Journal of Magnetism and Magnetic Materials 519 (2021) 167496

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Journal of Magnetism and Magnetic Materials

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

Research articles

Insulation layer design for soft magnetic composites by synthetically

comparing their magnetic properties and coating process parameters
Jinghui Wang a, b, Shengqiang Song a, b, Haibo Sun c, d, Guihua Hang a, b, Zhengliang Xue a, b, *,
Ce Wang c, Weihong Chen c, Dongchu Chen d, e, *
a
State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China
b
School of Materials and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China
c
Product R&D Center, China Amorphous Technology CO., LTD, Foshan 528241, China
d
School of Materials Science and Hydrogen Energy, Foshan University, Foshan 528000, China
e
Guangdong Key Laboratory for Hydrogen Energy Technologies, Foshan University, Foshan 528000, China

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

Keywords: The soft magnetic performances of the Fe-6.5 wt.%Si (FeSi) soft magnetic composites (SMCs) insulated with
Soft magnetic composites different materials, including organic, inorganic, and soft magnetic materials with high resistivity, and composite
Magnetic properties coating of inorganic-magnetic layer, under the same fabrication condition have been compared and analyzed by
Loss-separation fitting model
synchronously considering their coating preparation parameters. The core–shell structure of the coated powder
Fe-6.5wt.%Si magnetic powders
Coating preparation condition
was characterized by using a combination of SEM-EDS, FTIR, and XRD. Loss separation fitting model was
established to evaluate the source of each part loss for the corresponding FeSi SMCs above. Due to the fact that
the SMCs insulated with inorganic or/and magnetic ferrite materials exhibit high bulk resistivity more than 1.4
Ω⋅m, their eddy current losses account for lower contribution of only 20.2 ~ 22.1% of total core loss compared
with that of 61.9% for the SMCs coated alone with organic resin. As compared to the other insulation materials,
the SMCs coated using inorganic material (SiO2 or TiO2) exhibit a better DC-bias over 75.5%, higher retain real-
part permeability exceed 44.6 at an applied field of 7960 A/m, a relatively low total core loss of 1040.6 kW/m3 at
100 kHz, 0.1 T, and can be fabricated at room temperature with a total preparation time of 70 min, which is
favorable for being widely used in industry. The results of this work offered a referable ideal to design insulating
layer for other SMCs.

1. Introduction transformers, inductors, active filters etc., and attracted growing

Soft magnetic composites (SMCs), fabricated by compacting the
mixture of resin binder and coated magnetic powders with a thin insu­
lating layer, are one kind of typical soft magnetic materials [1]. Their
intergranular insulation structure with high bulk resistivity can lead to a
stable permeability and a significant reduction of the eddy current loss
in high frequency range [1,2], as well as an anti-saturation magnetiza­
tion capability under an increasing DC-bias field [2,3]. Moreover, the
SMCs also possess the unique advantages of three-dimensional physical
property isotropy, relatively high magnetic flux density, and flexible
design with high-dimensional accuracy beneficial for the reduction in
mass production cost [4,5]. Thus, the SMCs have been commercially
used as a key component of electrical and electronics devices, such as
attention from scientists and producers over the last few decades [5–7].
Undoubtedly, coating an insulating layer with a suitable material on
the magnetic powder surface is a significant part during the fabricating
process of SMCs. The frequently-used insulation can be classified as
organic and inorganic materials. In general, the organic coating layer
can be divided into two types: thermoplastic (such as polyimide [8]) and
thermosetting (such as epoxy resin and silicone resin [9,10]). In view of
the poor thermal stability for the organic coating layer, the inorganic
coatings, such as SiO2, Al2O3, and TiO2 [9,11,12] normally prepared
using a chemical sol–gel method, which can persist at the high annealing
temperature for a long time, have been proposed as the electro-
insulation for SMCs. To mitigate the reduction in effective perme­
ability and saturation magnetic induction caused by the two types of

* Corresponding authors at: School of Materials and Metallurgy, Wuhan University of Science and Technology, 947 Heping Road, Qingshan District, Wuhan
430081, China (Z. Xue); School of Materials Science and Hydrogen Energy, Foshan University, Foshan 528000, China (D. Chen).
E-mail addresses: xuezhengliang@wust.edu.cn (Z. Xue), Chendc@fosu.edu.cn (D. Chen).

