Ceramics International 45 (2019) 14322–14326

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Ceramics International
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Critical behavior in Ni0.15Cu0.15 Zn0.7Fe2O4 spinel ferrite T

Li-an Han , Wan-lin Zhai, Bing Bai, Hua-ze Zhu, Jing Yang, Zheng-xin Yan, Tao Zhang
∗

Department of Applied Physics, Xi'an University of Science and Technology, Xi'an, 710054, China

ARTICLE INFO ABSTRACT

Keywords: We report an in-depth investigation of the critical behavior in Ni0.15Cu0.15Zn0.7Fe2O4 (NCZFO) spinel ferrite
Critical behavior synthesized via the solid-state reaction method. The structural analysis demonstrates that NCZFO belongs to the
Spinel ferrite Fd3m space group of the cubic crystal system. The magnetic transformation in NCZFO at approximately
Magnetic transformation TC = 290 K is of the second order, as per the Banerjee criteria. Employing various models, we have attempted to
estimate the CP (critical parameter) values. The self-consistency of the CPs is confirmed by Widom's relation as
well as the scaling hypothesis. The values of the CPs manifest that the magnetic ordering in NCZFO belongs to
the Heisenberg theory in three dimensions, signifying short-range ferromagnetic interactions. The relationship
between the exchange distance (J(r)) and the spatial distance (r) in NCZFO are expected to decline as J(r)
∼r−4.947.

1. Introduction width contribution of Fe-deficient NieCueZn ferrites. Houshiar et al.

Ferrites are regarded as one of the most attractive materials because
of their potential applications such as antenna rods, recording heads,
transformer cores, loading coils and magnetic memory. Apart from their
technological importance in the magnetic and electronic industries,
ferrites can be used as gas sensors and transformer cores [1]. Among
ferrites, spinel ferrites have been gaining prominence owing to a couple
of rich microstructures, their magnetic behavior, and their dielectric
and electronic performance as well as their possible application in
spintronics, ferrofluid, catalysis, memory storage, and so forth [1–3].
Spinel ferrites possess the general stoichiometry AB2O4, where A re-
presents a divalent cation, such as Ni, Cu, Zn, Co, Mg, Mn, etc., and B
stands for the trivalent cation Fe [4]. As per the cation distribution (CD,
which can be obtained by X-ray diffraction, Mössbauer and magneti-
zation methods) [5] at the tetrahedral and octahedral positions, spinel
ferrites are classified into three types [5], i.e., normal, inverse and
mixed. Several studies have revealed that the CD in the tetrahedral and
octahedral sub-lattices of AB2O4-type ferrites has a decisive impact on
various properties, such as the microstructure, magnetism, permeability
and electronic resistivity [6–9].
Recently, the interest in NieCueZn ferrites has been rapidly in-
creasing because of their intriguing physical features. Guo et al. [10]
revealed the relationship between TC and the temperature character-
istics of the Brillouin function for NieCueZn ferrites by a nonlinear
fitting calculation. Sun et al. [11] investigated the microstructure and
static magnetic properties as well as the ferromagnetic resonance line-
[12] reported the crystal structure and magnetic and dielectric perfor-
mance of NieCueZn nanoparticles. Currently, extensive experimental
efforts have been extended towards exploring the magnetocaloric effect
(MCE) in NieCueZn ferrites for potential use as refrigerant materials
that can operate near ambient temperature. Felhi et al. [13] examined
the MCE in Ni0.3-xCuxZn0.7Fe2O4 (0 ≤ x ≤ 0.2) nanoparticles, and the
authors found that the samples exhibit excellent magnetocaloric per-
formances near room temperature. Oumezzine et al. [14] studied the
MCE of NixCu0.4Zn0.6-xFe2O4 (0 ≤ x ≤ 0.6) nanoparticles and observed
that the nickel doping increases -ΔSMmax and Curie temperature.
Although the micro-structural, magnetic, dielectric, and electronic
properties of NieCueZn spinel ferrites, as well as their MCEs, have
been extensively studied, investigations into the critical behavior in
these systems have rarely been reported. The study of the critical be-
havior of magnetic materials around their magnetic transformation is
quite significant, since establishing the relevant universality class pro-
vides more information on the range of the fundamental interactions,
from which one can draw inferences about the likely interaction me-
chanisms [15]. To shed some light on this issue, this work is focused on
two main issues. First, we have carried out the structure and magnetic
characterization of polycrystalline Zn0.7Ni0.15Cu0.15Fe2O4, verifying the
existence of a second-order magnetic transformation. Second, we have
clarified the magnetic coupling of NCZFO. In particular, the comparison
of the critical behavior of spinel ferrites is also a matter of our interest.
Our results indicate that the estimated values of the critical parameters
(CP) approach those of the Heisenberg theory in three dimensions,

