Ceramics International xxx (xxxx) xxx

Contents lists available at ScienceDirect

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

Structural, magnetic and electrical properties of Y1-xScxFeO3 (x= 0, 0.5 & 1)

nanoparticles synthesized by the sol-gel method
Mehrnoush Nakhaei a, *, MarcosA.L. Nobre b, **, Davoud Sanavi Khoshnoud a, Martin Bremholm c,
Hossein Ali Khonakdar d
a
Faculty of Physics, Semnan University, P. O. Box 35195-363, Semnan, Iran
b
São Paulo State University (Unesp), School of Technology and Sciences, Presidente Prudente, SP, 19060-900, Brazil
c
Department of Chemistry and Interdisciplinary Nanoscience Center (iNANO), Center for Materials Crystallography, Aarhus University, 8000, Aarhus C, Denmark
d
Department of Polymer Processing, Iran Polymer and Petrochemical Institute, P. O. Box 14965-115, Tehran, Iran

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

Handling Editor: Dr P. Vincenzini Nanoparticles exhibiting crystalline and single-phase characteristics with Y1-xScxFeO3 (x = 0, 0.5 & 1) nano­
particles synthesized by sol-gel method. The sizes of nanocrystals determined by X-Ray Diffractometry (XRD)
Keywords: were obtained between 30 and 39 nm. The shape of nanoparticles and the surface morphology of the samples
Sol-gel were carried out using Field Emission Scanning Electron Microscopy (FE-SEM) and energy dispersive spectros­
XRD
copy (EDS). The magnetic properties of Y1-xScxFeO3 samples were investigated by Vibrating Sample Magne­
Magnetic properties
tometry (VSM) and Field-Cooled (FC) and Zero-Field-Cooled (ZFC) measurements. The results showed
Electrical properties
antiferromagnetic and paramagnetic behaviors for these prepared perovskites. The electrical properties of the
samples were investigated by measuring the polarization-electric loops, dielectric constant changes and dielectric
loss through frequency and temperature. These measurements showed the TN values of the samples to be 628 and
578 K for YFeO3 and ScFeO3 nanoparticles, respectively. In addition, diffuse reflectance spectroscopy analysis
was used to calculate the band gap energy of the samples based on the Kubelka-Munk function. The achieved
values showed the band gap energy of 2.97 and 3.07 eV for YFeO3 and ScFeO3.

1. Introduction
In recent years, rare earth orthoferrites (RFeO3; R = rare earth ele­
ments or Y3+ & Sc3+) with almost perovskite structure have been shown
useful magnetic, electrical and optical properties. These features lead to
different applications of this group of materials, such as: photocatalysis,
spintronics, gas sensors, optoelectronic devices and electrodes for fuel
cells [1,2]. Having two cations with different ionic radius and one anion
made this structure wonderful to accept various doping to have bene­
ficial magnetic and electrical features [3]. Orthoferrites typically consist
of diamagnetic ions at the R site, resulting in antiferromagnetic ordering
with their Néel temperature (TN) below 750 K. Additionally, Fe3+ ions in
this structure present a Dzyaloshiskii-Moriya (D-M) interaction which
leads to a weak ferromagnetic ordering due to spin-lattice canting [4,5].
The magnetic spin reorientation transition temperature (TSR) in this
family is closely affected by the ionic radius of the R site elements and
TSR decreases with decreasing the R ionic radii [6]. In fact, as the
magnetic ordering needs the empty d orbitals of the ions [7], therefore,
RFeO3 perovskites show both types of this ordering [8,9]. In this regard,
these orthoferrites control their magnetic properties with the electric
field and vice versa [10,11]. These features make this group of materials
attractive for different potential applications [12–14].
Yttrium orthoferrite (YFeO3) is one class of RFeO3 family. YFeO3
usually shows antiferromagnetic properties due to the D-M interaction
[15]. It is usually cusses an antisymmetric exchange interaction [16]. In
fact, YFeO3 has a weak Fe3+ spins anisotropy in the plane of a-c and
strong anisotropy along the b-axis [17]. The spin ordering and antifer­
romagnetic transition in YFeO3 comes from Y–Y, Fe–Fe and Y–Fe
super-exchange interactions [18]. Additionally, the oxygen present in
the YFeO3 structure leads to antiferromagnetic behavior in this com­
pound because of its super-exchange interactions based on
Goodenough-Kanamori-Anderson (GKA) rules [19,20].
This orthoferrite showed a high amount of TN ~640 K [21]. In
addition, the Curie temperature (TC) of YFeO3 is about 600 K [22].