https://doi.org/10.1016/j.jmmm.2020.167496
Received 2 August 2020; Received in revised form 26 September 2020; Accepted 16 October 2020
Available online 22 October 2020
0304-8853/© 2020 Elsevier B.V. All rights reserved.
J. Wang et al.
non-magnetic coatings above, the soft magnetic coating of NiZn- [13] or
MnZn-ferrite [14] with the combined advantages of high permeability
and resistivity has been putted forward for SMCs. There are three main
approaches to coat the ferrite layer onto the magnetic powders: a)
mixing the nano-ferrite fabricated by the sol–gel method with magnetic
powders using the resin as binder [14,15]; b) compositing the ferrite,
directly prepared by a ceramic method using oxide as raw materials with
magnetic powders [16]; c) in-situ generation of ferrite on the surface of
magnetic powder via a co-precipitation method [13,17]. Recently, to
further enhance the bulk resistivity and comprehensive soft magnetic
properties of powder core, multilayer insulation core–shell structure
based on dielectric-magnetic coupled shell has been prepared and re­
ported. Li [18] et al fabricated a Fe@SiO2@(MnZn)Fe2O4 core–shell-
shell structural SMCs using a continuous co-precipitation. Luo [19] et al
presented a FeSi SMCs coated with a novel Fe2SiO4-γ-Fe2O3-Fe2SiO4
layer via high temperature sintering. However, the integrated compar­
ison of soft magnetic performances and coating preparation conditions
for the SMCs insulated with different materials, which is a worthwhile
and meaningful work to provide the basis for selecting a suitable insu­
lating material for SMCs in industrial application, has been not sys­
tematically analyzed and reported.
In this paper, the commercial Fe-6.5%Si (FeSi) powders were
employed as original powder substrate. The FeSi SMCs coated with five
different insulating layers, including organic silicon resin, inorganic
SiO2 and TiO2, soft magnetic NiZn-ferrite with high resistivity, and
composite coating layer of SiO2&NiZn-ferrite were first prepared. And
then, the comprehensive soft magnetic performances, including the
permeability and its frequency characteristic, DC-bias property, and loss
separation analysis, for the FeSi SMCs insulated with different materials
were compared and evaluated by synthetically considering their coating
preparation conditions. The results of this work will give a pertinent
advice on designing insulating coating process suitable for industrialized
production of SMCs.
2. Experimental section
2.1. Materials and reagents
The commercial gas-atomized FeSi spherical powders with size
below 75 μm (-200 mesh, the particle size ranges from 6 μm to 75 μm
and its corresponding average particle size is 37 μm) were purchased
from Hunan Ruihua Hi-Tech Material Technology Co., Ltd. Poly­
vinylpyrrolidone (PVP) with an average molecular weight of 130
kg⋅mol− 1, tetraethyl orthosilicate (TEOS, 99 wt%), and tetraethyl
orthotitanate (TBOT, 99 wt%) were purchased from Aldrich. Aqueous
ammonia solution (NH3⋅H2O, 25 wt%), anhydrous ethanol (EtOH),
acetone, silicon resin, ferric chloride (FeCl3⋅6H2O), nickel chloride
(NiCl2⋅6H2O), zinc chloride (ZnCl2), sodium hydroxide (NaOH), and
zinc stearate were from the Guangzhou Chemical Reagent Co., Ltd.
Deionized (DI) water was prepared by LDF-II water purification system
(Ludao Instruments Co, Ltd, Shanghai, China) in laboratory.
2.2. Fabrication of core–shell structural FeSi@RO2 (R = Si or Ti)
powders
The inorganic (SiO2 or TiO2) insulation layer coated on the FeSi
spherical powder surface was prepared using the conventional sol–gel
method (Eqs. (1) and (2)) for improving electrical resistivity. During a
typical synthesis procedure, the spherical FeSi powders (100 g) were
first dispersed in a mixture solution of PVP (3 g) and EtOH (200 ml) in a
500 ml three-necked round-bottomed flask under mechanical stirring
with a speed of 400 revolutions per minute (rpm) for 20 min at room
temperature. And then, a certain amount of NH3⋅H2O dissolved in DI
water (50 ml) was added into the mixture solution to adjust the PH value
into the range of 8 ~ 10. Subsequently, the silicon source TEOS (0.14
ml/g, relative to the mass of the magnetic powders) diluted in the EtOH
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Journal of Magnetism and Magnetic Materials 519 (2021) 167496
(150 ml) was poured into the reaction mixture solution under the
continuous mechanical stirring with a speed of 500 rpm for 50 min to
prepare the FeSi@SiO2 powders at room temperature. Regarding to the
fabrication of FeSi@TiO2 powders, instead of the diluted TEOS solution,
the titanic source TBOT (14 ml) dissolved in the EtOH (100 ml) was
dropwise added into the alkaline mixture using a dropping funnel for 50
min under the continuous mechanical stirring with a speed of 500 rpm at
room temperature. Finally, the as-coated FeSi powders were filtered,
rinsed with EtOH or DI water for several times, and dried in a drying
oven at 105 ◦ C for 80 min.
(C2 H5 O)4 R + 4H2 O→R(OH)4 + 4C2 H5 OH (1)
R(OH)4 →RO2 + H2 O (R = Ti or Si) (2)
2.3. Preparation of FeSi@(NiZn)Fe2O4 composite powders
Co-precipitation method was employed to create the (NiZn)Fe2O4
insulation layer on the FeSi powder surfaces. In a typical synthesis
process, the reagents of FeCl3⋅6H2O (2.3 g), NiCl2⋅6H2O (0.5 g) and
ZnCl2 (0.3 g) were dissolved in 75 ml DI water in the 500 ml round-
bottomed flask and mixed with a mechanical stirring to obtain solu­
tion A. 1.8 g NaOH was dissolved in 75 ml DI water and mixed with a
glass rod to form alkaline solution B. Hereinto, the reagent weights
above were determined according to the ratio of chemical formula
(Ni0.5Zn0.5)Fe2O4 (0.4 wt%). The prepared solution A and B were then
slowly heated up to 80 ◦ C in a diplopore water bath. Subsequently, the
solution B was gently added into solution A with a mechanical stirring
for 5 min. And then, the 100 g FeSi powders were added into the mixture
under a continuous mechanical stirring for 15 min. After a period of
settling, the obtained sludge was then repeatedly washed with DI water