∗
Corresponding author.
E-mail address: hanlianvivian@163.com (L.-a. Han).

https://doi.org/10.1016/j.ceramint.2019.04.146
Received 16 January 2019; Received in revised form 1 April 2019; Accepted 16 April 2019
Available online 17 April 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
L.-a. Han, et al. Ceramics International 45 (2019) 14322–14326

Fig. 1. XRD spectra with Rietveld analysis for the NCZFO ferrite. Fig. 2. M (T) curve at 0.01 T for the NCZFO ferrite in ZFC mode inset: The
derivate dM/dT.
implying the presence of short-range interactions in NCZFO.
method that relies on the following expression [21].
2. Experimental 1/
H T TC
= a1 + a2 M1/
M T (1)
Using the standard ceramic process, powder with a composition of
Zn0.7Ni0.15Cu0.15Fe2O4 (NCZFO) was fabricated. Stoichiometric ratios where a1 and a2 are fitting constants. The critical parameters, β and γ,
of NiO, CuO, ZnO and Fe2O3 were carefully mixed and first fired at are related to the reduced temperature t = T C by two functions [22].
T T

1273 K for 5 h. Then, the material was ground and heated at 1373 K for
C

7 h. The obtained powder was repeatedly ground and subsequently MS (t ) = M0 t , t < 0 (2)
pressed into plates of 10 mm in diameter, which were calcined at
1493 K for 5 h. To characterize the NCZFO, X-ray diffraction (XRD) was
1
0 (t ) = (h 0/ M0 ) t , t > 0 (3)
performed with the help of a Rigaku D/Max 2400 diffractometer
(λ = 1.54056 Å) in the range of 15–80°. A commercial magnetometer where Ms (≡MH = 0) stands for the spontaneous magnetization, χ0−1
was employed to obtain the magnetic characteristics of the NCZFO. (≡∂H/∂M ⎢H=0) denotes the inverse susceptibility. M0 and h0 are fitting
constants [23]. β and γ are relevant to Ms and χ0−1, respectively.
Fig. 4 depicts the results of the attempted MAP calculations using
3. Results and discussion
four sets of possible parameters including the β = 0.25 and γ = 1 (Tri-
critical mean-field theory), β = 0.325 and γ = 1.241 (Ising theory in
The Rietveld-refined XRD spectra from the NCZFO ferrite are de-
three dimensions), β = 0.345 and γ = 1.316 (XeY theory in three di-
picted in Fig. 1 and reveal that the NCZFO shows a single phase,
mensions), as well as β = 0.365 and γ = 1.386 (Heisenberg theory in
polycrystalline specimen. All diffraction peaks perfectly match the
three dimensions) [24], respectively. There are two criteria to select the
cubic spinel-type structure (JCPDS# 22–1119) belonging to the
most appropriate model: (1) all MAP curves must be straight, and the
Fd3m space group [16]. The lattice parameter, a = 0.8357 nm, is
isotherm at TC has to cross through the zero coordinate; (2) all plots
slightly larger than that of Zn0.7Ni0.3Fe2O4 [17] and is related to the
should be parallel to each other and have the same slope. Among these
partial replacement of Ni2+ (0.69 Å) by Cu2+ (0.72 Å).
models, the most appropriate universal model can be identified by
The magnetization measurements as a function of temperature (T)
plotting their normalized slopes [25] NS]S(T)/S (TC). By comparing
from 15 to 350 K at 0.01 T for the NCZFO sample are shown in Fig. 2. As
the proximity of NS to “1”, we can choose the most preferred model.
the temperature decrease, the magnetization (M) values increase
Fig. 5 displays the NS-T curves using the abovementioned possible CP,
sharply at the Curie temperature TC = 290 K, which is a signature of the
revealing that the Heisenberg theory is the most appropriate theory to
magnetic transformation from paramagnetic to ferromagnetic ordering.
disclose the critical behavior in NCZFO. The linear extrapolation from
The TC value is assigned as the temperature at which dM/dT (inset of
the high fields (μ0H ≥ 0.3 T) gives MS(T) and χ0−1(T) (see Fig. 6). By
Fig. 2) reaches its minimum. The decrease in TC can be interpreted in
multiple nonlinear fitting of the data for MS(T) and χ0−1(T), one finally
terms of the decrease in the magnetization of the B sub-lattice [18].
obtains two sets of β = 0.367 ± 0.011 with TC = 289.877 ± 0.104 K
and γ = 1.382 ± 0.049 having TC = 290.053 ± 0.021 K.
3.1. Modified arrott plot (MAP)