* Corresponding author.
** Corresponding author.
E-mail addresses: mnakhaei137@gmail.com (M. Nakhaei), marcos.nobre@unesp.br (MarcosA.L. Nobre).

https://doi.org/10.1016/j.ceramint.2023.01.177
Received 4 November 2022; Received in revised form 12 January 2023; Accepted 25 January 2023
Available online 31 January 2023
0272-8842/© 2023 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Mehrnoush Nakhaei, Ceramics International, https://doi.org/10.1016/j.ceramint.2023.01.177
M. Nakhaei et al. Ceramics International xxx (xxxx) xxx

Fig. 1. a) X-Ray diffraction profiles and b) Rietveld refinements plots of YF, SF and YSF NPs; c) a new diagram of the lattice distortions of YF: Y3+ ions are in green
spheres, Fe3+ ions are in brown ones and O2− ions are shown with red spheres and d) the Williamson-Hall type plots of YF, SF and YSF NPs. (For interpretation of the
references to colour in this figure legend, the reader is referred to the Web version of this article.)

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Table 1
Rietveld refinement results, the sizes of crystals and particles of YF, SF and YSF NPs.
Sample YF YSF SF

position X Y Z X Y Z X Y Z

Lable

Y/Sc 0.9819 0.0678 0.2500 0.9721 0.0562 0.2500 0.9700 0.0522 0.2500
Fe 0.0000 0.5000 0.0000 0.0000 0.5000 0.0000 0.0000 0.5000 0.0000
O1 0.1060 0.4586 0.2500 0.0926 0.4432 0.2500 0.0903 0.4356 0.2500
O2 0.6935 0.3092 0.0573 0.6534 0.3010 0.0510 0.6501 0.2990 0.0489

Reliability factors (%) RP = 2.46 RP = 2.50 RP = 2.52

Rwp = 2.99 Rwp = 3.04 Rwp = 3.05
Volume ((Ȧ)3) 224.9845 221.9925 220.2574
Cell Parameters (Ȧ) a = 5.2836 (3) a = 5.1257 (4) a = 5.0425 (3)
b = 5.5969 (5) b = 5.3999 (5) b = 5.3246 (4)
c = 7.6082 (4) c = 7.5123 (3) c = 7.4562 (5)
Bond length (Ȧ) (Fe–O1)avg = 1.9962 (Fe–O1)avg = 1.9985 (Fe–O1)avg = 1.9992
(Fe–O2)avg = 2.0562 (Fe–O2)avg = 2.0583 (Fe–O2)avg = 2.0595
Bond angle (ᵒ) Fe–O1–Fe = 144.031 Fe–O1–Fe = 145.562 Fe–O1–Fe = 146.033
Fe–O2–Fe = 144.650 Fe–O2–Fe = 145.952 Fe–O2–Fe = 147.003
τ 0.888 0.893 0.871
DXRD (nm) 39 ± 0.05 37 ± 0.05 30 ± 0.03
DW− H (nm) 46 ± 0.06 41 ± 0.05 35 ± 0.04
< D >SEM (nm) 49 ± 0.03 46 ± 0.06 39 ± 0.05
Lattice strain (ε) 0.0394 ± 0.05 0.0244 ± 0.05 0.0127 ± 0.03

