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Magnetic, Electrical and Humidity Sensing Properties of Multiferroic GdCrO 3

Nanoparticles Fabricated by Metal Organic Precursor Method

Article  in  ChemistrySelect · September 2022

DOI: 10.1002/slct.202202547

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 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547

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Magnetic, Electrical and Humidity Sensing Properties of

Multiferroic GdCrO3 Nanoparticles Fabricated by Metal
Organic Precursor Method
Irfan H. Lone,[a, b] Huma Khan,[a] Irshad A. Wani,[c] Arvind Kumar Jain,[d] and Tokeer Ahmad*[a]

Monophasic GdCrO3 nanoparticles have been fabricated by
ethylene glycol-assisted metal citrate precursor method. The
as-prepared nanoparticles have been characterized for phase
purity, size and morphology by using powder X-ray diffraction,
transmission electron microscopy and scanning electron micro-
scopic techniques. GdCrO3 nanoparticles showed excellent
crystallinity with an average particle size of 78 nm and high
specific surface area of 184 m2 g 1. The two band gap values of
1.9 eV and 2.3 eV were calculated using K M function of the
UV-visible diffuse reflectance spectroscopy. Magnetic results of
GdCrO3 nanoparticles possess the well defined ferromagnetic
loop, which confirms the ferromagnetic characteristics of these
nanoparticles. Our results further exhibit improved P E loop for
GdCrO3 nanoparticles showing ferroelectric behaviour at room
temperature for the first time which indicates the presence of
multiferroic nature. The dielectric constant and dielectric loss of
sintered/unsintered pellet of GdCrO3 were measured as a
function of frequency and temperature. Lastly, the humidity
sensing parameters of GdCrO3 nanoparticles have also been
reported.

Introduction
temperature.[10] The rare earth chromites and ferrites seem to
In the recent past, multiferroics have attracted a great interest be a new possible candidate for multiferroic characteristics,
as multifunctional materials[1–3] and depicts enormous applica- with perovskite ABO3 structure and play a crucial role in
tions in memory devices, sensors and actuators.[4–6] The ferroic fabricating solid oxide fuel cells, catalyst material to design
properties in such materials may be ferrotoroidicity, ferroelas- electrodes and chemical sensors.[1,2,11] The possibility of ferro-
ticity, ferroelectricity and ferromagnetism.[7] Particular attention electric property in rare earth orthochromites was earlier
has been paid to the synthesis of nanocrystalline orthoferrites discussed.[2,12,13] The mechanical grinding of the oxides (Gd2O3,
due to their functional properties having huge diversity and Fe2O3 and Cr2O3) was required for the solid-state powder
makes them the ideal choice to study the electric and magnetic synthesis of GdFeO3 and GdCrO3 at high calcination temper-
properties.[1,8, 9] Earlier reports have shown strong magneto- ature of around 1800 °C.[14] These stringent conditions lead to
electric coupling by the single crystals of DyFeO3 and GdFeO3 bulk sample and the procedure involving a higher calcination
but the multiferroic nature occur only at very low temperature come with limitations like high porosity, poor
homogeneity and poor control of grain size, which adversely
affects the functional properties of the materials. The successful
[a] I. H. Lone, H. Khan, T. Ahmad
preparation of nanosized rare-earth (orthoferrite and chromite)
Nanochemistry Laboratory,
Department of Chemistry, with precise stoichiometry faces a synthetic challenge. The
Jamia Millia Islamia, advantage of low temperature preparation yields materials of
New Delhi-110025, India small particle size with high surface area and obviously it is
E-mail: tahmad3@jmi.ac.in
required to prepare nanoscale GdCrO3 compound, however the
Homepage: https://www.jmi.ac.in/tahmad3
[b] I. H. Lone detailed investigation was not reported in literature till date.
Department of Chemistry, Several methods such as reverse micelle,[15,16]
[17,18] [19]
University of Kashmir, solvothermal, hydrothermal, sonochemical,[20,21] poly-
Hazratbal, Srinagar-190006, [22,23]
meric citrate precursor and co-precipitation[24,25] methods
Jammu & Kashmir, India
[c] I. A. Wani etc. are available in literature for the synthesis of metals, metal
PG Department of Chemistry, oxide and complex metal oxide nanoparticles. Gadolinium
Govt. Postgraduate Degree College Bhadarwah, based ferrites were reported in literature by using sol–gel
University of Jammu,
process,[26] hydrothermal,[27] soft-chemical[28] and colloidal
Jammu & Kashmir,
182222, Jammu, India synthesis[29] methods. Pulsed laser deposition,[30] hydrothermal
[d] A. K. Jain method,[31] metathesis of metal chlorides,[32] decomposition of
School of Basic and Applied Sciences, co-precipitated precursors,[33] hydrazine method,[34] spray
Galgotias University,
pyrolysis[35] and polyol mediated synthesis[36] have been used
Greater Noida-201306, UP,
India earlier for the synthesis of rare earth chromites. In this study,
This publication is part of a Special Collection on ‘’Celebrating 100 years of we report the synthesis of GdCrO3 nanoparticles by using
JMI University’’ (JMI-2022). Please follow this link to visit the whole collection. simple and inexpensive synthetic metal organic precursor

