Journal of Magnetism and Magnetic Materials 489 (2019) 165411

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Journal of Magnetism and Magnetic Materials

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Research articles

Characterization of texture and magnetic properties of Ni0.5Zn0.5TixFe2−xO4 T

spinel ferrites
⁎
Jiyu Hu, Xiansong Liu , Xucai Kan, Shuangjiu Feng, Chaocheng Liu, Wei Wang,
Khalid Mehmood Ur Rehman, Mudssir Shazed, Shengqiang Zhou, Qiuyue Wu
Engineering Technology Research Center of Magnetic Materials, School of Physics & Materials Science, Anhui University, Hefei 230601, PR China

A R T I C LE I N FO A B S T R A C T

Keywords: In this paper, The aim is to evaluate the magnetic properties and structure of Ni-Zn doped ferrites with trivalent
NiZn spinel ferrites Ti4+ cations substitute in Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) synthesized by conventional solid state method.
Morphological The magnetic properties, surface morphology, and cations distribution of the ferrites have been investigated by
Magnetic properties X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer
Permeability
(VSM). The experimental results shown that under the optimum doping content, the real permeability µ′ can
reaches 345H/m. The nanocrystal of composition Ni0.5Zn0.5Fe1.9Ti0.1O4 has the maximum value of
Ms = 117.6 emu/g as evinced in VSM measurements. Meanwhile, the real permeability µ′ was improved sig-
nificantly with the increase of Ti substitution when x ≤ 0.1, and decreased when x > 0.1.

1. Introduction successfully synthesized and investigated microstructure, magnetic and

permeability properties systematically. The sample prepared in this
With the rapid development of science and technology, the spinel work displayed a considerable performance in soft magnetic char-
ferrites are known as the most universal soft magnetic materials due to acteristic and high frequency permeability. Meanwhile, better soft
their prominent magnetic properties for high frequency applications magnetic properties we hoped to obtain including low porosity, high
[1,2]. Spinel ferrites are widely applied in aerospace area, transporta- permeability and large saturation magnetization (Ms) are achieved in
tion region, medical field, electric power and normal domestic appli- this work.
ance are all tightly integrated with soft magnetic materials [3–5],
owing to its higher-value of high magnetization, high Curie tempera- 2. Experimental details
ture, large porosity, high resistance (up to 108 Ω·m) and low power loss
at high frequency [6–8]. Therefore, it is valuable to further research the 2.1. Synthesis of specimens
properties of Ni-Zn soft magnetic material systematically.
For spinel ferrites, due to its large oxygen ion radius, the lattice All samples of Ni-Zn spinel ferrites with the composition of
structure takes oxygen ions as the dense accumulation. The metal ion Ni0.5Zn0.5TixFe2−xO4 (x = 0.0, 0.1, 0.2, 0.3, 0.4, 0.5) were prepared by
radius is small and filled in the clearance of dense accumulation [9]. the solid-state reaction. The raw materials used in this study are TiO2
There are large amount of relative literatures proved that the Ni2+ ions (99.8% purity), ZnO (99% purity), Fe2O3 (98.5.8% purity) and Ni2O3
prefer to occupy the octahedral position (B-site) in Ni0.5Zn0.5Fe2O4 (72% purity). These raw materials were weighted according to the
ferrites materials [10–12]. The Zn2+ ions have the characteristic of formula and mixed in the planetary mill for 3 h. The mixing progress
occupation “A” site, and Fe3+ ions both prefer to occupy “A” and “B” were operated by using two size of hardened steel balls with diameters
sites. Therefore, replacing the Fe3+ ions with some appropriate cations of 5 mm and 8 mm obey the ratio of 2:1, and ball-to-powder weight
will cause meaningful characteristics in soft magnetic properties. The obey the ratio of 15:1. Consequently, the dried gel was placed in an
purpose of this study is to investigate the specific effect on micro- oven at a temperature of 150 °C. Then, the powders were pre-sintered at
structure and soft magnetic properties replace the occupation of Fe3+ a temperature of 1000 °C for 3 h. After this, the second ball mill process
ions with doping Ti4+ ions [13,14]. were operated with adding (0.08% CaCO3, 0.03% MoO3, 0.025% Bi2O3,
In this study, Ni-Zn ferrites with various Ti4+ ions additions were 0.04% V2O5 and 0.08% Co2O3) additives and wet milled for 2 h. Then

⁎
Corresponding author.
E-mail address: xiansongliu@ahu.edu.cn (X. Liu).

https://doi.org/10.1016/j.jmmm.2019.165411
Received 15 April 2019; Received in revised form 31 May 2019; Accepted 3 June 2019
Available online 04 June 2019
0304-8853/ © 2019 Elsevier B.V. All rights reserved.
J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

the powder samples were pressed into toroids (Φ18 mm × Φ9

mm × h3.6 mm) under 20 MPa. Finally, the powders were calcined at a
temperature of 1200 °C for 2 h and the good quality sample could be
obtained.

