3 or 4 point bending tests, the cracks which are
parallel to the tensile direction (parallel to the longitudinal direction)
in bar type specimens, do not lower the fracture strength of the test
specimen. However, in a biaxial strength measurement, more reliable
fracture strength can be measured because cracks existing in the disc
type specimen lower the strength, independent of the directions of
cracks [36].
It is important to remember that fracture strength of a brittle
material is not a characteristic material property, but depends on the
size of aws and their distribution, which in turn depends on the
fabrication process, specimen size and testing methods [37].
The fracture strength of pure 3YSZ and 8YSZ specimens, prepared
under the same conditions are also presented in Fig. 8.
As both strength and fracture toughness of composite samples
increase with increasing the amount of 3YSZ, it can be said that the
fracture strength of these materials is limited by aw size [14].
4. Conclusions
In this study, Composite electrolytes of 3YSZ/8YSZ with 10, 25 and
35 wt.% of 3YSZ were prepared. All the composite grades showed
appropriate structural stability during sintering. The presence of 3YSZ
particles in composite electrolytes hindered grain growth of cubic
phase so cubic phase had lower grain size than pure 8YSZ samples. It
was shown that addition of 3YSZ particles to 8YSZ matrix decreased
electrical conductivity of matrix at high temperatures (T N 550 C). The
lowest conductivity ( = 0.088 S/cm at T = 900 C) was obtained [26]
for sample with 35 wt.% of 3YSZ. On the other hand, conductivity of
specimens was enhanced with increasing 3YSZ content at low tem-
peratures (T b 550 C). Composite electrolytes showed lower activation
energy of electrical conductivity with respect to pure 8YSZ at both low
and high temperatures which can be due to the lower activation
energy of 3YSZ with respect to 8YSZ. It was also found that addition
of 3YSZ decreases the grain boundary contribution of the composite
electrolytes to total conductivity. The reduction of grain boundary
contribution to total conductivity along with lower activation energy of
composite electrolytes can be manipulated to design solid electrolytes
with improved performance and lower working temperatures.
The fracture toughness and strength of pure 8YSZ improved
by addition of 3YSZ particles. The highest fracture toughness and
strength were obtained for composite samples with 35 wt.% 3YSZ,
with magnitudes of 4.3 MPa m1/2 and 375 MPa respectively.
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