ChemistrySelect 2022, 7, e202202547 (1 of 8) © 2022 Wiley-VCH GmbH

 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547
approach. As-prepared nanoparticles (NPs) were investigated
by means of X-ray diffraction, UV-visible, transmission electron
microscopy (TEM) and scanning electron microscopic (SEM)
studies. The surface area, magnetic, electrical and sensing
properties have also been measured that established the high
Figure 1. Powder X-ray diffraction pattern of GdCrO3 nanoparticles.
Figure 2. (a) TEM and (b) SEM micrographs of GdCrO3 nanoparticles.
ChemistrySelect 2022, 7, e202202547 (2 of 8)
quality nanocrystalline multiferroic material which could be
applied for the fabrication of novel devices.
Experimental Section
The following analytical grade chemicals were used as received
without any further purification: Gadolinium (III) nitrate hydrate
(Alfa Aesar; 99.9 %), chromium (III) nitrate nonahydrate (Alfa Aesar;
99.9 %), ethylene glycol (SD fine-chem Ltd; 99%) and citric acid
(Spectrochem; 99%). For the synthesis of GdCrO3 nanoparticles
using polymeric citrate precursor route, initially the molar contents
of ethylene glycol (EG): citric acid (CA): chromium nitrate were
taken at the fixed molar ratio of 10 : 40 : 1. The stirring of the
mixture was performed at room temperature for 2 h to achieve
clear solution of the reaction precursor. After achieving complete
solubilization, 25 ml of 0.1 M aqueous solution of gadolinium
nitrate was added to the solution and allowed for stirring further
for 2 h. As-prepared solution was then heated at 70 °C for 2 h to
remove excess water and to accelerate the esterification reaction
between EG and CA. The viscous solution as-obtained was then
heated in muffle furnace at 135 °C for 20 h. Note that no turbidity
could be seen at this stage during the polymerization reaction. The
resin was then charred at 300 °C for 3 h in a muffle furnace which
turned into the black mass, referred to as precursor, and was finely
ground to the powders with Teflon rod. As-received precursor was
annealed at desired temperature for 12 h in high temperature tube
furnace to obtain the nanocrystalline powders of GdCrO3 which
was green in color.
Characterization Techniques
Powder X-ray diffraction (PXRD) studies have been explored on
Bruker D8 Advance X-ray diffractometer using Cu Kα radiations of
wavelength of 1.54056 Å fitted with Ni-filter. The diffraction
patterns were obtained in the 2θ range of 10 ° to 70 ° at the scan
rate of 0.05 °/sec. TEM investigations have been performed on FEI
Technai G2 20 TEM operated at 200 kV and equipped with digital
imaging and 35 mm photography system. A small amount of the
fine powders was dispersed in ethanol, and sonicate for 30 minutes
UP-500 ultrasonicator. A drop of the dispersion was placed on a
carbon coated copper grid to make the TEM film. SEM images were
taken using ZEISS EVO 50 SEM operated at 30 kV acceleration
voltages. The powder samples of GdCrO3 NPs were dissolved in
ethanol and the band gaps were determined using a Perkin-Elmer
double-beam Lamda-35 spectrophotometer. Surface area studies of
the samples have been carried out at 77 K temperature using Nova
2000e BET surface area analyzer procured from Quantachrome
Instruments Limited, USA using the procedure as reported
elsewhere.[20,25] For dielectric and ferroelectric studies, a pellet of
10 mm circular diameter was prepared by mixing GdCrO3 nano-
powders with 2–3 drops of 5 % PVA solution as binder agent which
was allowed to dry and dried powder was then pelletise at a
pressure of 5 tons. Two pellets were made, one without sintering
and other was sintered of GdCrO3 nanopowder in air at 1000 °C for
8 hrs. Silver paste (Ted Pella) was applied to both faces and dry in
oven at 90 °C for 1 h. The experiments of dielectric properties have
been carried out using 6505 P HF-LCR meter procured from Wayne
Kerr electronics, UK in 100 kHz - 2 MHz frequency range and 25 °C
to 450 °C temperature range. Room temperature ferroelectric study
of the un-sintered pellet of GdCrO3 was performed at 50 kHz
frequency at different applied voltages on P E loop tracer procured
from M/s Radiant Instruments, USA. The magnetization measure-
ments have been done using MPMS SQUID magnetometer at an
© 2022 Wiley-VCH GmbH
 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547
Figure 3. (a) UV-Visible reflectance spectra, (b) converted K M plot and (c) band gap plot of as-prepared GdCrO3 nanoparticles.