until a PH value of 7 was reached. Finally, the as-coated powders were
dried at 105 ◦ C for 80 min in a drying oven. Moreover, a small amount of
the coated powder was heated at 580 ◦ C for 90 min in a tube furnace
under a nitrogen atmosphere for comparison.
2.4. Synthesis of FeSi@SiO2@(NiZn)Fe2O4 composite powders
To synthesize the FeSi@SiO2@(NiZn)Fe2O4 composite powders, the
100 g of SiO2-coated FeSi powders were first prepared according to the
fabrication route as described in the Section 2.2 above, wherein the
usage amount (0.07 ml/g) of the silicon source TEOS is half of that of
TEOS used in Section 2.2. Subsequently, the obtained FeSi@SiO2 com­
posite powders were added into the 80 ◦ C mixed solution of the solution
A (1.15 g FeCl3⋅6H2O, 0.25 g NiCl2⋅6H2O and 0.15 g ZnCl2 dissolved in
75 ml DI water) and the alkaline solution B under a continuous me­
chanical stirring for 15 min, resulting in the formation of 0.07 ml/g-
SiO2-0.2 wt%-(NiZn)Fe2O4 composite insulation layer on the FeSi
powder surfaces. Finally, the obtained FeSi@SiO2@(NiZn)Fe2O4 com­
posite powders were washed with DI water for several times and dried in
a drying oven at 105 ◦ C for 80 min.
2.5. Preparation of FeSi soft magnetic composites
1.5 wt% of thermosetting silicone resin, as an organic binder, dis­
solved in 10 ml acetone by ultrasonic treatment was added to the as-
coated FeSi magnetic powders and continuously stirred using a glass
rod until the acetone totally evaporated, followed by mixing 0.5 wt% of
zinc stearate as a lubricant agent. The collected FeSi composite powders
were subsequently compressed into toroidal powder cores with the
dimension of Φ26.9 mm (outer diameter) × Φ14.8 mm (inner diameter)
× 11.2 mm (thickness) under a pressure of 2100 MPa with a holding
time of 5 s at room temperature, marked as C-SMCs. Additionally, the
raw FeSi soft magnetic composites insulated alone with 1.5 wt% of sil­
icone resin were prepared and marked as R-SMCs for comparison.
Finally, these toroidal powder cores were orderly cured at 150 ◦ C for 1 h
J. Wang et al.
and annealed at the temperature of 580 ◦ C for 90 min under a nitrogen
atmosphere to release the internal stress caused by the cold compaction.
2.6. Characterization
The surface morphologies and element analysis of the raw FeSi
powders and the coated powders with different materials were charac­
terized by a scanning election microscopy (SEM, Phenom ProX) equip­
ped with an energy-dispersive spectrometer (EDS). The phase
identification of the coated powders was examined by X-ray diffraction
(XRD, Siemens, D500) with Cu Kα radiation at a range of 2θ = 20 ~ 90◦ .
The green compact density and bulk resistivity of the fabricated SMCs
were tested using the principle of Archimedes and an AC impedance
spectrum (Zahner, Zennium). Fourier transform infrared (FTIR) spec­
trum (FTIR, Bruker Uecior-22) was measured within a range of 400 ~
4000 cm− 1 by a Nicolet IS10 FTIR spectrometer. The SMCs’ core losses
at the frequency ranging from 25 kHz to 250 kHz with the maximum
magnetic flux density (Bm) of 0.1 T (1000 Gs) were measured by a B-H
curve analyzer (Iwastu SY-8218). The complex permeability spectra
within the range of 10 ~ 120 000 KHz, and the DC-bias performance
with the maximum applied field of 10 000 A/m were collected by an LCR
meter (Wayne Kerr 6500B) for all specimens. Hereinto, real-part (μ′ ,
equal to the effective permeability, μe) and imaginary part (μ′′ ) of the
complex permeability can be obtained by following formulas.
Ls le
(3)
′
μ =
μ0 N 2 A e
Rac le
μ′′ = (4)
ωμ0 N 2 Ae
where N is the total number of coil turns, Ls, Ae and le are the inductance,
the cross-section area, and the mean flux density path length of the ring
sample cores, respectively, Rac is the AC resistance of the core, ω is the
Fig. 1. Surface morphologies of raw FeSi powders (a), FeSi@SiO2 (b), FeSi@TiO2 (c), FeSi@(NiZn)Fe2O4 (d), and FeSi@SiO2@(NiZn)Fe2O4 (e) composite powders,
and their corresponding XRD patterns (f).
3
Journal of Magnetism and Magnetic Materials 519 (2021) 167496
angular frequency (2πf), and μ0 is the permeability of vacuum (4π ×
10− 7H/m).
3. Results and discussion
3.1. Characterization of the core–shell structural FeSi powders
Fig. 1 gives the SEM images of the morphologies of raw FeSi pow­
ders, FeSi@SiO2, FeSi@TiO2, FeSi@(NiZn) Fe2O4, and FeSi@SiO2@
(NiZn)Fe2O4 composite powders, and their corresponding XRD patterns.
The raw FeSi powders are almost in spherical shape within size range of
6 ~ 75 μm and exhibit good dispersion and relatively smooth surfaces.
As compared to the surfaces of the raw FeSi powders, the surface of the
chemically coated powder became rough and was uniformly clad with
something, and the as-coated powders appeared aggregation to some
extent (as shown in Fig. 1 (b ~ e)). The XRD patterns of both the FeSi
powders before and after chemical coating process as shown in Fig. 1 (f)
exhibit three diffraction peaks centered at 44.7◦ , 65.3◦ and 82.8◦ ,
indicating that only a single body-centered cubic α-Fe (Si) solid-solution
without other phase presented, confirming that the thickness of the
inorganic and/or magnetic coating layer on the FeSi powder surface is
extremely thin [18].
To characterize the core–shell structure of the FeSi powders, Fig. 2
presents SEM images of the chemically coated FeSi powders and their
EDS elemental distribution maps and spectrums. As shown in Fig. 2(a)
and (b), besides the signals of Fe, Si, and O elements, Ti element signal,
Ni and Zn element signals are also uniformly presented on the FeSi
powder surfaces after chemical coating process using sol–gel technique
and co-precipitation method, respectively. Additionally, as shown in
Fig. 2(e), the EDS spectrums exhibit that the O element signals on all the
chemically coated FeSi powder surfaces are obviously enhanced. Here­
into, as compared to that of the raw FeSi powder, the maximum mass
fraction of the O element on the coated FeSi powder surfaces increases
J. Wang et al. Journal of Magnetism and Magnetic Materials 519 (2021) 167496