Fig. 3(a) presents the isothermal magnetization from 270 to 340 K 3.2. Kouvel-Fisher approach
for the NCZFO. As is well known, magnetic transformations in magnetic
materials are roughly probed through the M2 against μ0H/M curves Kouvel and Fisher (KeF) [26] suggested an effective method, which
(Arrott curves) [19]. Fig. 3 (b) illustrates the Arrott curves converted allowed the determinations of β and γ with high accuracy. Presently,
from the M (H, T) data. Two things can be seen from the Arrott curves: this method is widely used in the critical behavior investigation of
first, the presence of positive slopes throughout the range of magnetic magnetic materials [27–29]. The KeF approach on the basis of equa-
fields implies that the magnetic transformation is of second-order [20]. tions (2) and (3) is in the following form [30]:
Second, the isotherms are nonlinear and unparallel, demonstrating that 1
dMS (T ) T TC
the Landau's theory is insufficient to describe the critical behavior of MS (T ) =
the NCZFO ferrite. To obtain an accurate model, we use the MAP
dT (4)

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L.-a. Han, et al. Ceramics International 45 (2019) 14322–14326

Fig. 3. (a) M-H data for the NCZFO ferrite close to TC (b) Arrott curves for the NCZFO ferrite.

1 1
1 0 (T ) T TC
0 (T ) =
dT (5)
1 1 (T ) 1
dMS (T )
As per the KeF method, MS (T ) dT
and 0
1 (T ) 0
dT
are
linear functions of T giving slopes 1/β and 1/γ, respectively [31]. The
linear fit shows =0.364 ± 0.071 with TC = 289.783 ± 0.115 K
and =1.385 ± 0.126 having TC = 290.068 ± 0.018 K (Fig. 7). These
values are in good accordance with those from Fig. 6.
At TC, the third parameter δ relates M and H by Ref. [22].

M = H1/ , t = 0, T = TC , (6)

where is a fitting constant.

As per Eq. (6), the reciprocal of δ can be achieved by means of the
slope of Ln(M) against Ln(H) (nominal critical isothermal analysis
(CIA)). The linear fit LnM -LnH plot (Fig. 8) gives δ = 4.786 ± 0.03.

3.3. Self-consistency of the CP Fig. 5. NS vs. T for the NCZFO ferrite.

In this section, we will attempt to discuss the self-consistency of the

Using the β and γ values deduced from MAP and KeF methods, the δ
estimated CP. In an earlier study, Widom suggested that three CP, β, γ
values are found to be δ = 4.766 and 4.805, respectively. These cal-
and δ, have to obey the following relation [32]:
culated values of δ are very close to those estimated from Fig. 8, sug-
δ = 1+γ/β (7) gesting that the values of β and γ are credible.

Fig. 4. MAPs with the (a) tri-critical mean-field theory, (b) Ising theory, (c) XeY theory, and (d) Heisenberg theory for the NCZFO ferrite.