YFeO3 has a useful orthorhombic structure [23]. Basically, YFeO3 ex­
hibits both ferroelectric and antiferromagnetic phases [23,24], and the
magnetic phase transition temperature may change its electric behaviors
[25–28]. YFeO3 has advantageous applications in gas sensitive sensors,
catalyst of magnetic devices and as photocatalyst [29]. For controlling
the physical properties of YFeO3 compound, it can be useful to dope it
using chemical materials through chemical methods [10,30]. Various
previous researches showed substitution on the side of R3+ ion to
improve the physical properties of YFeO3 compound [31–33].
The ionic radius of Y3+ is ~1.01 Ȧ and the Y+3 substitution showed
an increase in magnetization and also electrical behavior. In addition,
the Fe3+ site substitution in the YFeO3 structure will increase the coer­
civity field [34–37]. Additionally, scandium (Sc) is a good candidate for
substituting at the Y3+ site, because the ionic radius of Sc3+ ion (~0.74
Ȧ) is almost near that of Y3+ ion. Therefore, the lattice structure and the
space group of YFeO3 might be stable after doping [38].
In addition to the above explanations about YFeO3 and its sub­
stitutions, the determination of ScFeO3 is important in this research.
ScFeO3 is another important member of the RFeO3 family.
In their work, Kawamoto et al. [38] found that ScFeO3 exhibits
orthorhombic structure at temperatures above T = 800 ◦ C, and at lower
calcination temperature, its structure becomes hexagonal with R3C
space group [39]. Due to the strong p-d hybridization in ScFeO3, it is a
magnetoelectric material [40,41]. Therefore, a weak ferroelectric po­
larization will present in this compound at room temperature [42,43].
The TN of ScFeO3 is ~545 K, which is related to the G-type antiferro­
magnetic canting of Fe3+ ions [40,44]. Therefore, in this research,
YFeO3 and ScFeO3 ferrites have been investigated and their physical
properties have been compared. In addition, Y0.5Sc0.5FeO3 compound
was synthesized to investigate the Sc3+ and Y3+ ion effects on the
physical properties of YFeO3 and ScFeO3, respectively.
In recent years, many different synthesis methods have been used to
prepare the RFeO3 family, such as: solid-state reaction, hydrothermal,
sol-gel, and co-preparation [45–47]. As the size and shape of the parti­
cles are important factors that must be controlled in the synthesis pro­
cess [48,49], here in this research it is preferred to use sol-gel methods to
produce Y1-xScxFeO3 (x = 0, 0.5 & 1) compounds. In general, nanosize
particles shows beneficial applications [50–56]. On the other hand, the
sol-gel method is a low-cost, controllable and easy way to prepare
nano-sized materials [57–60].
2. Materials and methods
2.1. Synthesis of Y1-xScxFeO3 nanoparticles
Y1-xScxFeO3 (x = 0, 0.5 & 1) nanoparticles (NPs) were synthesized
via the appropriate amount of yttrium (III) nitrate hexahydrate (Y
(NO3)3⋅6H2O), scandium nitrate hexahydrate (Sc(NO3)3⋅6H2O), iron
nitrate nonahydrate (Fe(NO3)3⋅9H2O) and citric acid (C6H8O7) by using
sol-gel combustion method. Firstly, at room temperature, 0.024 mol
citric acid was added to 60 ml distilled water on a magnetic stirrer.
Secondly, to prepare Y1-xScxFeO3 samples, 0.003 mol of prematerials
consisting Y(NO3)3⋅6H2O, Sc(NO3)3⋅6H2O and Fe(NO3)⋅9H2O were
separately added to the first solution in appropriate stoichiometry. The
pH values of all three samples were adjusted to 7 using NH3. Next, the
solutions were stirred for about 2 h until homogenous. Thereafter, the
solutions were stirred at T = 80 ◦ C for 3 h to form a light green gel. The
prepared gel was dried at T = 120 ◦ C for 15 h. At last, they were calcined
at T = 950 ◦ C for 2 h. The achieved YFeO3, ScFeO3 and Y0.5Sc0.5FeO3
were named YF, SF and YSF, respectively.
2.2. Characterization methods
In this work, X-ray diffractometry (XRD) was used for the structural
characterization. The X-ray wavelength was ~1.542 Å of Cu Kα radia­
tion. The analysis of XRD patterns were carried out by using X-pert and
FullProf software. Crystallite sizes and lattice strains were calculated
according to the Williamson-Hall (W–H) method. Field emission scan­
ning electron microscopy (FE-SEM, LEO 912 AB, Carl Zeiss SMT, Ger­
many, 120 kV) technique was used to determine the particle
morphology. The elemental compositions of the samples were analyzed
via energy dispersed spectroscopy (EDS) analysis. In addition, the
Quantum Design PPMS system model 6000 was used to measure the
field-cooled (FC) and zero-field-cooled (ZFC) behavior of the prepared
samples. Besides these useful magnetic measurements, vibration sample
magnetometer (VSM) analysis at T = 300 K was used under applied
magnetic fields up to 20 kOe. The electrical properties of the samples
were determined with using the polarization-electric field (P-E) method.
Additionally, the dielectric properties of Y1-xScxFeO3 samples were
measured by an LCR meter (GW Instek 8110G). For this measurement,
YF, YS and YSF samples were compressed into a number of pellets with a

