International Journal of Engineering and Advanced Research Technology (IJEART)

Volume-1, Issue-1, July 2015

AC Impedance Study of NiOx-GDC(1-x)

Nanocomposites
A.U. Chavan, L. D. Jadhav, S. Varma, S.R. Bharadwaj

batteries, gas sensors as well as membranes also. Further this

Abstract The synthesis of nanostructured Gd doped ceria kind of nano-composites usually shows conductivity
(GDC) and NiO has been reported by a simple and cost effective significantly higher than in both of the constituent phases.
solution combustion method. The powders were formed at low An electrical nano-composite NiO-GDC (gadolinium
temperature (~300C). The NiOx-GDC(1-x) where x = 0.1, 0.2,
doped ceria), which can be reduced in-situ during the first
0.3, 0.4, 0.5, and 0.6; nano-composites were formed by physical
mixing of these nano powders. The grain interior charge
operation of SOFC [6]-[7] is a suitable anode material for
transfer mechanism in these nano-composites was confirmed by Intermediate Temperature Solid Oxide Fuel Cell (IT-SOFC).
using impedance spectroscopic measurements in the frequency NiO acts as good catalyst for oxygen activation [8], and
range from 1 Hz to 10 MHz. The impedance spectroscopic provides good electrical conductivity while GDC mainly acts
measurements of the composites were examined in the as matrix to support the catalyst and prohibits the Ni from
temperature range100C-600C. The grain and grain boundary agglomeration under operating conditions [6]. It also provides
contributions to the electrical conductivity varied with the better matching of thermal expansion coefficient and
composition and temperature. The activation energies for both suppresses carbon deposition on electrodes in methane rich
grain and grain boundary conductivity decreased with increase
fuels [9]. The cermet nano-composites can substantially
in NiO content. The study also revealed that 40 % NiO content is
a percolation limit for NiO-GDC nano-composites. The effect of
enhance the hydrogen dissociation with reduced electrode
NiO addition on relaxation behaviour of these NiOxGDC(1-x) polarization resistance, and also increase the TPBs.
nano-composites is investigated for the first time using In recent years, NiO30-GDC70 has been exhaustively
impedance measurements. studied as an anode for the SOFC. But little work can be
found on the composite series. In our earlier work, we
Index Terms Electrical properties, Nano-composites, reported the structural, morphological and dc conductivity
Porosity, Relaxation. studies of solution combustion synthesized NiOx-GDC(1-x)
composites, where x = 0.1, 0.2, 0.3, 0.4, 0.5, and 0.6 [10].
Nevertheless, the electrical properties, which were found to
I. INTRODUCTION vary with varying amounts of the constituent phases, need to
be explored. Therefore in present report series of
Composites have gained substantial interest due to their NiOx-GDC(1-x) nanocomposites was intensively studied by
interesting electrical and magnetic properties and impedance spectroscopy. As impedance spectroscopy (IS) is
technological applications [1]. Basically electrical composite powerful method of characterizing the electrical properties of
is a physical mixture of two or more solid phases that materials and their interfaces. It is also capable to identify the
possesses mixed conductivity. Therefore, its electrical different relaxation frequencies owing to different charge
properties can be tailored by controlling the relative mole mechanisms. Park et al [9] have studied ac impedance of
fraction of the phases for specific applications. The properties NiO-YSZ (yttria stabilized zirconia) but there are no previous
of composites are strongly influenced by the microstructural studies on the ac impedance spectroscopy as well as
features such as grain size distribution and morphology, in relaxation behavior of NiO-GDC nano-composites. In the
addition to the electrical properties of each phase. In recent present work the effect of NiO variation on conduction
past, composites are widely used in solid oxide fuel cells mechanism in correlation with the relaxation is investigated
(SOFCs). For example, composite electrolytes exhibiting first time for the series of NiOx-GDC(1-x) nano-composites,
mixed H+ and O2- ionic conductivity have better efficiency for where x = 0.1, 0.2, 0.3, 0.4, 0.5, and 0.6.
direct operation of the hydrocarbon fuel [2]. Composite
electrodes exhibiting ionic and electronic conductivity not
only increase the length of triple phase boundary but also II. EXPERIMENTAL
provides thermal expansion coefficient match with electrolyte For the combustion synthesis of 10 mol% Gd doped ceria
hence improves electrode catalytic reactions and thereby fuel (GDC10: Ce0.9Gd0.1O1.95) nanopowder, metal nitrates
cell performance. An electrical composite consisting of ionic Ce(NO3)3.6H2O and Gd (NO3)3.6H2O were used as oxidants
and electronic phases are of great importance [1]-[5] in and glycine (C2H5NO2) as a fuel. The stoichiometric amounts
of metal nitrate precursors were dissolved in deionized water
Dr. Archana Chavan Postdoctoral Fellow at Chonnam National [11]-[12]. With the help of burette, fuel was added drop by
University, South Korea
Dr. L. D. Jadhav Assistant Professor at Department of Physics,
drop while stirring at room temperature to form homogeneous
Rajaram College Kolhapur, Maharashtra, India. solution of metal nitrates and fuel. The solution was stirred
Dr. Salil Varma Scientist-F at Chemistry Division, Bhabha Atomic and heated on a magnetic stirrer for the removal of moisture
Research Centre, Trombay, Mumbai - 400085, INDIA. and hence to form gel. The formed gel was kept on preheated
Prof. S. R. Bharadwaj Senior Scientist Chemistry Division, Bhabha
Atomic Research Centre, Trombay, Mumbai - 400085, INDIA.
hot plate to combust [13]. The resultant nanopowder of
GDC10 was then collected and calcined in air at 600C for 2h.

