Mater. Res. Express 4 (2017) 046104 https://doi.org/10.

1088/2053-1591/aa686e

PAPER

Fabrication of anisotropic NdCeFeB hybrid magnets by

hot-deformation: microstructures and magnetic properties
RECEIVED
11 January 2017
RE VISED
14 March 2017
ACCEP TED FOR PUBLICATION
Ren-quan Wang, Ying Liu1, Jun Li, Wei Zhao and Xiao-jiao Yang
22 March 2017 College of Materials Science and Engineering, Sichuan University, Chengdu 610065, People’s Republic of China
1
PUBLISHED Author to whom any correspondence should be addressed.
21 April 2017
E-mail: liuying5536@scu.edu.cn (Y Liu)

Keywords: hot-deformation, microstructure, hybrid magnets, NdCeFeB

Abstract
An experimental study is performed on Ce-based NdCeFeB hybrid nanostructure magnets. The
hybrid magnets were prepared using a mixture of NdFeCoB and CeFeB melt-spun ribbons with
different ratios, followed by hot-pressing and subsequently hot-deformation, in which a certain
amount of Nd is substituted by Ce. For comparison, single magnets using NdCeFeB melt-spun
ribbons directly as the starting material, with the same Ce composition, were also prepared under the
same conditions. The results show that the magnetic properties and Curie temperature decrease with
increasing Ce content. The hybrid magnets have a layered structure, in which alternating layers of the
two starting alloys lay perpendicular to the pressing direction. As a consequence, the hybrid magnets
have better magnetic properties than the single magnets with the same Ce content when the Ce
content is less than 40%. With a Ce content of 20% by weight ratio, the (BH)max value of the hybrid
magnet was 32.7 MGOe, compared to 23.6 MGOe for the single magnet.

1. Introduction

In recent years, Ce2Fe14B-based magnets have attracted increased attention due to their high availability and
low-cost [1–4]. However, pure Ce–Fe–B magnets have very low magnetic properties because of their mixed-
valence state in Ce2Fe14B [5–7]. Great efforts have been made to improve the performance of Ce2Fe14B-based
magnets by researchers [8–13]. Herbst et al [8] systematically investigated the magnetic properties of Ce–Fe–B in
dependence on composition. The results suggested that the best performance was only Br  =  4.9 kG and Hci  =  6.2
kOe for melt-spun Ce17Fe78B6 powder, which is far lower than the intrinsic magnetic properties of Ce2Fe14B
(saturation magnetization 4πMs  =  11.7 kG and anisotropy field Ha  =  26 kOe at 295 K). Alam et al [6] reported
that the Ce valence in its compounds remained in a strongly mixed-valence state, which greatly inhibited the
performance of Ce2Fe14B. Interestingly, Pathak et al [14] later reported an unexpected increase of Hci (17.7 kOe)
for melt-spun (Nd0.8Ce0.2)2.4Fe12Co2B and a die-upset magnet with favorable performance Hci  =  9.4 kOe and
(BH)max  =  31 MGOe, which suggests that a certain amount of Nd substituted by Ce is beneficial for increased
magnetic properties.
With this motivation, we have developed a route for fabricating an anisotropic NdCeFeB magnet, using hot-press-
ing and subsequently hot-deformation with a mixture of NdFeCoB and the CeFeB melt-spun ribbons. The intention
is to achieve a certain amount of Nd substituted by Ce, in order to improve the magnetic properties. For comparison,
a single magnet with the same Ce substitution for Nd in NdCeFeB was also prepared under the same conditions. The
influence of the Ce content and microstructure on the magnetic properties of NdCeFeB magnets are studied.

2. Materials and methods

The raw materials, Nd (99.5 wt.%), Ce (99.5 wt.%), Fe (99.8 wt.%) and FeB alloy (80.64 wt.% Fe and 19.36 wt.% B),
were used to prepare NdCeFeB powders. Other melt-spun powders used are the commercial magnetic powders
MQP-C (Nd29.82Fe64.42Co6.76B1.0, Magnequench Inc.).