2.2. Characterization

The phase of prepared samples was analyzed by X-ray dif-

fractometer (XRD, Rigaku D/max-2550 V/PC) with Cu Kα
(λ = 1.5406 Å) radiation. Scanning electron microscopy (SEM) was
used to investigate the microstructure. Energy Dispersive X-Ray
Spectroscopy (EDX) was used to verified the chemical composition.
Fourier transformer infrared (FTIR) spectrometer was done to in-
vestigate the infrared spectral analysis. M(T) curve was performed by a
Quantum Design superconducting quantum interference device mag-
netic property measurement system (SQUID-MPMS 3). M(H) curve was
Fig. 2. The tendency of lattice parameter and cell volume for
carried out by using a Quantum Design superconducting quantum in- Ni0.5Zn0.5Fe2−xTixO4 (x = 0–0.5) spinel ferrites.
terference device vibrating sample magnetometer (SQUID-VSM). The
permeability and core loss were characterized by the B-H alternating
current magnetic (AC) characteristic analyzer (Riken Denshi ACBH- bigger than that of Fe3+ (0.67 Å) [15], so the lattice parameter increase
100K). a little with increasing Ti4+ doping content, and this will lead to the
peak shift as expected in the pattern.
Fig. 2 gives the plot of lattice parameters (a, b and c) and cell vo-
3. Results and discussion lume (V) for all Ni0.5Zn0.5Fe2−xTixO4 samples, the values are calculated
by the following equations [16]:
3.1. Analysis of structure and composition
−1/2
4 h2 + hk + k 2 l2
dhkl = ⎛ ∙ + 2⎞
Powder XRD patterns of Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) fer-
⎜ ⎟

3 a2 c
⎝ ⎠ (1)
rites are shown in Fig. 1. The reflection planes (2 2 0), (3 1 1), (4 0 0),
(4 2 2), (5 1 1), (4 4 0) and (5 3 3) confirm the formation of single- 3 2
phase cubic spinel structure for samples. The patterns match the stan- Vcell = a ∙c
2 (2)
dard Ni0.5Zn0.5Fe2O4 ferrite alignment card (PDF# 08-0234). As seen
that when x = 0.3, two small miscellaneous peaks start to appear in Here, dhkl is the interplaner spacing, h, k and l are the Miller indices,
patterns, and these two miscellaneous peaks are the phase pattern of and the calculated values are listed in Table 1. As shown clearly that
TiO2 and α-Fe2O3, and gradually get higher with x content increase. lattice parameter and cell volume display the same trend, which are
With the increasing of titanium, it gets oxidized by the air and as a closely related with the result of XRD analyses.
result of TiO2 appeared. Because Ti4+ ions take the place of Fe3+ ions The surface morphologies of Ni0.5Zn0.5Fe2−xTixO4 are shown in
sites so the extruded Fe3+ ions is oxidized by air into α-Fe2O3. The Fig. 3. As shown, doping titanium into the sample has a certain influ-
enlargement part of Fig. 1 in the 2θ = 34°–37° range exhibits an ob- ence on its size and structure. The average grain size increases slightly
vious shift to lower diffraction degree for 311 peak, this is due to the with the addition of titanium and the results show that the average
truth that the difference of ionic radii. The ionic radii of Ti4+ (0.69 Å) is particle size of the sample is estimated within the range of 1 μm. In

Fig. 1. The XRD patterns of Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) spinel ferrites.

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J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