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M. Nakhaei et al.
Fig. 2. The FE-SEM images of YF, SF and YSF NPs.
diameter of 10 mm and a thickness of 2.1 mm. Next, they were sintered
at 950 ◦ C for ~1 h. The samples were coated by gold paste for this
measurement. To measure dielectric changes through temperature, the
frequency was set to 1000 Hz. Finally, the optical characterization of the
samples was done by using diffuse reflectance spectroscopy (DRS)
measurement.
3. Results and discussion
3.1. Structural studies
The XRD patterns of YF, SF and YSF NPs are shown in Fig. 1a. These
graphs were compared with sample diffraction data (JCPDS) file No. 00-
047-0071 for YF and SF and file No. 01-082-2421 for YSF. According to
this comparison, it was found that all three samples were produced
without additional peak as impurities or second phases. They showed an
orthorhombic structure with Pbnm space group. The XRD results of YSF
NPs showed an extra peak with the (210) miller index in YSF NPs. This
peak showed that this sample has the most overlapping via ortho­
rhombic lattice structure. Additionally, some peaks related to YSF
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structure became clearer. Next, FullProf suit software was used to refine
the obtained XRD data. Accordingly, in this Rietveld refinement used the
Pseudo-Voigt function to confirm the structural parameters of XRD data
with the basic structure. The Rietveld refinement curves of YF, SF and
YSF samples are illustrated in Fig. 1b. The refined parameters are con­
taining the ionic positions of the elements (x, y, z), reliability factors (Rp,
Rw), volume cells (V), cell parameters (a, b and c) important bond
lengths and bond angles are shown in Table 1.
The degrees of crystalline structure of the samples were estimated by
√̅̅̅
tolerance factor (τ). In this regard in τ = (Y − O) / 2(Fe − O) [61,62],
Y–O and Fe–O parameters are bond lengths, and they are achieved from
the FullProf refinement. Totally, the τ value of the orthorhombic struc­
ture is usually between 0.71 and 0.9 [62].
As it can be seen in Table 1, the τ values of SF, YSF and YSF NPs have
increased, respectively. Therefore, YSF NPs showed the closest structure
with orthorhombic distortions. These distortions affect the physical
properties of the samples, which will be discussed later. It was predict­
able that due to the smaller ionic radius of Y3+, YF should have a larger τ
value compared to SF, and this happened to the prepared samples. In
fact, the FeO6 octahedron was tilted towards the center of the Y3+ ions to
M. Nakhaei et al.
Fig. 3. The EDS spectra of YSF NPs.
form the Y–O bond [45]. Fig. 1c shows the schematic structure and
lattice distortions of the prepared YF nanoparticles. This graph was
drawn using VESTA software according to FullProf refinement achieved
data.
The size of YF, SF and YSF nanocrystallites was calculated based on
the XRD results through Scherrer’s equation [62] and then based on the
Williamson-Hall (W–H) method [63]. The results of Scherrer equation
(Dscher = Kλ/β cos θ; λ is the X-ray wavelength (λCukα = 1.542 Å), β is the
full width at half maximum (FWHM) of the lines, θ is the diffraction
angle and K = 0.94 is Scherrer’s constant) calculations are listed in
Table 1. In this calculation, the highest peak of XRD data of YF, SF and
YSF nanocrystallites was used. The changes in the crystal size of the
samples (DXRD) showed the influence of rare earth elements in
Y1-xScxFeO3 compounds, in fact the nanocryatalliane sizes decreased
from YF to YSF due to the decrease in the ionic radius of Y to Sc ele­
ments. In addition to the Scherrer equation, the Williamson-Hall (W–H)
method: β cos θ = kλ/D + 4ε sin θ; was used to calculate crystallite sizes
and lattice strains of samples [62]. In this way, the highest peaks of XRD
curves with the 2 theta values of 29, 32, 33, 41, 47, 48, 53, 60 & 64◦
were used. The W–H plots (β cos θ versus 4 sin θ) are shown in Fig. 1d. By
linear fitting of these curves, the crystallite sizes of the samples are
estimated from the y-intercept, and the lattice strains (ε) are determined
from the slope of this fitting. The sizes of crystals (DW-H) and their lattice
strain (ε) are listed in Table 1 based on the W–H plot. Both of these two