© 2017 IOP Publishing Ltd

Mater. Res. Express 4 (2017) 046104 R-q Wang et al

Two different approaches were used to prepare the Ce-based anisotropic magnets by hot-pressing and hot-
deformation with the same experimental conditions. This first approach is called ‘single magnets’, and produces
anisotropic magnets directly using (Nd1.0−xCex)32.7FebalB1.08 powder as the starting material. The second approach
is called ‘hybrid magnets’, and uses a mixture of Nd29.82Fe64.42Co6.76B1.0 and Ce32.7FebalB1.08 powders with different
ratios as starting materials.
For the first approach, a series of Ce-substituted ingots with nominal compositions of (Nd1.0−xCex)32.7FebalB1.08
(x  =  0.2, 0.4, 0.6, 0.8 and 1.0) were prepared by induction melting under an argon atmosphere. The ingots were
then crushed into small particles. Transforming the particles to melt-spun ribbons was achieved by using a molyb-
denum wheel with a surface speed of 28–30 m s−1 under an argon atmosphere. The ribbons were subsequently
crushed into 100 mesh powders. (Nd1.0−xCex)32.7FebalB1.08 powders are used as the starting material, and followed
by hot-pressing and hot-deformation to produce the ‘single magnets’. To produce the ‘hybrid magnets’, Nd29.82
Fe64.42Co6.76B1.0 and Ce32.7FebalB1.08 powders with different ratios are mechanically mixed in an agate mortar for
10 min under pure argon, and then the blends were hot-pressed and hot-deformed under the same conditions. The
two sets of raw materials mentioned above are both hot-compacted at 670 °C for 2 min at a pressure of 200 MPa
under a vacuum and subsequently hot-deformed at 750 °C by a height reduction of 70%.
For the sake of simplicity of discussion, the single magnets will be labeled as S20, S40, S60, S80 and S100 when
x  =  0.2, 0.4, 0.6, 0.8 and 1.0, respectively. Likewise, the hybrid magnets with different Ce ratios in total rare earth
(RE) will be denoted as H20, H40, H60 and H80, respectively. The number represents the content of Ce in the total
RE. For example, H20 means that the hybrid powder was made by mixing 2.78 g Ce32.7FebalB1.08 (S100) powder
with 12.22 g MQP-C powder, that is, the weight ratio of Ce accounting for 20% in the overall RE.
The crystal alignment was examined by x-ray diffraction (XRD, DX-2000) with Cu-Kα. The microstructure
was observed using field emission scanning electron microscopy (FESEM, FEI Inspect F20), energy-dispersive
spectroscopy (EDS), transmission electron microscopy (TEM, JEM-2100) and energy-dispersive x-ray spectr­
oscopy (EDX). The magnetic properties were measured using a vibrating sample magnetometer (VSM, Lake
Shore 7410) and a physical property measurement system (PPMS; Quantum Design Inc) in a magnetic field up
to 9 T and temperatures up to 1000 K.