Fig. 2. SEM images of FeSi@TiO2 (a), FeSi@(NiZn)Fe2O4 (b), FeSi@SiO2 (c), and FeSi@SiO2@(NiZn)Fe2O4 (d) composite powders and their EDS elemental dis­
tribution maps (a, b) and spectrums (e).

from 0.92 wt% to 5.12 wt%. These results above indicated that the
FeSi@TiO2 and FeSi@(NiZn)Fe2O4 composite powders may have been
obtained. The C element signal in the corresponding EDS patterns pri­
marily came from the conducting resin to fix the magnetic powders on
the specimen stage. Meanwhile, it is also observed that the Si signals are
amplified when the FeSi powders coated by the sol–gel technique and
the composite approach (sol–gel plus co-precipitation methods) using
the silicon source TEOS. Hereinto, the corresponding Si concentrations
separately increase to 10.47 wt% and 8.46 wt% from the mass fraction
of 6.44 wt% in the raw FeSi powders, indicating that both the SiO2
coating layer and the composite coating layer of SiO2&(NiZn)Fe2O4 may
have been formed on the FeSi powder surfaces in combination of the
existence of Ni and Zn signals in the EDS pattern.
To further verify the existence of different coating layers on the FeSi
powder surfaces, Fig. 3(a) gives the FTIR spectra of the FeSi powders
before and after chemical coating process via sol–gel method. Obvi­
ously, there is no distinct absorption peak for the raw FeSi powders,
while some characteristic peaks appeared for the coated powders. The
broad absorption bands centered at 3441 cm− 1 and 1632 cm− 1 can be
attributed to the –OH bond stretching vibrations from the chemisorbed
water [20]. The stretching vibration of C=O caused by the atmospheric
CO2 can be observed at the absorption peak of 2349 cm− 1 [21].

Fig. 3. (a) FTIR spectra of the FeSi powders before and after chemical coating process via sol–gel method, (b) XRD patterns of the coated powders with raw pre­
cipitate and annealed powders at 580 ◦ C for 90 min.

