Physica E: Low-dimensional Systems and Nanostructures 108 (2019) 100–104

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Physica E: Low-dimensional Systems and Nanostructures

journal homepage: www.elsevier.com/locate/physe

Impact of magnesium substitution in nickel ferrite: Optical and T

electrochemical studies
M.K. Shobanaa,∗, Kyungbae Kimb, Jae-Hun Kimb
a
Department of Physics, School of Advanced Sciences, VIT University, Vellore, Tamilnadu, 632014, India
b
School of Materials Science and Engineering, Kookmin University, 77 Jeongneung-ro, Seongbuk-gu, Seoul, 02707, Republic of Korea

ARTICLE INFO ABSTRACT

Keywords: Magnesium doped Ni ferrite nanoparticle (Ni1-xMgxFe2O4) has been synthesized by sol-gel combustion method
Nanoferrite and it has been analyzed using XRD, UV, FTIR and electrochemical charge-discharge studies. The observed XRD
X-ray diffraction result confirms the nanostructure and it ranges from 23 to 28 nm. Furthermore, band gap energy values and
Electrochemical study functional group elements have been observed by UV and FTIR, respectively. The lattice constant values varies
Bandgap energy
slightly with respect to magnesium concentration. The band gap energy values increase at the calcination
temperature of 500 °C as 0.85, 1.15, 1.2, and 1.45 eV and it decreases when it was calcined at 900 °C as 1.3, 1.25,
1.15, 1.1 eV for x = 0.25, 0.5, 0.75, 1, respectively. The voltage profiles of Ni1-xMgxFe2O4 nanoparticle elec-
trodes show the discharge and charge capacities of 1021 and 718 mAh/g at 500 °C and 1099 and 747 mAh/g at
900 °C, respectively. The high reversible capacities for the Mg doped Ni ferrite nanoparticle electrodes are
confirmed as anode materials for Li ion batteries.

1. Introduction
Ferrites nanomaterials have been attracted in various applications
owing to their inimitable properties than bulk materials. Recent dec-
ades, the investigation on nanoferrite materials reveals astonishing
achievement in several fields such as medicine, microwave device,
sensors, supercapacitors, fuel cells and catalysts [1–6]. Among those
materials, substituted nickel ferrite nanomaterials illustrate notable
changes in various applications [7–10] than pure nickel ferrite. Several
researchers [11–15] reported the influence of substituted nickel ferrites
in storage applications to improve the energy storage and energy har-
vesting applications.
Kondawar et al. [16] reported the zinc substituted nickel ferrites
reinforced conducting polyaniline nanocomposites. The electrical
properties of the sample shows the decrease in conductivity when the
concentration of zinc increases as 5%–15% at room temperature. When
the temperature increases, the conductivity of the sample exhibits
semiconductor behavior. Polycrystalline NiCrxFe2−xO4 (0.0 ≤ x ≤ 1.0)
ferrites were prepared by conventional ceramic technique [17]. The
observed result reveals that bulk densities decrease with Cr content,
whereas the porosity increases. The conduction mechanism has been
confirmed by the values of activation energy and the AC resistivity
decreases with frequency. Variation of loss tangent with frequency
enhances the hopping of charge carriers between the Fe2+ and Fe3+
ions, and as a result the conduction increases and resistivity decreases.
Devmunde et al. [18] reported the various properties Cd substituted Ni
ferrite and spherical shaped, fused grain nature with intergranular
diffusion in Ni1−xCdxFe2O4 nanoparticles was observed in scanning
electron micrographs. The value of loss tangent (tan δ) decreases ex-
ponentially with an increasing frequency indicating normal Maxwell-
Wagner type dielectric dispersion due to interfacial polarization. De-
creasing values of Curie temperature (Tc) from 860 °C to 566 °C with
increasing Cd2+ content x in Ni1−xCdxFe2O4 nanoparticles were de-
termined from AC-susceptibility. Activation energy ΔE ranges within
0.03∼0.15 eV. Graphene with nickel ferrite electrode materials shows
the capacitance of 105 F g−1 after 1500 cycles at current density of
10 A g−1 which makes it an outstanding supercapacitor electrode ma-
terial with promising long cycle performance [19]. The optimal Au/
NiFe2O4 plasmonic photocatalysts with 1.5% gold nanoparticles (NPs)
displays the hydrogen production rate of 0.256 mmol g−1h−1 by loca-
lized surface plasmon resonance effect of Au NPs [20]. The optimum
rate for hydrogen generation reached 3.162 mmol g−1h−1 and the rate
is about 60-fold and 12-fold higher than that of pure NiFe2O4. Based on
the review of available published research reports, the research on Mg
substituted nickel ferrites are much less especially on optical study
and electrochemical performance. Hence, this paper deliberately in-
vestigates the optical and electrochemical properties of sol-gel prepared
Ni1−xMgxFe2O4.