3. Results and discussion

The demagnetization curves of the hot-deformed single and hybrid magnets are shown in figures 1(a) and (b). The
remanence (Br), intrinsic coercivity (Hci) and maximum energy products [(BH)max] all decrease monotonously
with increasing Ce content in the hybrid magnets (figure 1(b)) and the precise values are listed in table 1. For single
magnets, the variation of Br and (BH)max is similar to that of the hybrid magnets. However, an irregular increase of
coercivity is observed. The Hci of the S40 magnet is 9.23 kOe compared to that of 8.90 kOe for the S20 magnet. In
particular, both the S20 and S40 magnets have a higher coercivity than an MQP-C magnet, 8.58 kOe. The abnormal
increase of Hci in S40 may be related to the microstructure, phase distribution and the site-preference of RE atoms
in the S40 magnet. An similar phenomenon is also observed in the annealed (Nd1.0−xCex)32.7FebalB1.08 ribbons at
x  =  0.4 (not shown here). This may be ascribed to the S20 and S40 magnets having higher RE contents than MQP-C
[15]. The excessive REs in single magnets are designed to improve the process of deformation in hybrid magnets.
A peak (BH)max value of 32.72 MGOe is obtained in the H20 magnet compared to 23.66 MGOe in the S20 magnet.
Br and Hci for samples H20 and S20 are 13.27 kG, 10.52 kG, and 6.29 kOe, 8.9 kOe, respectively. In addition, the Br
for hybrid magnets is much superior to that of the single magnets under the same Ce concentration when x  ⩽  0.4
and, in contrast, this pattern disrupted when the Ce substitution for Nd exceed 60% (x  ⩾  0.6). Furthermore, the
Hci of hybrid magnets is always lower than that of single magnets, as shown in figure 1 and table 1. Apparently,
the hybrid magnets possess a higher Br and (BH)max at the expense of a lower Hci when the Ce content less than
40%. With further increasing Ce content, the magnetic properties in both kinds of magnets decrease rapidly.
Figures 1(c) and (d) show the magnetization of hot-deformed single and hybrid magnets measured as a function
of temperature in a 1 kOe magnetic field, respectively. The Curie temperature (Tc) of single magnets decreases with
increasing Ce concentration, and it varies from 223 °C for x  =  0.2 to 110 °C for x  =  1.0, as listed in table 1. The
decrease in Tc with increasing Ce concentration can be attributed to the decreasing magnetic exchange interaction
with Ce substitution. On the other hand, the hybrid magnets exhibit two transitions: a high temperature transition
(T2) and a low temperature transition (T1) which roughly correspond to a Tc of Nd2(Fe1−xCox)14B [16–19] and
Ce2Fe14B [8], respectively. This result also indicates that the raw materials remain independent of each other. The
variation of Curie temperature in the mixed magnets with different ratios of CeFeB is mainly caused by interfacial
diffusion.
In order to clarify this phenomenon, the texture and microstructure of hot-deformed magnets were further
examined by XRD, SEM and TEM. The XRD patterns are performed on the surface perpendicular to the pressure
direction for all of the hot-deformed magnets, as shown in figure 2. For the single magnets, enhanced intensity
(0 0 l) peaks are obtained for all samples except for the S100 magnet, indicating that a c-axis crystallographic

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Mater. Res. Express 4 (2017) 046104 R-q Wang et al

Figure 1. (a) and (b) Demagnetization curves of hot-deformed magnets; (c) and (d) magnetization of hot-deformed magnets
measured as a function of temperature in a 1 kOe magnetic field. (a) and (c) show single magnets and (b) and (d) hybrid magnets.

Figure 2. XRD patterns of two types of hot-deformed magnets: (a) single magnets and (b) hybrid magnets. (c) Demagnetization
curves in easy and hard directions. (d) The variation of DOT in single and hybrid magnets.

­texture is formed when x  ⩽  0.8, as shown in figure 2(a). With regard to the S100 sample, the peaks of (4 1 0), (3 1 1)
and (2 2 0) still appear as the main reflection, implying that the random orientation of grains in the pure CeFeB
magnet. In addition, some impurity phase, CeFe2, is detected. Previous research [20] revealed that the CeFe2 phase
mainly plays a impeditive role in the process of deformation due to its high melt point, 925 °C [21]. For the hybrid

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Table 1. Dependence of the magnetic properties [Br, Hci and (BH)max] and Curie temperature (Tc) on the compositions in single and
hybrid magnets.

Br/kGs Hci/kOe (BH)max/MGOe Tc/°C

Hybrid

Magnets Single Hybrid Single Hybrid Single Hybrid Single T1 T2

0% (NdFeB) 14.13 / 8.58 / 41.96 / 450a / /

20% 10.52 13.27 8.90 6.29 23.66 32.72 223 151 458
40% 9.16 10.94 9.23 4.13 17.57 17.79 204 134 442
60% 9.14 9.12 4.37 2.04 12.46 7.33 181 127 425
80% 6.03 5.16 2.53 0.98 5.24 1.75 153 134 /
100% (CeFeB) 4.50 / 0.83 / 1.26 / 110 110 /

a
Data from [17].