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L.-a. Han, et al.
Fig. 6. MS (T) and χ0−1 (T) data; the red lines reveal the nonlinear fits fol-
lowing Eqs. (2) and (3). (For interpretation of the references to colour in this
figure legend, the reader is referred to the Web version of this article.)
Fig. 7. K–F plots for the NCZFO ferrite.
Fig. 8. Ln(H) dependence on Ln(M) at TC = 290 K inset: linear fit using Eq. (6).
To double-check the self-consistency of the determined β, γ and TC,
we conducted the test as per the scaling relation [33].
M (H , t ) = t f± (H / t + ) (8)
where f ± is the scaling function above (+)/below (−) TC. The relation
shows the existence of two sets of universal curves, one for T lower than
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Ceramics International 45 (2019) 14322–14326
Fig. 9. Scaling curves for the NCZFO ferrite inset: the same data re-plotted on a
double-logarithmic scale.
TC and the second for T higher than TC [34]. Fig. 9 displays the M t
versus H t ( + ) relation near TC by using the values of β, γ and TC from
the KeF method. For improved clarity, the same data are drawn in the
inset of Fig. 9 on a double-logarithmic scale. Clearly, for the NCZFO
spinel ferrite, the scaling hypothesis is well followed, i.e., all data merge
into two categories; one for T < TC and the other for T > TC [35], which
indicates that the estimated CPs and TC support the scaling hypothesis.
For comparison, we list the evaluated CP values of NCZFO and the
widely used theoretical models in Table 1. Evidently, the calculated CP
values of NCZFO in this work are fairly close to those of the 3D Hei-
senberg theory.
3.4. Nature of exchange interaction
Fisher et al. suggested that J(r) relies on d and σ via the relation
[36]:
1
J (r )
r d+ (10)
where J(r), d and σ represent the exchange interaction, the lattice di-
mensionality and the range of the interaction, respectively.
Numerically, the exponent γ and σ satisfy a mathematic relation
given by Refs. [37,38]:
=1+
4 4n + 2
+
8(n + 2)(n 4)
× 1+
2G ( ) (7n + 20)
2
d 2
d n+8 2
d (n + 8) 2 (n 4)(n + 8)
(11)
2
with Δσ = σ−d/2 and G (d/2) = 3–0.25 (d/2) , here, n stands for the
spin dimensionality [39].
By solving Eq. (11), σ = 1.947 ± 0.007 can be obtained and is
mostly close to the σ = 2 for the 3D Heisenberg theory. As our sample is
a 3D material, according to relation (10), J(r) declines as r−4.947.
Hence, the critical behavior of the NCZFO belongs to the Heisenberg
theory in three dimensions together with the short-range interactions.
4. Conclusion
In summary, we have presented a detailed study on the critical
behavior of NCZFO prepared via the solid-state reaction method. The
Rietveld refinements of XRD spectra reveal that the sample exhibits a
cubic structure belonging to Fd3m space group. The Arrott plots show
that NCZFO experiences a second-order magnetic transformation at
TC = 290 K β and γ have been estimated from the MAP and KeF
L.-a. Han, et al.
Table 1
Critical parameters values of the NCZFO spinel ferrite and the theoretical models. MAP: Modified Arrott plots; KeF: Kouvel-Fisher; CIA: Critical isothermal analysis;
cal.: calculated value; exp.: experimental value; P. W.: The present work.
Composition Method TC (K) β γ
Ni0.15Cu0.15Zn0.7Fe2O4 MAP 289.97 0.367 ± 0.011
Ni0.15Cu0.15Zn0.7Fe2O4 KeF 289.93 0.364 ± 0.071
Ni0.15Cu0.15Zn0.7Fe2O4 CIA (cal.) 290 – –
Ni0.15Cu0.15Zn0.7Fe2O4 CIA (exp.) 290 – –
Mean-field model Theory – 0.5
3D-Heisenberg model Theory – 0.365
3D-Ising model Theory – 0.325
3D XeY model Theory – 0.345
Tricritical mean field Theory – 0.25
methods, and the δ values have been generated by the Ln(M) vs. Ln(H)
curve. The self-consistency of the CPs has been verified based on
Widom's relation as well as the scaling hypothesis. The estimated CP
values are close to the theoretical values given by the 3D Heisenberg
theory. This result indicates that the short-range interaction dominates
the critical behavior of NCZFO. In addition, the exchange distance in
NCZFO declines as J(r) ∼r−4.947.
Acknowledgements
This work was financially supported by the National Natural Science
Foundation of China (Nos. 11605133, 61201088) and ShaanXi
Provincial Research Foundation for Basic Research (2018JQ1047).
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