∗
Corresponding author.
E-mail address: mkshobana@gmail.com (M.K. Shobana).

https://doi.org/10.1016/j.physe.2018.12.013
Received 5 November 2018; Accepted 12 December 2018
Available online 12 December 2018
1386-9477/ © 2018 Elsevier B.V. All rights reserved.
M.K. Shobana et al. Physica E: Low-dimensional Systems and Nanostructures 108 (2019) 100–104

2. Experimental detail
(a) 500 C x=1
2.1. Materials preparation
x=0.75

Transmittance (a.u.)
Magnesium substituted nickel ferrites were synthesized by sol-gel
combustion technique using analytical grade nitrate elements. Here
nickel nitrate (99% Sigma Aldrich, India), magnesium nitrate (99%
Sigma Aldrich, India), iron nitrate (99% Sigma Aldrich, India) materials
x=0.5
were used as starting materials. Additionally, polyvinyl alcohol (PVA)
was used a chelating agent. Metal nitrates, citric acid and PVA were x=0.25
dissolved in distilled water and it was stirred constantly for 3 h.
Furthermore, it was treated in various temperatures for diverse analysis 1000 1384 1593
as specified in the previous report [21]. NO 1384 1606
C O O H
2.2. Characterization

The structural properties of the magnesium substituted nickel fer-

rites have been analyzed by powder X-ray diffraction method using
BRUKER D8 ADVANCE equipment (X-ray, 1.546 Å). Morphology of the
400 600 800 1000 1200 1400 1600 1800
synthesized samples has been analyzed by scanning electron micro- -1
Wavenumber (cm )
scope (SEM, ZEISS EUVA 8), Fourier transform infrared spectroscopy
(FTIR) was used in KBr medium using Shimadzu, FTIR-8400 spectro-
meter in the wave number range from 400 to 4000 cm−1 with a re-
solution of 4 cm−1 and Optical study was carried out using JASCO (b) 900 C x=1
UV–visible spectrophotometer (V-670 PC). Electrochemical charge-dis-
charge tests were performed using CR2032 coin-type half cells con-
x=0.75
sisting of a working electrode and Li foil counter/reference electrode
Transmittance (a.u.)

with a polyethylene separator. Electrolyte was 1 M LiPF6 in ethylene

carbonate (EC)/diethylene carbonate (DEC) (3:7 vol ratio, PANAX
Etec). The cells were galvanostatically tested at a constant current of x=0.5
100 mA/g using a battery cycler (CTS-Lab, BaSyTec).
x=0.25
3. Results and discussion
1000 1384 1593
3.1. Structural studies
NO 1384 1606
C O O H
The structural analysis of the magnesium substituted nickel ferrites
(Ni1-xMgxFe2O4) (x = 0.25, 0.5, 0.75, 1) have been analyzed by X-ray
Diffraction technique and the formation of single phase spinel ferrite
structure has also been identified and it is shown in Fig. 1. The occur-
rence planes (220) (311) (222) (400) (422) (511) (440) in the XRD 400 600 800 1000 1200 1400 1600 1800
-1
Wavenumber (cm )
(311)
Fig. 2. FT-IR spectra of Ni1-xMgxFe2O4 (x = 0.25, 0.5, 0.75 & 1) calcined at (a)
500 °C and (b) 900 °C.
(220) (440)
(400)
x=1 (222) (422)(511) pattern expose the cubic structure of the sample and it matches with
corresponding standard file of nickel ferrite [22]. At the same time, it
Intensity (a.u.)