external magnetic field of � 60 kOe in the temperature range of 5
to 300 K. The humidity sensing was studied by the sensor fitted in
as series on SHAW dew point meter (Model: SADPTR R).
Results and Discussion
Figure 1 shows the XRD pattern of GdCrO3 nanoparticles. All
the reflections were indexed on the basis of pure GdCrO3
having orthorhombic structure. The peaks of decreasing
intensity could be assigned to the planes which matches
correctly with the standard X-ray diffraction pattern of GdCrO3
(JCPDS. 25–1056).
To examine the concrete size and morphology of GdCrO3
NPs, the samples were systematically examined by electron
microscopic investigations. The average particle size of the
sample was determined by taking the average diameters of
∼ 50 nanoparticles manually from the different micrographs.
The shapes, morphology and size of GdCrO3 NPs were
investigated by means of TEM and SEM studies as shown in
figure 2 (a, b). Figure 2 (a) shows the representative TEM image
of the GdCrO3 NPs, exhibiting monodisperse and hexagonal
particles. The average particle diameter, based on the dimen-
sion of 10 particles, was found to be 78 nm. SEM micrograph as
shown in figure 2 (b) exhibits the uniformity and well
dispersion of GdCrO3 NPs.
Optical characterization of GdCrO3 nanoparticles was
carried out by measuring the reflectance spectra at room
ChemistrySelect 2022, 7, e202202547 (3 of 8)
temperature. The optical energy band gap was determined
using the Tauc’s formula[37] by applying the Kubelka-Munk
equation. It can be seen from the reflectance spectra of GdCrO3
NPs as shown in figure 3 (a, b&c) that there are two prominent
peaks at about 464 nm and 608 nm which corresponds to the
transition of O 2p-Cr 3d (t2g) and Cr 3d (t2g)-Cr 3d (eg)
respectively.[38] In this case, the best fit of [F(R).Eg]n versus Eg
(photon energy) was obtained for n = 2 and provide the Eg
values by extrapolating the linear portion of the curve to the
point y-axis = 0 as shown in figure 3 (c). The two band gap
values of 1.9 eV and 2.3 eV were found as shown in figure 3 (c)
that may be associated to the transitions of chromium ion from
the ground level.[39]
BET surface area measurement is the versatile method
which is used to express the specific surface area, type of pores
and the pore size distribution of GdCrO3 nanoparticles. The BET
surface area of GdCrO3 NPs is shown in figure 4 (a) and its value
is found to be 184 m2 g 1. This value of GdCrO3 surface area is
significantly higher than the reported values so far in the
literature.[40] The shape of the isotherm of GdCrO3 NPs is typical
type IV isotherm as shown in figure 4 (b). The DA plot as shown
in figure 4 (c) confirmed the predominance of mesopore of
radius 14.8 Å of GdCrO3 nanoparticles.
Dielectric properties (dielectric constant, ε and dielectric
loss, D) of GdCrO3 NPs were measured by using high frequency
LCR meter. The temperature variation of dielectric constant (ε)
at different frequencies of GdCrO3 pellet with and without
© 2022 Wiley-VCH GmbH
 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547
Figure 4. (a) BET, (b) N2 adsorption isotherm and (c) DA plots of as-prepared GdCrO3 nanoparticles.
sintering is shown in figure 5 (a, b). It seems that the sample
might be a dielectric relaxor, and therefore dielectric constant
increases with increase in temperature and became maximum
at Curie temperature (Tc). Such anomalies in GdCrO3 may be
related to ferroelectric phase transition at particular temper-
ature. For sintered and unsintered pellets, the observed Tc is
nearly 312 °C and 390 °C, that could be associated to the
constrained grains. Such type of behaviour has also shown by
rare earth chromites (LnCrO3, Ln = Ho, Er, Yb and Lu) which
undergo a transition in the temperature range 439 K–485 K,
accompanied by a maximum in the dielectric constant.[41]
Hiroshima et. al. has reported an expression between Tc and
internal stress developed in the constrained grains at the phase
transition temperature. The bigger grained structure and
change in internal stress can shift Tc to higher temperature
which may be expected in the pellets due to higher sintering
temperature.[42] It can be observed that the dielectric constant
increases with the increase of sintering temperature and this
phenomenon was also found in other dielectrics.[43] Frequency
dependence of ε and D at room temperature of GdCrO3 NPs is
shown in figure 6 (a), which shows that the dielectric properties