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 AC Impedance Study of NiOx-GDC(1-x) Nanocomposites

to remove any carbon based residues that might have

(1)
remained in the oxide powder. Similar procedure was
repeated to form NiO wherein Ni(NO3)2.6H2O was used as
The variation of lattice parameters a1and a2 with NiO
metal nitrate and glycine as fuel. Ash obtained was calcined at
content was studied and it is shown in Fig. 1. From Fig. 1 it is
500C for 2h. The morphology of the particles in ceramic
observed that there is no deviation in both lattice parameters
materials is a consequence of the preparation method, and the
from the reported values, 5.418 for GDC and 4.179 for
combustion method favors porous nanoparticles. This method
NiO.
can produce homogeneous powder composed of small and
uniform particles. The nano powders of GDC and NiO were
Density Measurements
characterized by XRD, FTIR and SEM which have been
reported in our previous report [10-12].
X-ray density of individual phases was calculated by using
NiOx-GDC(1-x) where x = 0.1, 0.2, 0.3, 0.4, 0.5, and 0.6
the formula,
were formed by grinding the nano powders of NiO and GDC
in agate mortar for 3h. These nano-composite powders were
pressed in the form of cylindrical pellets by applying a
uniaxial pressure of 7 tons for three minutes with the help of (2)
hydraulic press. The formed pellets have 13mm diameter and
1mm thickness. Extreme care was taken to see that Where, M is the molecular weight,
palletization of all the samples was done under identical a is the lattice parameter, and
conditions. All the pellets were pre-sintered at 900C for 2h N is the Avogadros number.
and finally sintered at 1000C for 8h at heating rate of 1C Similarly X-ray density of nanocomposite samples was
/min in air atmosphere. The process of pre-sintering gives calculated by using the formula,
slow heating of the pellets with removal of carbonaceous
products if any, formed during palletization and hence no
formation of cracks in the samples during final sintering still (3)
at higher temperatures. These nanocomposite samples were
named as N1G1, N2G1, N3G1, N4G1, N5G1, N6G1 Where,
respectively for x = 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 in M1 = (1-x) (Molecular weight of GDC)
NiOx-GDC(1-x). M2 = x (Molecular weight of NiO)
Structural studies of these samples were carried out by V1= M1 / x1 and V2 = M2 / x2
XRD (Phillips-3710 powder X-ray diffractometer) in the 2 and x1 and x2 are X-ray density of GDC and NiO,
range of 20 - 80 using CuK1 radiation (= 1.54056). The respectively.
XRD patterns were compared with standard JCPDS files of The X-ray density of the all nanocomposite samples
NiO (78-0643; cubic NiO) and GDC10 (75-0161). The calculated using equation (3) is tabulated in Table I.
conventional Archimedes method was used to measure the Experimental density of all the samples was calculated by
density of these samples. The ac electrical conductivity Archimedes principle. It is more appropriate technique for the
measurements were carried out in air atmosphere with the determination of density of porous materials. It is seen from
help of electrochemical impedance spectroscopy in the table that both X-ray and actual density decrease with an
temperature range of 100C to 600C using platinum increase in NiO content. The results were used to estimate
electrodes. Pt paste obtained from Ma TecK Germany was percentage porosity tabulated in Table I.
applied on both surfaces of pellets and after that the pellets
were heated at 600C in air for 4h to remove the organic
binders. The complex impedance was measured at different
signal frequencies ranging from 0.1Hz to 10 MHz using a
Solartron SI 1260 impedance analyzer. The impedance
response was studied in the temperature range 100C to
600C. These measurements were performed at temperature
interval of 25C; each temperature was kept constant with an
accuracy of 5C during the measurement. Sufficient
stabilization time was ensured at each particular temperature.
The data analysis was done by using Z-view frequency
response analyzer.