can be seen from the observed XRD pattern that crystalline nature
slightly increases with increase of magnesium concentration [23]. The
x=0.75 lattice parameters of the sample synthesized at 500 °C are 8.316, 8.316,
8.347 and 8.347 Å for x = 0.25, 0.5, 0.75 and 1, respectively. However,
there was small change in lattice parameter with Mg content. Moreover,
it is attributed to slight change in intensity in observed XRD pattern
x=0.5 with respect to magnesium concentration [24]. This can be explained
by ionic radii of the Mg2+ (0.72 Å) and Ni2+ (0.69 Å) is small. The
average crystallite size were calculated by Debye-Scherrer's formula
and ranges between 23.7 and 28.3 nm. The observed pattern shows the
x=0.25 single phase structure, as there is no other additional peaks for im-
purity.

20 30 40 50 60 70
3.2. Fourier transmission infrared spectra analysis
2 Theta (degree)
FTIR spectra samples at prepared 500 and 900 °C was measured in
Fig. 1. XRD patterns of Ni1-xMgxFe2O4 (x = 0.25, 0.5, 0.75 & 1) at 500 °C. the frequency range of 4000–400 cm−1 and they are shown in Fig. 2.

101
M.K. Shobana et al. Physica E: Low-dimensional Systems and Nanostructures 108 (2019) 100–104

(a) 1.0 500 C x = 0.25 (b) 1.0 900 C x = 0.25

0.9 x = 0.5 0.9 x = 0.5
x = 0.75 x = 0.75
Absorbance (a.u.)

Absorbance (a.u.)
0.8 x=1 0.8 x=1

0.7 0.7

0.6 0.6

0.5 0.5

0.4 0.4

0.3 0.3
200 300 400 500 600 700 800 200 300 400 500 600 700 800
Wavelength (nm) Wavelength (nm)

(c) 2.0 500 C (d) 2.0 900 C

9001 9001
1.6 x = 0.25 x = 0.5 x = 0.75 x = 1 1.6 x = 0.2 x = 0.5 x = 0.7 x=1
1.32 eV 1.06 eV 1.51 eV 1.13 eV 1.69 eV 1.46 eV 1.68 eV 1.56 eV
( h ) (a.u.)

( h ) (a.u.)

1.2 1.2
2

0.8 0.8

0.4 0.4

0.0 0.0
1.0 1.2 1.4 1.6 1.8 2.0 1.0 1.2 1.4 1.6 1.8 2.0
Photon energy (eV) Photon energy (eV)
Fig. 3. (a,b) UV absorbance spectra and (c,d) plot of (αhv)2 as a function of photon energy (eV) of Ni1-xMgxFe2O4 (x = 0.25, 0.5, 0.75 & 1) calcined at 500 °C and
900 °C, respectively.