4
J. Wang et al.
Moreover, for the case using TEOS as the single-source precursor, the
strongest absorption peak centered at 1098 cm− 1 is owing to the
asymmetric stretching vibration of Si-O-Si [22]. The absorption peaks of
803 cm− 1 and 467 cm− 1 are associated with the symmetric stretching
vibration of Si-O-Si [22]. The stretching vibration of Si-OH gives rise to
the absorption peak located at 949 cm− 1 [23]. For the case using TBOT
as the single-source precursor, the absorption band in the range of 500
~ 800 cm− 1 is associated with the stretching vibration of Ti-O-Ti
[12,24]. The asymmetric stretching vibration of Ti-O gives rise to the
absorption peak of 1037 cm− 1 [24]. These results above further indi­
cated that the SiO2 or TiO2 layer has been deposited on the FeSi powder
surfaces
Fig. 3(b) presents the XRD patterns of the coated powders with raw
precipitate using the co-precipitation method and their corresponding
heated powders at 580 ◦ C for 90 min. Except for the three characteristic
peaks of 44.7◦ , 65.3◦ and 82.8◦ for the phase of α-Fe (Si) solid-solution,
no other sharp peaks in the XRD pattern were observed for the coated
FeSi powders, indicating that the raw precipitate on the FeSi powder
surface has not crystallized. For the coated powder annealed at 580 ◦ C
for 90 min, many new Bragg peaks in the XRD pattern appeared as
compared to that of the coated powder with raw precipitate. The new
peaks centered at 2θ values of 30.1◦ , 35.5◦ , 43.1◦ , 53.7◦ , 56.8◦ and 62.8◦
are associated with the (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1) and (4 4 0)
planes of Ni0.5Zn0.5Fe2O4 coating phase with spinel structure (JCPDS
Card No. 52-0278), respectively. Generally, the simplified chemical
pathway for the formation of Ni0.5Zn0.5Fe2O4 coating layer can be
summarized as following formulas (5) and (6). Hereinto, at the stage of
co-precipitation, the hydroxides in Eq. (5) were deposited on the powder
surfaces. And then, at the annealing stage, a well-crystallized NiZn-
ferrite with formula of Ni0.5Zn0.5Fe2O4 can be obtained as shown in Eq.
(6). Thus, an equation for the overall reaction above can be described as
in Eq. (7) [25].
Zn2+ + Ni2+ + Fe3+ + 7OH − →Zn(OH)2 + Ni(OH)2 + Fe(OH)3
when annealed at 580 C: ◦
0.5Zn(OH)2 + 0.5Ni(OH)2 + 2Fe(OH)3 →Ni0.5 Zn0.5 Fe2 O4 + 4H2 O
Zn2+ + Ni2+ + 4Fe3+ + 16OH − →2Ni0.5 Zn0.5 Fe2 O4 + 8H2 O
3.2. Magnetic properties of FeSi SMCs
Fig. 4 presents the frequency dependences of real (μ′ ) and imaginary
(μ′′ ) parts of complex permeability within the range of 10 ~ 120 000 kHz
for the R-SMCs and the C-SMCs insulated with different coating mate­
rials and their corresponding green compact densities and bulk re­
sistivities. Hereinto, the core specimen was winded turns of 10 with
copper wire of Φ1.4 mm to ensure a stable and strong input signal during
testing process for complex permeability. No obvious reduction in μ′ can
Fig. 4. Frequency dependences (a) of real and imaginary parts of complex permeability within the range of 10 ~ 120 000 kHz for the R-SMCs and the C-SMCs
insulated with different coating materials and their corresponding green compact density and bulk resistivities (b). (For interpretation of the references to colour in
this figure legend, the reader is referred to the web version of this article.)
Journal of Magnetism and Magnetic Materials 519 (2021) 167496
be observed even increasing the frequency up to 2000 kHz (2 MHz) for
all the C-SMCs. On the contrary, seen from Fig. 4(a), gradual attenuation
in the μ′ began to emerge when the frequency over 100 kHz for the R-
SMCs (fabricated using the FeSi particles coated alone with silicon
resin). These phenomena above can be mainly attributed to the mag­
netic powders favorably insulated with each other beneficial for
enhancement of electrical resistivity of SMCs, leading to an increase in
the relaxation frequency (fr) shown as the Eq. (8) [26]. Hereinto, as
shown in Fig. 4 (b), the C-SMCs exhibit a higher bulk resistivity up to 3.8
Ω⋅m as compared to that of 0.007 Ω⋅m for R-SMCs. Generally, the
attenuation rate of μ′ with increasing test frequency can be delayed by
increasing the value of fr as shown in Eq. (9) [27] from the Visser’s
coherent model. The μ′′ reveals the energy losses relating to the hys­
teresis response and eddy current, and its peak position corresponds to
the fr [28]. The μ′′ for all core specimens exhibit low values in a wide
frequency range of 10 ~ 200 kHz, but then grow up with further
increasing frequency. The decrease of μ′′ at the very beginning fre­
quencies should be caused by the decreasing field current induced by the
increasing AC resistance of copper coil when the skin effect appeared
[29]. Moreover, it is observed that the value of R-SMCs’ fr is 16.6 MHz,
while all the C-SMCs did not attain their fr in the maximum frequency
test range of the employed LCR meter owing to their high electrical
resistivities.
ρb
fr = (8)
2πμ0 μi d2
1
(9)
′
μ = μi
1 + f 2 /fr2
where ρb is the bulk electrical resistivity of SMCs, μi and d are separately
the initial permeability and the effective particle dimension.
Moreover, as depicted in Fig. 4 (b), the bulk densities of the C-SMCs
insulated with different materials are nearly equal and fluctuate within a
(5)
small range of 5.75 ~ 5.76 g/cm3. For the μ′ , it is observed that the C-
SMCs coated with NiZn-ferrite magnetic layer show a largest μ′ of 73.8 at
100 kHz as compared to these of the R-SMCs and the C-SMCs insulated
(6)
with other materials. Obviously, the introduction of soft magnetic ferrite
can be beneficial to elevating the SMCs’ μ′ , which is owing to that the
(7)
NiZn-ferrite can be much easier to be magnetized than the non-magnetic
materials, such as the silicon resin, SiO2 and air gaps, between the FeSi
powders in the SMCs. Under this situation, the C-SMCs coated with
composite coating layer of SiO2&(NiZn)Fe2O4 exhibit a higher μ′ than
that of C-SMCs insulated with SiO2 or TiO2 layer. Furthermore, it is seen
that the R-SMCs posses a relatively higher μ′ of 69.4 at 100 kHz than
these of the C-SMCs coated with the layer of SiO2, TiO2, or SiO2&(NiZn)
Fe2O4. This should be mainly ascribed to its high bulk density of 5.79 g/
cm3, which can help for reducing the volume fraction of non-magnetic
phase (Vn, Eq. (10) [2,23]) in the SMCs, thus weakening the intensity
of effective demagnetizing field, resulting in the increase of μ′ for the R-
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J. Wang et al. Journal of Magnetism and Magnetic Materials 519 (2021) 167496