methods for calculating the crystal sizes of the samples showed the same
mechanism of the size variations of YF, YSF and SF samples with the
ionic radius of Y site elements.
The FE-SEM images of the YF, SF and YSF NPS are shown in Fig. 2 to
investigate the morphology and grain size of the particles. According to
these images, the samples show semispherical shape, but there is more
evidence in YSF NPs. In addition, grain boundaries are more distinct in
this sample. The sizes of nanoparticles were determined by using Dig­
imizer software and they are listed in Table 1. In fact, YSF showed a
more homogeneous shape and the disappearance of grain boundaries of
this sample may be due to kinetic diffusion [64]. These results are in
agreement with the XRD results of the prepared YF, SF and YSF NPs.
For determining the elemental composition of YSF NPs, the EDS
spectrum of this sample is shown in Fig. 3. The weight and atomic
percentage of the elements (Y, Sc, Fe & O) are listed instead of Fig. 3.
These values and the EDS curve support the Y:Sc ratio because Y is
heavier than Sc and the ratio of Y/Sc:Fe is exactly equal to 1.
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Fig. 4. VSM curves of the YF, SF and YSF NPs measured at T = 300 K.
Table 2
Magnetic parameters of YF, SF and YSF NPs.
Sample Mnet (emu/g) Mr (emu/g) Hc (Tesla) MCW(emu/g) θCW (K)
YF 0.600 0.172 − 0.04 2.24 − 34
YSF 0.600 0.010 − 0.03 1.07 5
SF 0.261 0.002 − 0.01 0.09 15
3.2. Magnetic studies
Fig. 4 Depicts the VSM measurements of YF, SF and YSF-NPs. YF-NPs
show anti-ferromagnetic behavior due to its ionic structure. In fact, the
magnetic behavior of the most transition metal oxides in the perovskite
structure can be explained by their crystal structure. Accordingly, in the
orthorhombic lattice structure of YF, each Fe3+ ion is surrounded by six
O2− ions which forms an FeO6 octahedral structure and each O2− ion is
connected by two adjacent octahedral sites to form a super-exchange
interaction [65]. Based on the antisymmetric D-M exchange interac­
tion mechanism, each magnetic moment of Fe3+ ion is slightly anti­
parallel to the moments of the six nearest neighbor Fe3+ moments, and it
produces a small spin canting that leads to weak ferromagnetic prop­
erties in antiferromagnetic YF-NPs [66,67]. Based on the crystal struc­
ture of YF, a G-type isotopic antiferromagnetic spin ordering can be
predicted for this sample. Many different previous researches showed
the same magnetic behavior of YF [68–72].
It is well known that in rare-earth orthoferrites (RFeO3), the R3+-R3+,
Fe -Fe3+ and R3+-O2+-R3+ interactions are responsible for the mag­
3+
netic behaviors of this family [69]. But here in YF, as Y3+ is a
nonmagnetic ion with filled orbitals, therefore, only Fe3+-Fe3+ in­
teractions have magnetic responsibilities. According to the
Goodenough-Kanamori-Anderson theory, the nature of the antiferro­
magnetic behavior of YF is because of the Fe3+-O2--Fe3+ super-exchange
interactions at about 180◦ [73]. According to Table, this super-exchange
angle in YF NPs is less than 180◦ due to the octahedral site rotation in the
orthorhombic structure [74]. Another reason for this antiferromagnetic
behavior of YF NPs can be the overlapping of the eg orbitals of Fe3+ ions
which are located along the crystal axes [17]. The net magnetization
(Mnet), remnant magnetization (Mr) and coercive field (Hc) values of the
samples are reported in Table 2. Based on these values, the coercive field
(Hc) of YF is about − 0.03 T in spite of its high Mnet value. This difference
created a peculiar shape around H = 0 T of YF. It is due to the anisotropy
effect of the magnetic crystal of nanoparticles; because two Fe3+ ions in
YF have a pedding distortion. In addition, with decreasing the external
M. Nakhaei et al.
Fig. 5. FC & ZFC plots of YF, SF and YSF NPs.
magnetic field, the overcoming of this material is decreased [75]. Ac­
cording to Fig. 4 SF NPs show a linear dependence of magnetization via
magnetic field. Therefore, SF shows the paramagnetic behavior. The low
value of Mnet in SF is due to the effect of diamagnetic Sc3+ ions [76].
As it can be seen in Fig. 4 and Table 2, the Mnet of YSF NPs is as same
as that of YF NPs but it is higher than that of SF NPs. Besides the Hc value
of YF is the highest value among these three samples, and followed by