III. RESULTS AND DISCUSSION

Structural Studies
The XRD patterns obtained for all NiOx-GDC(1-x) Fig. 1 Variation of lattice parameters with NiO content.
nanocomposite samples were compared with the JCPDS files
of NiO (78-0643; cubic NiO) and GDC10 (75-0161). The Impedance spectroscopy
XRD study has been already reported in our previous report
[10]. From the XRD patterns, the lattice parameter a1 and The mechanism of the composite electrodes has been
a2 for NiO and GDC respectively was calculated using the illustrated by Zhao et al. [14] and it can also be applied to the
relation, NiO-GDC nano-composites prepared in this study. They

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 International Journal of Engineering and Advanced Research Technology (IJEART)
Volume-1, Issue-1, July 2015
applied two phase composite model and percolating model. corresponding grain boundary resistance (R2) and grain
According to the two-phase composite model, both e- and O2- boundary capacitance (CPE2). CPE is a non- intuitive circuit
transfer can be achieved respectively through continuous element that represents the responses of real-world systems,
networks formed by NiO and GDC. While in the percolating and it has been proposed to explain a number of phenomena
model, the TPBs must be electrochemically active through the on the basis of the common thread that there exist some
percolation of the ionic and electronic phases to the bulk distributions of some physical properties in the heterogeneous
electron and ion conductors at either end of the interface. In system [16]. It is the constant phase element with minimum
cermet, there is large amount of TPB regions. The ionic phase chi square value. The inductances of the circuits, L, may be
and percolating metal oxide phase provide continuous paths the result of the Pt current/voltage probes or the
(two phase composite model) from TPBs to the bulk gas, high-frequency phase shift of the electrochemical equipment.
whereas electronic and ionic phases (percolating model), The diameter of the semicircles was found to decrease with
enable these TPBs to remain active, where redox reaction is increase in NiO content in the nanocomposite. This shows
considerably enhanced. that the bulk as well as grain boundary and hence the total
The NiO-GDC composite is a heterogeneous composite. resistance decrease with increase in NiO content. As NiO
The two phases in this composite have different electrical content increases, the grain growth of GDC is retarded and
conductivities. The NiO is electron conducting (p-type results into decreased grain size whilst number of NiO grains
semiconducting) while GDC is ion conducting. Therefore, which are more conducting is increased. This results into
their ac conductivities are presumed to be affected by NiO increased grain conductivity. The grain is more resistive than
content, which is studied with impedance spectroscopy. the grain boundary for GDC rich composites (N1G1 and
The impedance spectroscopy is an efficient tool to resolve N2G1) while the grain boundary is more resistive than the
the contribution from various microscopic elements such as grain for NiO content 30 mol%. Similar studies by Park et
the grain, grain boundary, and electrodes to the total al. [9] carried out on NiO-YSZ composites showed that upto
conductivity response. Cole-Cole and Bode representation of 40 mol % NiO content, Rgb > Rg and for higher NiO content Rg
impedance effectively probes the series or additive processes. > Rgb. The dissimilarity is due to difference in particles size of
The Cole - Cole representation of impedance data is the plot the starting materials used in this work [10] and that reported
of real part of impedance (Z) verses negative of imaginary in [9]-[10], [16]-[17].The less resistive grains are, obviously,
part (Z). It is also called as Nyquist plot. It depicts the series attributable to nano-sized grains.
or additive processes in solids such as non-depletive grain From Fig. 2 it can be observed that in the low temperature
resistance (Rg) and depletive grain boundary resistance (Rgb) region, the composites N1G1 to N4G1 have spike at low
for ion transport [15] i.e. total resistance (Rt) of the material at frequency which is due to electrode polarization. On the
the given temperature is, contrary, the composites N5G1 and N6G1 showed no spike.
This predicts that the electrode response is merely due to
Rt = Rg + Rgb (4)
(a) (b)

The Nyquist plots of all composites were recorded in the

temperature range of 100C to 600C and are shown in Fig.2
and 3.
(a) (b)

(c)

(c) (d)

(d)

Fig. 3 Nyquist plots of (a) N1G1and N2G1 (b) N3G1 and

N4G1 (c) N5G1 and N6G1 at 475C (d) Equivalent circuit
employed for evaluating the grain and grain boundary
resistance.