Table 1 are two relatively low peaks under each main peak, which represent the
The lattice parameter and cell volume of all Ni0.5Zn0.5Fe2−xTixO4 samples. distribution of ionic strength in different valence states [18]. From the
Comp. (x) a(Å) b(Å) c(Å) V(Å3) discussion of XPS analysis, the types of elements in Ni-Zn spinel ferrites
materials and the distribution of the valence states of various elements
0 8.3325 8.3325 8.3325 578.53 are specifically investigated, the valence status results of major cations
0.1 8.3765 8.3765 8.3765 587.73
are consistent with the information of chemical formula as expected.
0.2 8.3901 8.3901 8.3901 590.61
0.3 8.3707 8.3707 8.3707 586.52
The Fourier transformer infrared (FT-IR) spectra of the sample is
0.4 8.3686 8.3686 8.3686 586.09 shown in Fig. 5. As depicted clearly, there are two specific absorption
0.5 8.3899 8.3899 8.3899 590.58 bands within the scope of 400–700 cm−1 and these are the typical
characteristics of Ni-Zn spinel structures [19]. A clear phenomenon in
the spectra exhibit the obvious slight shift of the absorption peaks can
short, all sample possess uniform grain size and distribute homo- be observed, which may attribute to the difference of the distance be-
geneously during the substitution. As known the difference of ionic tween octahedral and tetrahedral sublattice sites. The two absorption
radii between Ti4+ and Fe3+ ions, the difference between the ionic bands in the 400–700 cm−1 scale can be divided into range of high
radii of different ions will cause the phenomenon of the grain size in- frequency bands (wave number 595 cm−1–673 cm−1) and the low
creases slightly as shown in the morphology. frequency bands in the range of wave number 410 cm−1–438 cm−1,
Fig. 4 shows the XPS spectra of Ni0.5Zn0.5Ti0.1Fe1.9O4 sample re- which are common characteristics of all spinel structures [20]. Since
vealing the valence state distribution of elements on the surface. As can the Fe3+eO2− bond lengths for tetrahedron and octahedron positions
be seen in Fig. 4, the Fe 2p spectrum can be separated into three main are different, the high and low frequency bands are in accordance with
peaks. Peaks at 733 eV, 725 eV and 710 eV are associated with metallic the stretching vibration of Fe3+eO2− composite vibrations in tetra-
Fe species. There are four major peaks situated on 879.2 eV, 873 eV, hedral and octahedral positions respectively [21]. The low frequency
861 eV and 855 eV as illustrated are assigned to Ni 2p1/2 and Ni 2p3/2. band moved into lower frequencies because titanium ions prefer to
As shown, two main peaks situate on 1044.7 eV and 1021.8 eV as il- occupy A sites and that the difference in the ionic radius of A sites ions
lustrated are assigned to Zn 2p1/2 and Zn 2p3/2 [17]. In addition, there (Ti4+ and Fe3+) are much longer than that of B sites ions (Ni2+ and

Fig. 3. SEM images of the Ni0.5Zn0.5Fe2−xTixO4 powders (a-f: x = 0.0–0.5); The follow inset is EDX spectroscopy for Ni0.5Zn0.5Fe2O4.

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J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

Fig. 4. XPS spectra of Ni0.5Zn0.5Ti0.1Fe1.9O2 spinel ferrites and photoelectron peaks for Ni 2p, Zn 2p and Fe 2p.

to the vibration of FeeOH, CeO and C]O bonds respectively [6].

3.2. Analysis of magnetic performance

Fig. 6 shows the temperature dependent magnetic behavior of all

samples with different titanium doping conditions in two different
modes (ZFC and FC). Specifically, as can be seen from Fig. 6(a)–(f), ZFC
means cooling to a certain temperature without magnetic field, and
then adding magnetic field to measure the curve of magnetization in-
tensity with temperature change. FC means that after measuring the
zero field cooling curve, the magnetic field is used to measure the curve
of magnetization changing with temperature while cooling. It's visible
from the image that they all are ferrimagnetic behavior and the
blocking temperature of them are above 390 K [23]. When x = 0.1,
Tp = 314 K, which is significantly higher than that of pure sample
Tp = 285 K. According to Weiss theory of molecular field therefore, it
can be seen that the working temperature and application range are
significantly improved by substituting [24].
Fig. 7 shows magnetic hysteresis curves for Ni-Zn spinel ferrites
Fig. 5. Fourier transformer infrared (FT-IR) spectroscopy of the
Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) sample. powders with different titanium doped at a low temperature of 5 K. The
saturation magnetization (Ms) firstly increases at x ≤ 0.1, and then
decreases at x > 0.1 with increasing titanium content, which reaches
Fe3+). With increasing titanium quantity of A sites increased the radius
the maximum value 117.6 emu/g at x = 0.1. Fig. 8 shows the magnetic
of site, which thus lowers the frequency. And the transport of Fe3+ ions
hysteresis curves for all samples at room temperature. Obviously, the
to octahedral site cause a rise in the frequency, with A site being filled
change trend basically exhibit the same trend as that at 5 K, except that
with Ni2+ and Fe3+. Therefore, the band positions of the high and low
it is relatively small in numerical value due to the influence of mole-
frequency bands will be different theoretical [22]. The peaks appearing
cular thermal disturbance. For spinel ferrites with a large O2− radius,
around wavenumber of 839 cm−1, 1097 cm−1 and 1641 cm−1 are due
the lattice structure is densely packed with O2− ions layer. The metal

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J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

Fig. 6. Temperature dependent magnetization of Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) sample.