magnets (figure 2(b)), the reflections of (0 0 4), (0 0 6) and (0 0 8) become much stronger compared to the single
magnets, indicating that a strong magnetic anisotropy is obtained in the hybrid magnets. On the other hand, the
typical demagnetization curves of the S20 and H20 samples are measured along the parallel (ǁ) and perpendicular
(┴) directions, respectively, as shown in figure 2(c). Although both exhibit remarkable anisotropic texture, the H20
magnet has a better alignment comparing to the S20 magnet, which is in accordance with the results of XRD and
the magnetic properties. Meanwhile, the degree of texture (DOT) [(Br||  −  Br┴) / Brǁ] is a useful texture parameter
to evaluate the mean alignment of the c-axes of the 2:14:1 grains [22–24], where Br(ǁ) and Br(┴) were measured
parallel and perpendicular to the deformation direction, respectively. From figure 2(d) it can be seen that the
variation of DOT is opposite in the two magnets. For the single magnets, the DOT first increases with increasing
Ce content from 0.2 to 0.8, and then abruptly drops in the S100 magnet. The first increase can be ascribed to the
melt point of the (Nd, Ce)-rich phase gradually decreasing with the increasing of Ce content, which is beneficial
to the process of deformation [25]. As mentioned above, the inferior orientation of S100 is mainly attributed to
the phase segregation, as indicated in figure 2(a). It is noted that the values of Br decrease linearly with increasing
Ce content in spite of the DOT increasing continuously, as shown in table 1. This could be ascribed to the fact that
the intrinsic magnetic properties of Ce2Fe14B (saturation magnetization 4πMs  =  11.7 kG and anisotropy field
HA  =  26 kOe at 295 K) are inferior to those of Nd2Fe14B (4πMs  =  16 kG, HA  =  73 kOe) [19]. In contrast, the DOT
of hybrid magnets, as shown in figure 2(d), decreases monotonously with the increasing of S100 in blends, which
is mainly due to the poor texture in S100 layers, as shown in figures 3(d)–(f). This is consistent with the results of
Br values tested by VSM, as shown in figure 1(b) and table 1.
The microstructure of hot-deformed magnets was investigated by using SEM, as shown in figures 3 and 4.
First, the single magnets form a distinct two-zone structure: one zone is the typical texture consisting of fine
platelet 2:14:1 grains and the other zone, near the interfaces of the original flakes, is the coarse grain zone, as
indicated by white single arrows in figures 3(a)–(c). Early publications [26–30] pointed out that large grains are
mainly caused by the heterogeneous distribution of compositions and the uneven stress in the rough interface
between original ribbons during hot-deformation. Not only do the coarse grains hinder the process of hot-
deformation, but also become the nucleation sites of magnetization reversal domains. The crystal anisotropy
of the grains at the interface region is always lower than that inside the grains, which leads to a reduction in the
magnetic reversal nucleation field, and consequently to a decrease in coercivity [31]. However, the abnormal
increase of Hci in S40 compared to that of S20 (9.23 kOe versus 8.90 kOe) may arise from its finer grain size and
narrower coarse grains zone compared to the S20 magnet, as indicated in figures 3(a) and (b). Some analogous
phenomena were also reported by other researchers [6, 13, 14], who thought that those phenomena were related
to the microstructures, phase compositions and the valance of Ce. In the case of hybrid magnets, they possess a
totally different layered structure, in which alternating layers of the two starting alloys lie perpendicular to the
pressing direction, as shown in figures 3(d)–(f). The preferred orientation of the 2:14:1 grains was observed in
the Nd2Fe14B layers while the coarse and misaligned grains were found in the Ce2Fe14B layers. In order to further
confirm this, the chemical composition was determined using EDS in the two types of layers in the H80 magnet,
as shown by figure 3(f) and the results listed in table 2. The zone of area 2 primarily consisted of Fe (67.36 wt.%)
and Ce (32.64 wt.%) (figure 3(j)), which is very close to the composition of S100 ribbons. The region of area 1
is mainly composed of Fe (60.84 wt.%), Co (11.37 wt.%) and Nd (27.79 wt%) elements (figure 3(i)), which is
in rough agreement with the composition of MQP-C alloys. It is obvious that the well-aligned and mis-aligned
areas in hybrid magnets are corresponding with the original MQP-C and S100 ribbons, respectively. In addition,
a hot-deformed pure MQP-C magnet and S100 magnet were also examined. The former has an excellent texture
while the latter shows poor texture, as shown in figures 3(g) and (h), respectively, which is good correspondence
with the different layers in hybrid magnets.

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Figure 3. SEM morphologies of the hot-deformed magnets prepared by two different approaches with different Ce contents. Top
row: single magnets (a) S20, (b) S40 and (c) S80. Middle row: hybrid magnets (d) H20, (e) H40 and (f) H80. Bottom row:(g) MQP-C
magnet and (h) S100 magnet. The EDS profiles of (i) and (j) correspond to the marked areas in (f).