The spectra show the two peaks below 600 cm−1, which is a common
feature of the all the ferrites [25]. The bands around 510-550 cm−1 and
410-470 cm−1 are assigned as ν1 and ν2, respectively. The absorption
band ν1 is caused by the stretching vibration of the tetrahedral metal-
oxygen bond, and the absorption band ν2 is caused by the metal oxygen
vibration in octahedral site [26]. The slight deviation band position, by
the increase of Mg concentration, may be produced owing to variation
of the cation-oxygen bond length of the octahedral lattice of the spinel.
At magnesium concentration of x = 0.4 and 0.8, ν1 shows the new band
between ν1 and ν2. A similar band observed in ferrites synthesized by
Lopez et al. [27]. This band is attributed also to the stretching vibra-
tions of metal-oxygen atom.
The bands at 1334 and 1384 cm−1 are assigned to CeO stretching
vibration [28]. The variation in absorption position in octahedral and
tetrahedral complexes of synthesized is due to the different distance
between Fe3+-O2- in the octahedral and tetrahedral sites. The band near
1606 and 1688 cm−1 are due to the OeH stretching vibration of the
free or absorbed water [29]. This indicates the hydroxyl groups in the
synthesized sample, which is apparently seen in earlier reports [30,31].
The band around 1000 cm−1 is related to NO- stretching vibration due
to nitrate group [32,33] and these bands disappear when magnesium
content (thus calcination temperature) increased.
3.3. Optical studies
Fig. 3 illustrates the UV- absorption spectra of nanostructured Ni1-
xMgxFe2O4 calcined at 500 °C and 900 °C. It can be seen that absorbance
of Ni1-xMgxFe2O4 is shown in the range of 200–800 nm [34]. The
maximum absorbance taking place around 500 nm is a characteristic
peak of nanometer scaled magnetic materials [35]. In the Fig. 3(b,d), all
the samples show the absorption peaks around 700 nm. It shows hy-
pochromic effect in all the sample at 900 °C with an increase in calci-
nation temperature, the absorbance band red shifts towards high wa-
velength and lower energies, indicating the increasing the size of the
synthesized sample [36]. Furthermore, the bandgap energy values of
Mg substituted nickel ferrites were calculated related to percentage of
magnesium. A plot of (αhν)2 vs energy (eV) was used to estimate the
value of the indirect band gap energy of Ni1-xMgxFe2O4 by extra-
polating the curve to the zero absorption. The slope of the (αhυ)2 values
denotes the phonon involvement in an optical process [37,38]. Ad-
ditionally, the band gap energy values decreases when the temperature
of samples at 500 °C and 900 °C as 1.32, 1.06, 1.51, 1.13 eV and 1.69,
1.46, 1.68, 1.56 eV for x = 0.25, 0.5, 0.75, 1 respectively. From the
estimated band gap values, sample at 500 and 900 °C shows the de-
crease in band gap energy with respect to magnesium concentration

102
M.K. Shobana et al. Physica E: Low-dimensional Systems and Nanostructures 108 (2019) 100–104

(a) 3.0
500 C
3.4. Electrochemical studies

1st Fig. 4(a and b) illustrate the voltage profile of Ni1-xMgxFe2O4 na-
2.5
Potential (V vs. Li /Li)

2nd noparticles (x = 0.25, 0.5 and 0.75) prepared at 500 °C and 900 °C,
3rd respectively. The discharge and charge capacities of the sample pre-
+

2.0 pared at 500 °C are found to be 1021 and 718 mAh/g with the initial
coulombic efficiency of 70%. The sample calcined at 900 °C exhibits the
1.5 discharge and charge capacities of 1099 and 747 mAh/g with the initial
coulombic efficiency of 68%. For both electrodes, the high reversible
capacities of more than 700 mAh/g are observed, indicating that the
1.0
synthesized ferrite materials can be possible candidates as anode ma-
terials for Li secondary batteries. Fig. 4c shows the cycle performance of
0.5 both materials. The capacity retention properties are still not satisfac-
tory and they should be improved by further modification.
0.0
0 200 400 600 800 1000 1200 4. Conclusions
-1
Capacity (mAh g ) The Ni1-xMgxFe2O4 materials were synthesized by sol-gel combus-
tion method. The synthesized sample (500 °C) shows the single phase
(b) 3.0 900 C
ferrite with average particle size in the range of 23–28 nm. The char-
acteristics of common ferrites were identified by the peaks below
1st 600 cm−1. The results reveal that the absorption band ν1 was produced
2.5
Potential (V vs. Li /Li)

2nd by the stretching vibration of the tetrahedral metal-oxygen bond, and

3rd
+

the absorption band ν2 was produced by the metal oxygen vibration in

2.0
octahedral site. The band gap energy values of both sample at 500 °C
and 900 °C were found to be 1.32, 1.06, 1.51, 1.13 eV and 1.69, 1.46,
1.5 1.68, 1.56 eV, respectively. Electrochemical test results showed that the
material can store Li ions reversibly with the high capacities of more
1.0 than 700 mAh/g. The synthesized materials can be possible candidates
as anode materials for Li rechargeable batteries.

0.5
Conflicts of interest

0.0 There is no conflict of interest in the current work.

0 200 400 600 800 1000 1200
-1 Acknowledgements
Capacity (mAh g )
This work was supported by the National Research Foundation of Korea
(c) 1200 500 C Li insertion Li extraction (NRF) Grant funded by the Korean Government (2015R1A5A7037615,
900 C Li insertion Li extraction 2016R1C1B1014015, and 2017H1A2A1043359).
1000
Capacity (mAh g )
-1

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