SMCs. where the Bm is the maximum magnetic induction, Kh and a represent

rt − rb the hysteresis simulation coefficients.
Vn = × 100% (10)
rt Eddy current occurred in the soft magnetic composites under an
alternating magnetic flux can be separated into two different physical
where rt and rb are separately the true and apparent bulk densities of parts. The first part is inter-particle eddy current flowing between the
SMCs. magnetic powders insulated not well with each other in the entire cross-
Another significant magnetic property of the SMCs is the core loss section of SMCs, while the other part is intra-particle eddy current
(the amount of energy dissipation per unit volume or mass) determining flowing in the sale of single magnetic powder. Thus, the eddy current
the conversion efficiency of powder cores in the power application. loss is composed of inter- (Pinter intra
e ) and intra-particle (Pe ) eddy current
Based on the classical Bertotti’s [30] and Kollar’s [31] loss separation losses, and can be calculated by the following formulas.
theory, the total core loss per unit volume (Pcv, in kW/m3) can be divided
into three different parts: hysteresis loss (Ph), eddy current loss (Pe), and (π de Bm f )2 (πdp Bm f )2
Pe = Pinter + Pintra = + = Ke B2m f 2 (13)
excess loss (Pexc), and can be expressed as follows. e e
β 1 ρs β 2 ρp

Pcv = Ph + Pe + Pexc (11) 6

β1 = (14)
The value of pH can be calculated by multiplying the measured area 1 − 0.633 whtanh(1.58h
w
)
of hysteresis loop under quasi-static condition by frequency (f), thus can
be expressed as bellows. (π de )2 (πdp )2
Ke = + (15)
∮ β 1 ρs β2 ρp
Bf
Ph = dB = Kh Bαm f (12)
μ0 μe
where Ke is the eddy current loss coefficient, ρs and ρp separately

Fig. 5. Three-dimensional surfaces of the total core loss (a), the hysteresis loss (b) and the eddy current loss (d) versus frequency and the maximum magnetic flux
density, fitting results for Ph/f vs. Bm (c), Pexc vs. f (e), and Aexc vs. Bm (f) for the R-SMCs and the C-SMCs insulated with different materials.