Fig. 2 Nyquist plots of (a) N1G1, N2G1 (b) N3G1, N4G1 (c) GDC/Pt interface upto 40% NiO, which is changed to NiO/Pt
N5G1 and (d) N6G1 at 200C. interface above 40 mol% NiO i.e. for NiO rich composites.
Thus negligible electrode resistance is observed for NiO/Pt
The best fitting result of the impedance spectra for all six and hence no electrode response is observed. 375C the
samples was achieved with the equivalent circuit of L1 inductive loop is observed, for N1G1 and N2G1, at lower
(R1CPE1) (R2CPE2) as shown in Fig. 3(d), indicating at least frequencies. So far the nature of these inductivities is not well
two different electrode processes corresponding to high- and understood and only some rough explanations have been
low-frequency arcs. The first loop contains resistance given. This inductive loop may be due to impedance arising
(R1)corresponding to grain (bulk) resistance and grain from the chemical species segregated along the grain
capacitance (CPE1) and the second loop contains resistance

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 AC Impedance Study of NiOx-GDC(1-x) Nanocomposites

boundaries [18]. But as this loop appears above 375C, very

similar to the presence of electrode contribution at higher
temperatures, more likely it is due to the accumulation of Table I Variation of density, activation energy (Ea) and
adsorbed species at the interface of electrode (here Pt) and relaxation time () with NiO content.
sample. With increasing NiO content in the composites, the
inductive loop is not observed anymore in the investigated
frequency range of Nyquist plot. Density Activation Energy Relaxa
(eV) t-ion
Sampl
Time
Fig. 3 shows that the low frequency tail starts to appear e X-ray at
Name Experimenta Grai Grain
above 475C in case of N5G1 and N6G1. This ascertains that Density
l Density (%) n Boundary 200C
the main charge carriers at high temperature are the oxygen (gm/cc) (S)
vacancies of GDC, while at low temperature, the charge N1G1 7.20 94.05 0.88 1.25 1.59
carriers are electron hole pairs of NiO [9]. N2G1 7.16 93.48 0.74 0.75 1.00
N3G1 7.12 92.32 0.69 0.64 0.40
Further the grain boundary arc was depressed; indicative of N4G1 7.07 91.30 0.61 0.76 0.25
coexistence of several processes with different relaxation N5G1 7.03 88.82 0.59 0.75 0.12
times. This distribution of relaxation processes might be due N6G1 6.99 86.84 0.45 0.68 0.10
to different ionic species and mechanisms involved in charge
transport. Variation of Z with frequency (f) at temperature NiO content, the relaxation peak shifts towards the higher
200C for all the samples has been shown in Fig. 4a and 4b, frequency side. More and more free charges may accumulate
which helps to probe the relaxation processes. on the interface resulting in a decrease of relaxation time [20].
The relaxation time is related to the response of the charge It also shows that the height of the peak decreases with the
carriers to an applied ac field. The relaxation time is defined NiO content as relaxation time decreases (Table I).
as, Temperature dependence of relaxation frequency was also
studied for nano-composites in-particular. It was observed
that the relaxation peak shifts to higher frequency with rise in
(5) temperature, which is due to reduction in the time constant
(RC) of the relaxation associated with both inter and intra
Where f is the relaxation frequency that corresponds to the grain charge transport, indicative of thermally activated
maximum of the peak [19] and represents the mean time process. This leads to successive flattening of the relaxation
between two consecutive jumps of oxygen ion vacancies and peaks.
it is computed from peak frequency obtained from Fig. 4a and
4b. The dependence of the total electrical conductivity (T) on
Relaxation processes corresponding to both grain boundary NiO content, shown in Fig.5, reveals that increasing
and bulk were present but the relaxation peaks were not sharp semiconductor content has a strong effect on the transport
indicating non-Debye type behavior. properties of the composite. This also shows that increasing
A loss peak observed in all the curves at high frequency NiO content results in large magnitudes of (T) and that such
region may be due to the interfacial polarization at a particular a feature is much more pronounced at low temperatures (T
frequency range for each bulk composite. With increasing 300C). This pronounced increase of (T) is related to the
increasing electronic charge carriers with increasing NiO
(a) (b)
content and indicates that the percolation threshold is
achieved at 40 mol % of NiO in agreement with the previous
results [10]. So analogous to the results in [10], the studied
compositions were identified in three different NiO
concentration regions as (i) < 20 mol % of NiO (ii) 30-40
mol% of NiO (iii) 50 mol % of NiO. These regions indicate
that distinct transport mechanism takes place depending on
the NiO content. In region (i) the main charge carriers are the
oxygen ions, for further increase in the NiO content (region
(ii)), mixed conduction process is more likely to occur, and in
region (iii) the main charge carriers may be the electron holes
of NiO and GDC10 grains act as insulating scattering centers.