Figure 4. The magnification SEM morphologies of hot-deformed magnets: (a) the S20 magnet, (b) and (c) corresponding to the
zones marked in (a). (d) H20 magnet, (e) and (f) corresponding to the zones marked in (d).

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Table 2. The chemical composition of the H80 magnet in different areas.

Elements Nd Ce Fe Co

Area 1 27.79 / 60.84 11.37

Area 2 / 32.64 67.36 /

Figure 5. Bright field TEM images of the H20 hot-deformed magnet at different regions: (a) disorientated grains, (b) well-textured
grains and (c) high resolution TEM of the precipitation marked by circles in (a), and (d) is the corresponding EDX spectrum.

To further analyze the mechanism of orientation and magnetization reversal, the S20 and H20 magnets
were selected to investigate the microstructure at different zones. High magnification SEM micrographs of
hot-deformed magnets are shown in figure 4. An overview image of the S20 magnet is shown in figure 4(a),
where the fine rod-like grains are stacked together and, in contrast, the coarse and large grains are mainly existed
between the virgin ribbons. Figures 4(b) and (c) show magnified images of the regions marked by rectangles
in figure 4(a). The H20 magnet (figure 4(d)), is mainly composed of regular plate-like grains (figure 4(e)) and
polygonal grains (figure 4(f)). As is well known, the coercivity can be roughly estimated using the following
formula [31–33]: Hc   =  α(2K1/Ms)  −  NeffMs. Here Neff is an average effective demagnetization factor describ-
ing the internal stray fields acting on the grains, and the factor α describes the reduction of the nucleation field
due to inhomogeneous material parameters at grain boundaries and the influence of grain misorientation. The
S20 magnet has much more uniform grains and composition, and a finer grain size, but an inferior orientation
to that of the H20 magnet. In the hybrid magnets, the Ce2Fe14B layers are easy to reverse magnetically under an
external field because of their low anisotropy constant, irregular shape and the existence of an impurity phase.
Consequently, the hybrid magnets have an extremely low coercivity. In addition, early research indicates that
a good texture is a disadvantage for coercivity, while it improves the remanence due to the interaction between
aligned grains [34, 35].
Figure 5 shows the microstructure of the H20 magnet observed by TEM/EDX at different regions. It can be
seen in figure 5(a) that a lot of precipitates embedded in the major phase of Ce2Fe14B. A further high-resolution
TEM image and EDX spectrum indicate that the spherical precipitates are CeFe2 phase, as shown in figures 5(c)
and (d), respectively. As discussed above, they would first hinder the process of deformation, resulting in poor
texture in the Ce2Fe14B layers and thus deteriorating the magnetic properties. Secondly, CeFe2 is magnetically
soft at room temperature [36]. It would act as a magnetic reversal nucleation site and subsequently decrease the
coercivity of the hybrid magnets. Nevertheless, the presence of CeFe2 forms a hard/soft composite structure, which
may generate a strong exchange couple between the grains. In addition, good texture was observed in the region of
Nd2Fe14B ­(figure 5(b)), which provides high remanence for the hybrid magnets. The magnetostatic and exchange
interactions between the Nd2Fe14B layers and the Ce2Fe14B layers are supposed to further improve the Br in hybrid

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magnets [37, 38]. However, the grains on the interface will generate anisotropic internal stray fields due to the
distribution of the non-uniform grains, which lead to an inferior coercivity.

4. Conclusions

The magnetic properties of both hybrid magnets and single magnets are dependent on the Ce content—as the
Ce contents increases the magnetic properties decrease. The Curie temperature of single magnets decreases with
increasing Ce concentration while the hybrid magnets exhibit two transitions: a high temperature (T2) and a low
temperature (T1) transition, which roughly correspond to the Tc of Nd2(Fe1−xCox)14B and Ce2Fe14B, respectively.
In addition, an obviously layered structure was present in the hybrid magnet, in which alternating layers of the
two starting alloys lay perpendicular to the pressing direction. The (BH)max value of 32.7 MGOe was obtained in
the hybrid magnet with a ratio of 20% Ce, compared to 23.6 MGOe in the single magnet.

Acknowledgments

This research was supported by the Sichuan Province Science and Technology Support Program (2014GZ0090
and 2016GZ0262).

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