ion radius is small and filled in the gap of dense accumulation. There decreased when Ti4+ ion substituted [27,28]. Therefore, Ms will exhibit
are 64 A-sites formed by tetrahedral gaps and 32B-sites formed by oc- an increases situation with the increase of titanium substitution.
tahedral gaps, but only 8 A-sites and 16B-sites are actually filled. It is However, with the further increase of titanium substitution, excessive
well known that the Zn2+ ions prefer to occupy the A site, the Ni2+ ions non-magnetic Ti4+ ions will begin to occupy the B-site of octahedron,
occupy the B site, and the Fe3+ ions occupy both the A and B sites [21]. causing the two Fe3+ ions in octahedron position to be replaced by Ti4+
For spinel ferrites, the net magnetic moment can be defined as and Fe2+ ions (2Fe3+ → Ti4+ + Fe2+) [28]. As the magnetic moment
following [25]: of Fe3+ ion is 5 µB, and the magnetic moment of Fe2+ ion is 4 µB, B-sites
magnetic moment will decrease undoubtedly and lead to a decrease in
→ →
|M| = |MA + MB| = MB − MA (3) Ms with the increase of titanium substitution eventually.
Fig. 9 shows the frequency dependence of real permeability (µ′) for
where MA and MB are the magnetic moment of A and B sublattices [26]. Ni0.5Zn0.5Fe2−xTixO4 (0 ≤ x ≤ 0.50) spinel ferrites with the external
Accordingly, the results of Ms can be explained that Ti4+ ions will oc- magnetic field Hm = 50 A/m under the frequency range of
cupy the A sites first, as the concentration of A site is lower than B site, 100 kHz–1000 kHz. As depicted clearly, µ′ increases significantly with
and Ti4+ ions will replace Fe3+ ions at the tetrahedral position. Since the doping of titanium and reaches the maximum value µ′ = 340 at
Ti4+ ion is non-magnetic, the magnetic moment at A site should be

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J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

significant improvement as substituting in an appropriately extend.

When excessive titanium is doped, that is, when x = 0.3, x = 0.4 and
x = 0.5, µ′ decreases obviously compare with the pure sample. As
known, the initial permeability µi ∝ 1/K, here, K is magnetocrystalline
anisotropy. So the high µi want to be obtained, the sample can mix and
tune the materials with the properties of +K1 and −K1 in a certain
proportion, so that the small K1 can be obtained and result in a sig-
nificant improvement in the performance of Ni-Zn spinel ferrites. As
MFe2O4 has a high K1 in numerical values (K1 = −3.9), the addition of
a small amount of Ti4+ will increase the cationic concentration of Fe2+
(K1 > 0). Therefore, substituting a small amount of Ti4+ will reduce
the K1 value of the material, while substituting proper Ti4+ ions will
further decrease the K1 value and lead to µi increase [29]. Hence, the
relationship between the real permeability (µ′) and frequency will final
exhibit in Fig. 9. Initial permeability (μi) can be calculated by the fol-
lowing equation [29]:

μi = Ms2·D / K1 (4)
Fig. 7. Magnetic hysteresis loops of the samples at 5 K. Here, Ms is the saturation magnetization, K1 is the magnetocrys-
talline anisotropy constant, D is the average grain size. It can be seen
that in the range of x < 0.2, with the addition of titanium, Ms is de-
creased, D is slight increased initially then decreases rapidly, and K1
decreases a little. The change of µ′ may attribute to the different speed
of the K1 and Ms various ratio [30].
Fig. 10 shows the variations of power loss Pcv changing with fre-
quency at the maximum magnetic flux density Bm = 5 mT. As can be
seen from the picture clearly that the power loss increases with fre-
quency magnify. When x < 0.3, the power loss Pcv increases slightly
with the content of titanium. While the power loss Pcv increases sig-
nificantly when titanium substitution at x > 0.3. Generally, the sample
exhibits a promising application in soft magnetic field as high perme-
ability and low power loss can be obtained through this doping effort.

4. Conclusion

In summary, titanium additions positive impact the structural and

magnetic behavior of Ni-Zn ferrites by influencing the nanostructure. It
is observed that the magnetic properties, structure, and real perme-
Fig. 8. Magnetic hysteresis loops of the samples at 300 K. ability (µ′) are sensitively controlled by titanium substitution in Ni-Zn
ferrites. The various concentration of Ti4+ ions has effect on values of
lattice parameter and average grain size. The real permeability (µ′)
gradually increased with the increase of titanium substitution when
x ≤ 0.1, and decreased when x > 0.1. The values of core loss (Pcv)
augmentation with increase in Ti4+ substitution. The saturation

Fig. 9. Frequency dependence of real permeability µ′ for the samples with

different Ti addition in the frequency range of 100 kHz-1000 kHz.

x = 0.1, while begin to decline with the titanium content when x ≥ 0.3.
It is clearly obtained from figure that the titanium content at x < 0.3
Fig. 10. Power loss for the samples with different Ti addition with different
the values of µ′ are much higher than the pure sample, indicating a
frequency under the maximum flux density Bm = 5 mT.

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J. Hu, et al. Journal of Magnetism and Magnetic Materials 489 (2019) 165411

magnetization (Ms) firstly increases at x ≤ 0.1, and decreases at distribution, J. Alloys Compd. 696 (2017) 28–41.
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