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J. Wang et al. Journal of Magnetism and Magnetic Materials 519 (2021) 167496

represent the electrical resistivity of SMCs and FeSi particle (5.5 × 10− 7 C-SMCs insulated with non-magnetic materials, wherein the non-
Ω⋅m). dp represents the diameter of FeSi particle, and de is the effective magnetic coatings would increase the number of pinning sites that
eddy current dimension, which is equal to the shorter side of the rect­ impede the domain wall movement.
angular cross section of SMCs. β1 represents the geometrical factor for Moreover, according to the Bertotti’s [30] statistical theory for the
the rectangular cross section of SMCs, wherein the w and h represent the exceed loss portion, the number of domain wall movement during
width and height of the rectangle, respectively. β2 is the granular magnetic process at the cross section of core specimen can be identified
geometrical factor (for the spheres, β2 = 6). with the number n of active magnetic objects. For the SMCs, the number
Regarding to the excess loss (Pexc), it comes from the eddy currents n exhibits a close relationship to the exceed field Hexc owing to that the
mainly caused by the domain wall branching and bowing [2,28], and Pexc originates from the compensation of inhomogeneous internal
can be obtained by subtracting the Ph, Pinter
e , and Pe
intra
from the measured counter-field under an applied field, and can be described as following
value of Pcv. Considering that the Pexc is strongly associated with several Eqs. (17)–(19). Fig. 6 gives the dependence of Hexc on the n at Bm = 0.05
variables of the applied magnetic induction, frequency, number of active T for the FeSi C-SMCs and R-SMCs. Hereinto, the values of n0 and 1/V0
magnetic objects, and cross section area of the material perpendicular to can be obtained by linear fitting the relation of n vs. Hexc. It is observed
the magnetic flux [32]. Thus, the Pexc can be fitted by the following that the n increases with the elevating Hexc, manifesting that more
formula [33]. thermal energy to active the domain wall from defects and pores will be
generated with the increasing f. Comparing the C-SCMs coated with non-
Pexc = Kexc Bβm f γ = Aexc f γ (16)
magnetic coating layer, the C-SMCs insulated magnetic ferrite layer
possess more active magnetic objects beneficial for increasing number of
where Kexc, Aexc, β and γ are the simulated coefficients.
domain wall movement, which will generate less energy consumption
Fig. 5(a) gives the three-dimensional (3D) surfaces of total core loss
by promoting the magnetic interaction between the coated powders,
(Pcv) versus f and Bm for the R-SMCs and the C-SMCs insulated with
leading to the corresponding lower Ph and Pexc as shown in Fig. 5. Based
different coating materials. Clearly, the R-SMCs present a relatively
on the discussion above, Table 1 listed the coefficients of each formula of
higher Pcv than these of the C-SMCs in the whole measuring ranges of f
different partial losses for the FeSi C-SMCs and R-SMCs.
and Bm due to its lower electrical resistivity as shown in Fig. 4. As
compared to other coating materials, the C-SMCs insulated with NiZn- 16GSB2m f 2
(17)
ferrite soft magnetic layer exhibit the lowest Pcv of 974 kW/m3 at 100
n=
Pexc ρp
kHz for Bm = 0.1 T. Moreover, it is observed that the values of Pcv for the
C-SMCs insulated with inorganic materials of SiO2 and TiO2 are essen­ Pexc
Hexc = (18)
tially equal. To further analyze the variation rule of Pcv, the loss sepa­ 4Bm f
ration study has been carried out as follows according to the Eqs. (11)–
(16). n = n0 +
Hexc
(19)
Fig. 5 (b) displays the 3D surfaces of pH v.s. f and Bm for the R-SMCs V0
and C-SMCs insulated with different coating materials. As the soft
magnetic coating material, the C-SMCs insulated with NiZn-ferrite where G (=0.1356) is a dimensionless geometrical coefficient, S is the
magnetic layer show the minimum Ph in the given testing range cross section area of powder core perpendicular to the magnetic flux, n0
compared with these of the R-SMCs and the C-SMCs insulated with non- and V0 separately represent the number of activated domain walls and
magnetic materials, such as SiO2 and TiO2. Moreover, the variable of Ph/ the material parameter connected with the local pinning field.
f is the hysteresis energy loss (unit in J/m3) under quasi-static condition, DC-bias property is another significant performance index deter­
representing the value of energy loss per volume in SMCs in one com­ mining the size and rate power of SMCs used in the power applications.
plete magnetization cycle, and can be obtained by experimentally Fig. 7(a) displays the dependence of DC-bias field on the percent
measuring the area of the quasi-static hysteresis loop according to the permeability, defined as the ratio between the μ′ under a DC-bias field
Eq. (12). Thus, the hysteresis coefficients of kh and a in Eq. (12) can be and the μ′ at no DC-bias field, for the R-SMCs and C-SMCs insulated with
obtained by fitting the nonlinear curve of Ph/f v.s. Bm using a power different coating materials. As the DC-bias field increases, the SMCs are
function for the C-SMCs and the R-SMCs as depicted in Fig. 5(c). It is
seen that the C-SMCs insulated with NiZn-ferrite magnetic layer exhibit
a minimum kh of 661 as compared these of SMCs coated with other
materials, while the value of the coefficient a for all the FeSi SMCs
mentioned above is in the range of 2.02 ~ 2.05.
Obviously, as shown in Fig. 5(d), the R-SMCs (prepared using the
FeSi powders coated alone with silicon resin) exhibit a much higher Pe as
compared to those of C-SMCs (prepared using the chemically coated FeSi
powders), which can be contributed to their higher electrical resistivity
as shown in Fig. 4. Under this situation, it is observed that the Pe of R-
SMCs contributes about 61.9% of Pcv (total core loss), while the Pe of C-
SMCs only accounts for approximate 20.2 ~ 22.1% of Pcv within the test
frequency range of 25 ~ 250 kHz.
Fig. 5(e) shows the frequency dependence of Pexc for the R-SMCs and
C-SMCs insulated with different coating materials at Bm = 0.1 T. Ac­
cording to Eq. (12), the coefficients of Aexc (KexcBβm) and γ at Bm = 0.1 T
can be obtained by fitting the nonlinear curve of Pexc v.s. f using a power
function for the SMCs mentioned above. And then, the coefficient of Aexc
at different values of Bm can be obtained. Subsequently, the nonlinear
power fitting curve of Aexc v.s. Bm, as well as Kexc and β can be gained as
depicted in Fig. 5(f). Moreover, it is also shown that the C-SMCs coated
with NiZn-ferrite magnetic layer exhibits the minimum Pexc of 147.7 Fig. 6. Dependences of exceed field on the number of active magnetic objects
kW/m3 at 100 kHz, 0.1 T as compared with these of the R-SMCs and the at a maximum induction of 0.05 T and their corresponding linear fitting results
for the R-SMCs and the C-SMCs insulated with different materials.