(ε and D) of GdCrO3 NPs decrease with the increase in
ChemistrySelect 2022, 7, e202202547 (4 of 8)
frequency. The decrease in dielectric constant with increase in
frequency might be attributed to the fact that any species
contributing to polarization was found to lag behind the
applied field at higher frequencies. The temperature variation
of ε and D of GdCrO3 NPs at the frequency of 1 MHz was also
studied as shown in figure 6 (b). Both the dielectric parameters
(ε and D) were stable upto the 200 °C and thereafter both
abruptly increases and reach to the peak maxima at 300 °C,
although there is a little shift in the peak maxima between the
dielectric constant and dielectric loss. The observed dispersion
behaviour of the dielectric loss is attributed to the higher
domain mobility near the Curie temperature. Temperature
dependence on dielectric properties have also been reported
in chromium based YCrO3 and it was found that there is a
maximum value of dielectric peak at around 400–450 K. This
maximum value of dielectric peak shifts towards lower value of
temperature compound with leaky dielectric property arises
from local non centro-symmetry.[44] Monotonous increase in the
dielectric constant at low frequencies was not found in GdCrO3
compound as has been reported in case of YCrO3 thin films.[45]
But the dielectric phase transition properties found in prepared
© 2022 Wiley-VCH GmbH
 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547
Figure 5. Temperature dependence of dielectric constant of a sintered and
(b) un-sintered pellet of GdCrO3 nanoparticles.
GdCrO3 nanoparticles; has also been found in pellets and thin
films of YCrO3 that lends the evidence of a ferroelectric phase.
Temperature and magnetic field dependent dc magnet-
ization measurements of GdCrO3 nanopowders were carried
out at the temperature range of 5 to 300 K using the super-
conducting quantum interference device magnetometer at an
external magnetic field of � 60 kOe. The awl-shaped hysteresis
loop at 3 K of GdCrO3 nanoparticles is shown in figure 7 (a)
with weak ferromagnetic magnetization which is attributed to
the canted ordering called canted antiferromagnetism with a
weak magnetic moment of rare earth chromites. This behaviour
may be associated to the splitting of energy level of Cr3 + ions
in rare earth chromites in an octahedral coordination which
results the half-filled (t2g) orbits occupied by three parallel-spin
electrons and high energy (eg) empty orbits.[46,47] Secondly, the
bond angle (Cr O Cr) slightly deviates from 180° due to the
Dzyaloshinskii-Moriya type antisymmetric exchange interaction
between Cr3 + Cr3 + ions which results the imperfect super-
exchange interaction below the Neel temperature.[48,49] The
values of saturation magnetization, remanent magnetization
and coercive field were found to be 126 emu g 1, 9.5 emu g 1
and 432 kOe, respectively for the GdCrO3 nanoparticles. The
ChemistrySelect 2022, 7, e202202547 (5 of 8)
Figure 6. Variation of ε and D of GdCrO3 nanoparticles with (a) frequency and
(b) temperature.
temperature dependence magnetisation curve is also plotted
(figure 7b) which is shows the Neel temperature at 165 K which
is approximately similar to 170 K as reported literature.[50]
Polarization-electric field (P E) hysteresis studies for ferroe-
lectricity in nanocrystalline GdCrO3 have been carried out at
50 kHz under different applied voltages. Room temperature
P E loops was observed in GdCrO3 NPs by plotting a graph
between polarization vs. electric field under the applied voltage
range of 100 V to 500 V as shown in figure 8 (a, b) which
showed the remanent polarization (PR) of 0.00022-0.0152
μCcm 2, the saturation polarization (PS) of 0.0125–
0.060 μCcm 2 and the coercive field (EC) of 0.05–1.529 kV cm 1.
Note that the area under the loop decreases on decreasing the
applied voltage, therefore the P E characteristics (Ps, Pr and Ec)
of GdCrO3 nanoparticles strongly dependent on the applied
voltage. The relatively small, slim and non-ideal loop at
100 volt indicates that the applied voltage is not high enough
to obtain the significant loop but evidences, the presence of
room temperature ferroelectricity. In the prepared GdCrO3
nanoparticles, it can be claimed with reported earlier YCrO3
type compounds that the origin of phase transition (para-
electric-ferroelectric transition) is due to local non-centrosym-
© 2022 Wiley-VCH GmbH
 Research Article
ChemistrySelect doi.org/10.1002/slct.202202547