the Hc value of YSF NPs and then SF NPs. It can be due to the larger
crystal size of the YF NPs. In fact, nanoparticles with the average
diameter of under 100 nm are considered as single domain. Therefore,
Hc depends on the average crystal size of the particle based on the
following formula [77]:
h
Hc = g − (1)
D3 2
/
Here the g and h are constants, the D is the diameter of the particles.
Thus, based on Equation (1), the Hc value increases by increasing the
particle diameter. Next, according to Fig. 4, the YSF NPs show antifer­
romagnetic behavior with the lower value of Mr in comparison with YF
sample due to the existent of diamagnetic Sc3+ ions in YSF NPs.
Temperature dependence of magnetization at 1000 Oe in the FC and
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Ceramics International xxx (xxxx) xxx
ZFC process of YF, SF and YSF NPs in the temperature range of 2–300 K
is shown in Fig. 5. For all three samples, the FC curve is on the top of the
ZFC curve. This confirms their antiferromagnetic-to-paramagnetic
behavior seen in VSM measurements. The spin reorientation tempera­
ture (TSR) of YSF NPs is shown in Fig. 5, where the ZFC curve first in­
creases and then decreases. The TSR for YFS was about 15 K. For both YF
and YSF samples, the FC plots decreased with increasing temperature
and crossed the ZFC plots at a certain temperature, known as the Néel
temperature (TN) of the samples. After that, the magnetization values
became the same in the FC and ZFC plots. The TN values of YF and YSF
samples are presented in Fig. 5. As can be observed in this figure, the TN
of the samples increased for samples from YF to YSF. The reason may be
Sc3+ ions in YSF compound. Because the distortion of YF sample is
reduced by replacing Sc3+ ions with ions with smaller ionic radius. A
similar behavior of the Sc substitution effect was previously seen in
Shngan Ma’s et al., research [78]. But for SF NPs, FC and ZFC plots
behaved differently. As can be seen in Fig. 5, FC and ZFC plots of this
sample are far from each other; this type of behavior confirms the
paramagnetic behavior of this sample which was seen in VSM mea­
surement (see Fig. 4.) [79,80].
Next, the Curie-Weiss behavior of YF and YSF NPs was investigated
M. Nakhaei et al.
Fig. 6. P-E hysteresis curves of YF, SF and YSF NPs.
Table 3
Electrical parameters of YF, SF and YSF NPs.
2
Sample Pr (μC/cm ) Ec (kV/cm)
YF 0.017 − 6.028
YSF 0.008 − 3.272
SF 0.006 − 2.104
based on FC and ZFC plots. Curie-Weiss temperature (θcw ) was derived
from the inverse linear fit of the magnetic susceptibility (X = (T− CθCW )+ X0
, C is the Curie constant, X0 is the basic magnetic susceptibility under FC
protocol) [81]. Additionally, the Curie-Weis magnetization (Mcw) of the
system was calculated by this fitting. The values of θcw and Mcw are listed
in Table 2. Based on the vales achieved, the negative value of θcw for YF
NPs illustrates the antiferromagnetic behavior of this sample [82,83]. As
can be seen in Table 2, θcw goes to the positive values by adding Sc3+
diamagnetic element, which changes the magnetic structure from anti­
ferromagnetic for YF NPs and then for YSF NPs to paramagnetic for SF
NPs. Moreover, the Mcw became less from YF to YSF and then for SF NPs.
These observations confirm the variations in magnetic parameters (Mnet
and Mr), which are represented in the VSM explanation section of this
research.
3.3. Electrical and dielectric studies
Fig. 6 Illustrates the P-E hysteresis loops of YF, SF and YSF NPs,
which were measured at T = 300 K and the frequency of 50 Hz. Based on
these loops, no polarization saturation was seen for all three samples.
Under usual conditions, it is difficult to measure the P-E hysteresis loops
of rare-earth perovskites in the high electric field region and a break­
down will be seen in the loop due to the large leakage current (see
Fig. 6.). Other previous research also had this breakdown in their
measurement [84]. The values of remanent polarization (Pr) and coer­
cive field (Ec) are reported in Table 3. The weak ferromagnetic behavior
of YF arises from the D-M interaction due to the extra spin canting
related to the antiferromagnetic ordering described in the previous
section [85,86]. But by adding Sc3+ ion in YF NPs as YSF NPs both Pr and