Assuming that these oxides exhibit polaronic conduction in

the temperature range 100-500C which is governed by a
small polaron hopping mechanism,

Fig. 4 (a) Variation of Z with logarithmic frequency at

200C for N1G1 and N2G1. (b) Variation of Z with (6)
logarithmic frequency at 200C for samples N3G1 to N6G1; The plot of ln (*T) vs 1000/T (Fig. 6), called as Arrhenius
Inset: magnified view for sample N6G1. plot, shows linear relationship, validating above assumption
[21]-[22]. Basically there are two regions in the Arrhenius

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 International Journal of Engineering and Advanced Research Technology (IJEART)
Volume-1, Issue-1, July 2015
plot, which may be due to dominance of electronic and ionic IV. CONCLUSION
charge transport mechanism in the nanocomposite samples at Electrical nano-composites of NiOx-GDC(1-x) were
different temperature regions. At high temperatures, the successfully prepared by mixing combustion synthesized
nano-powders. All nano-composites were found to be well
crystalline with no solid solution among the constituent
phases. Crystallite size of these samples was in the range of
20-26 nm. Density measurement showed decrease in density
with increase in NiO content. The electrical properties of
NiO-GDC nano-composites were studied for the entire
composition range of composites by using impedance
spectroscopy. It was evidenced from the ac impedance spectra
that the grain was more resistive than the grain boundary for
low NiO content while reverse was true for high NiO content.
The total conductivity results manifested that the transport
Fig. 5 Dependence of electrical conductivity on NiO content mechanism has changed from oxygen vacancies of GDC to
at different temperatures. electron holes of NiO with increase in NiO content. This was
corroborated by the fact that at high temperatures, the
nano-composites with NiO content 40 mol% showed almost
same conductivity. The activation energies for grain and grain
boundary conduction were decreased with NiO content. The
electrical conductivity and activation energy showed
percolative behavior with 40 mol % NiO composition. The
relaxation studies showed that processes corresponding to
both grain and grain boundary were present. Further, it
revealed that the relaxation time decreased with both NiO
content and the temperature.
Fig.6 Arrhenius plots for N1G1 to N6G1 in the temperature ACKNOWLEDGMENT
range 200-600C.
The authors are very much thankful to Board of Research in
nano-composites with NiO content 40 mol%, showed Nuclear Sciences (BRNS) for financial assistance. A. U.
almost same conductivity. This again supports that the main Chavan is thankful to Council of Scientific and Industrial
charge carriers at high temperature are the oxygen vacancies Research (CSIR), New Delhi, India for financial support
of GDC 10 whose concentration decrease with NiO content. through Senior Research Fellowship.
The GDC 10 grains act as insulating scattering centers to
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 AC Impedance Study of NiOx-GDC(1-x) Nanocomposites

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Dr. Archana Chavan is currently working as a Postdoctoral Fellow at

Chonnam National University, South Korea. She joined the University of
Johannesburg (UJ), South Africa, as a post-doctoral research fellow in 2014.
Dr. Chavan received her PhD from Shivaji University, Kolhapur, India, in
2013 in physics. Her research interest is focused on the chemical synthesis of
nanostructured materials and their applications in energy storage and
conversion devices and sensor technology.

Dr. L. D. Jadhav is currently working as an Assistant Professor at

Department of Physics, Rajaram College Kolhapur, Maharashtra, India. She
was Principal Investigator (P.I.) of BRNS funded project and currently she is
P.I. of Defense Research and Development Organization (DRDO) project.
Total 3 Ph.D. students completed their degree and currently there are 5
students are working under her guidance for Ph.D. Her research interest is
focused on the synthesis of nanostructured materials and their applications
in SOFCs and batteries.

Dr. Salil Varma is currently working as a Scientist-F at Chemistry

Division, Bhabha Atomic Research Centre, Trombay, Mumbai - 400085,
INDIA. His research interest is focused on the synthesis of catalyst materials
and their applications in SOFCs.

Prof. S. R. Bharadwaj is currently working as a Senior Scientist

Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai -

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