Figure 7. (a) M H hysteresis plot of GdCrO3 nanoparticles. Inset shows the loop closer look, and (b) magnetization versus temperature curve while inset shows
blown up curve.

Figure 8. (a) Full and (b) closer view of P E hysteresis loops of GdCrO3
nanoparticles.
Figure 9. Variation of capacitance with (a) relative humidity and (b)
repeatability time for GdCrO3 nanoparticles.

ChemistrySelect 2022, 7, e202202547 (6 of 8) © 2022 Wiley-VCH GmbH

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metry caused by the Cr displacement along the z-direction of
the perovskite-type unit cell.[51–56]
The change in the capacitance with moisture content of
GdCrO3 nanoparticles measured by impedance analyzer at
1 kHz frequency is shown in figure 9 (a). The capacitance value
increases slightly below 80 % and then sharply increases by
moisture content and has been manifested that the dielectric
constant and capacitance will increase with water adsorption
as were found in other ionic materials.[55–57] The repeatability
tests for GdCrO3 sensor at moisture level for the several
moisture cycles is shown in figure 9 (b), which shows that there
exists little repeatability for sensor output and the response
and recovery times of the sensor are occurring at the same
pace. This may be due to that the absorption and desorption of
water molecules which take place at the similar rate.
Conclusion
Monophasic and highly crystalline GdCrO3 nanoparticles have
been prepared successfully by using polymeric citrate precursor
route. The nanoparticles have been investigated by means of
XRD, TEM, SEM and BET surface area studies. The optical
properties by UV visible diffuse reflectance indicate the band
gap of as-prepared GdCrO3 nanoparticles lies in the visible
range. The frequency and temperature variation of dielectric
properties of GdCrO3 nanoparticles was also reported. Multi-
ferroic natures of GdCrO3 nanoparticles were established by
well defined ferromagnetic and room temperature ferroelectric
studies with reasonably significant values. We believe that the
nano-crystalline GdCrO3 is definitely an interesting material,
which opens the perspective of combining optical, sensing,
ferroelectric and ferromagnetic functionalities in electronic
devices.
Acknowledgements
TA thanks the SERB-DST Govt. of India research scheme (EMR/
2016/001668) for financial support. IHL thanks to UGC New Delhi
for research fellowship. The authors thank to IIT-Delhi for XRD
and SEM analysis, AIIMS, New Delhi for electron microscopic
studies and Prof. K. V. Ramanujachary (Rowan University USA) for
carrying out magnetic measurements. Special thanks to Dr. V. R.
Reddy (UGC-DAE Indore) for P E measurements. Authors also
acknowledge the measurement support provided through DST
PURSE program at CIF, Jamia Millia Islamia.
Conflict of Interest
The authors declare no conflict of interest.
Data Availability Statement
The data that support the findings of this study are available
from the corresponding author upon reasonable request.
ChemistrySelect 2022, 7, e202202547 (7 of 8)
Keywords: GdCrO3 · Humidity Sensor · Multiferroic ·
Nanoparticles · Precursor Synthesis
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Submitted: July 2, 2022
Accepted: July 15, 2022
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