Ec values decreased and SF NPs showed their minimum values. The
reason might be the increase of lattice distortions after adding Sc3+ or
replacing Y3+ with Sc3+ ions. Because Sc3+ ion has smaller ionic radii.
Therefore, the lattice centrosymmetry in the Pbnm group space becomes
smaller, and so, the electric behavior of the samples is weakened [87,
88]. In fact, by decreasing the nanoparticle sizes from YF to SF, the
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Ceramics International xxx (xxxx) xxx
Fig. 7. Dielectric constant (ε) versus frequency variations; the inset shows the
dielectric loss (tanδ) versus frequency variations of YF, SF and YSF NPs.
polarization of the samples decreased. Similar behavior for YFeO3 NPs
was previously observed in other studies [89].
Totally, in these groups of materials, spin exchange striction is
known to be the source of weak ferroelectric polarization [90]. Spin
exchange striction is usually happen between Y/Sc and Fe ions in the
domain wall area [91].
The variations of dielectric constant (ϵ) versus the logarithm of fre­
quency in the range of 100 Hz to 10 MHz of YF, SF and YSF NPs at T =
300 K are shown in Fig. 7. In this figure, it is obvious that the values of ϵ
decrease by increasing frequency. This type of behavior is a feature of
this family due to the dipole relaxation process because ϵ arises from the
space charge polarization [92].
In fact, the ϵ values of the samples are large at low frequencies and
then show constant values at higher frequency of the applied electric
field [84]. The high values of ϵ at low frequencies are due to the local­
ization of charge accumulation, which leads to an increase in space
charge polarization when selective fields are applied. But as the fre­
quency increases, the electric dipoles cannot respond to this high electric
field, so ϵ decreases. This behavior can be explained by Maxwell-Wagner
electric polarization theory [93]. Another reason for this behavior of the
samples is the nanocrystal sizes of the prepared samples. Because in the
nanoscale, defects, dislocations and voids lead to constant values of ϵ by
creating declination in it [94]. Therefore, the SF NPs show the highest
value of ϵ due to the smaller size of nanocrystals, which were reported
before in Table 1. As seen in Fig. 7, it is clear that ϵ increases with the
addition of Sc3+ ions to YF.
Variations of dielectric loss (tan δ) versus frequency for YF, SF and
YSF NPs are shown in the inset of Fig. 7. The change in tanδ behaved
similarly to the change in ϵ. Changes in tanδ have various reasons such as
structural stoichiometry, sample homogeneity, and the behavior of Fe3+
ions, which can be influenced by the synthesis process [95]. According
to these curves, SF NPs show the highest value of tanδ but YF and YSF
NPs show the same values. Therefore, Sc3+ ions cannot affect the energy
loss of YF NPs. Similar behaviors of ϵ and tanδ for these samples have
also been seen in previous researches [68,84,96,97]. In addition, no
peak was seen in the tanδ curves of all three samples. The reason can be
related to their resistivity [96].
The temperature dependence of dielectric constant (ϵ) variations at a
frequency of 1000 Hz for YF, SF and YSF NPs are presented in Fig. 8. In
the inset of Fig. 8, the dielectric loss (tanδ) versus temperature curves are
shown. Based on these curves, the variations of both ϵ and tanδ values
are obviously increased. For all three samples, a peak is observed at
higher temperatures, which shows a change in polarization, leading to
M. Nakhaei et al.
Fig. 8. Dielectric constant (ε) versus temperatures variations; the inset shows the dielectric loss (tanδ) versus frequency variations of YF, SF and YSF NPs.
variation in the magnetic and electrical structures of the samples. These
abnormal peaks seen in YF, SF and YSF curves are close to their TN [98].
The TN values of the samples in Fig. 8 are determined as 628, 603 and
578 K for YF, YSF and SF NPs, respectively. It can be seen that the TN of
YF NPs is the highest, followed by YSF NPs and finally SF NPs with the
lowest value. This type of behavior for these samples is confirmed based
on the Fe–O–Fe values presented in Table 1. Because TN is theoretically
calculated by the equation: TN = 4S(S + 1)J/kB, which S is the spins of
Fe3+ ions and J is equal to cos4(ω/2)/d7. In this equation, J is the
super-exchange coupling and it is equal to 180-˂Fe–O–Fe > av and d =
˂Fe–O > av [99]. J increases with increasing values of Fe–O–Fe. There­
fore, it is acceptable that the TN values decrease as the lattice distortions
of the sample increase in the order of YF > YSF > SF. The mechanism of
decreasing the lattice distortions was explained in the previous sections.
In fact, the increase of ϵ versus T is characteristic of a suitable dielectric
compound, which was observed for YF, SF and YFS NPs [100]. The same
dielectric behavior of this research was seen in previous research [87,97,
101].
8
Ceramics International xxx (xxxx) xxx
3.4. Optical studies
To investigate the band gap energy (Eg) values of YF, SF and YSF
samples, DRS measurement was carried out in this research. Therefore,
DRS curves was used to calculate Eg based on the Kubelka-Munk (K-M)
function as: F(R) = (1-R)2/2R; which F(R) is the K-M function and R is
the reflectance [102]. F(R) and Eg can be entered into the equation as: F
(R)*hν = A(hν-Eg)1/n for direct Eg; that h is the Planck constant, A is a
constant and ν is the frequency [102,103]. The K-M plots of YF, SF and
YSF NPs are represented in Fig. 9. The Eg value was estimated by fitting
the K-M curves by drawing a line in its linear region that crosses the
energy axes at (F(R)*hν)2 = 0. Therefore, the achieved Eg values are
comprised inset of Fig. 9. As it can be seen in the figure, the Eg values of
YF, YSF and SF NPs are about 2.97, 3.05 and 3.07 eV, respectively. The
increase in Eg value of YF NPs compared to the Eg value of SF NPs may be
due to the decrease in nanocrystalline size of these samples [104,105].
The reason is the decrease in energy level and the overlap of orbitals
with decreasing crystalline size [106]. Another mechanism for this
M. Nakhaei et al.
Declaration of competing interest
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Appendix A. Supplementary data
org/10.1016/j.ceramint.2023.01.177.
References
Fig. 9. Kubelka-Munk transformed reflectance spectra of YF, SF and YSF NPs;
the insert shows the comparison of the band gaps.
change of Eg values is the change of their Fe–O–Fe bond angle and their
Fe–O bond length, which play an important role in modifying the width
of an electron band (W), which of course also changes Eg. This is
confirmed by the equations: Eg = Δ-W, where Δ is the transfer energy of
the charges and ∝cos w
. Hence, W is 1/2[π-(Fe–O–Fe)] and d3.5
d3.5 Fe− O is Fe–O
Fe− O
bond length [17,107]. Therefore, according to Table 1, it is acceptable
that Eg values increased for YF to SF samples, respectively.
4. Conclusions
Orthorhombic single phase Y1-xScxFeO3 NPs were synthesized via
sol-gel method successfully. The size of nanoparticles showed a
decreasing trend in YF, YSF and SF, respectively. YF NPs showed a
strange magnetic hysteresis loop behavior, but by adding Sc3+ ion (YSF
sample), it behaved as a typical antiferromagnetic, while SF showed
paramagnetic behavior. FC and ZFC measurements confirmed the
magnetic behaviors of the samples presented in this research. The
maximum values of Pr and Ec for YF NPs were about 0.017 μC/cm2 and
-6.028 kV/cm, respectively. In addition, the variations of ε and tanδ
versus increasing T illustrated TN values of 628, 603 and 578 K for YF,
YSF and SF NPs, respectively. At last, by using DRS analysis and
Kubelka-Munk function, the Eg values of the samples were calculated as
2.97, 3.05 and 3.07 eV for YF, YSF and SF NPs, respectively, which can
be used in engineering of optical gap and semiconductor materials.
Funding
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
CRediT authorship contribution statement
Mehrnoush Nakhaei, Conceptualization, Methodology, Software,
Writing-Original draft preparation.
Marcos Augusto Lima Nobre conceptual, Reviewing, Editing.
Davoud Sanavi Khoshnoud, Data curation, Investigation, Validation,
Editing.
Martin Bremholm, Data curation, Investigation, Validation.
Hossein Ali Khonakdar, Investigation, Writing-Reviewing and
Editing.
9
Ceramics International xxx (xxxx) xxx
The authors declare that they have no known competing financial
Supplementary data to this article can be found online at https://doi.
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