7
J. Wang et al. Journal of Magnetism and Magnetic Materials 519 (2021) 167496

Table 1
Coefficients of each formula of different partial losses for the FeSi C-SMCs and R-SMCs.
Different coating conditions Ph Pe Pexc n0 1/Vo

Kh a Ke Kexc β γ

FeSi@resin 706 2.04 9.15 1.98 1.82 1.55 954.7 561.1

FeSi@TiO2 766 2.02 1.22 2.28 1.87 1.61 864.9 158.8
FeSi@SiO2 785 2.04 1.22 2.29 1.86 1.62 770.7 124.7
FeSi@(NiZn)Fe2O4 661 2.03 1.23 2.02 1.86 1.53 1236.2 829.8
FeSi@SiO2@(NiZn)Fe2O4 749 2.05 1.21 1.81 1.75 1.57 869.8 283.4

Fig. 7. Dependence of DC-bias field on the percent permeability (a) and the retained permeability at an applied field of 7960 A/m (b) for the R-SMCs and C-SMCs
insulated with different coating materials.

progressively magnetized and eventually saturated. Accordingly, the
inductance, Ls, and μ′ for all the SMCs gradually decrease. In view of that
the values of μ′ at no DC-bias field for the R-SMCs and C-SMCs are
different (seen from Fig. 4), the value of retained permeability at an
applied field (H) of 7960 A/m (μ′ @7960 A/m) has practical meaning to
electromagnetic design in power applications. Fig. 7(b) shows the values
of μ′ @7960 A/m for the corresponding SMCs above. It is observed that
the C-SMCs insulated with the inorganic SiO2 or TiO2 layer exhibit
relatively high percent permeability over 75.5% at H = 7960 A/m and
μ′ @7960 A/m greater than 44.6, while the R-SMCs and the C-SMCs
coated with NiZn-ferrite magnetic layer show comparatively low
percent permeability below 61.5% for H = 7960 A/m and μ′ @7960 A/m
less than 40.6. Moreover, the C-SMCs coated with the composite coating
layer of SiO2&(NiZn)Fe2O4 exhibit a relative high percent permeability
of 71.6% for H = 7960 A/m and highest μ′ @7960 A/m of 47.1. The
reason leading to these phenomena above can be attributed to that the
non-magnetic insulating layer (SiO2 or TiO2) can offer an equivalent of
distributed air gap, which can hinder the domain wall motion for SMCs
during magnetization process, thus suppressing the reduce of the real-
part permeability. Inversely, the easily magnetized NiZn-ferrite layer
on the FeSi powder surfaces or the case of the particles not perfectly
insulated to each other (R-SMCs) will be conductive to accelerating the
magnetization process of powder core under an increasing DC-bias field,
leading to the rapid decrease in the real-part permeability.
Table 2 summarizes the soft magnetic properties of R-SMCs and C-
SMCs and their corresponding coating process parameters under the
same fabrication conditions, including powder size distribution,
compaction pressure and annealing process. It is seen that the C-SMCs
coated with the composite coating layer of SiO2&(NiZn)Fe2O4 exhibit a
favorable comprehensive soft magnetic performance, including rela­
tively high μ′ of 67.4 at 100 kHz, good DC-bias property of 72.4% at H =
7960 A/m, and low Pcv of 990.9 kW/m3 at 100 kHz for Bm = 0.1 T. But
the FeSi@SiO2@(NiZn)Fe2O4 SMCs faced two salient imperfections:
long total preparation time exceed 110 min and high synthesis tem­
perature of 80 ◦ C, which go against the popularization in industrial
application. For the FeSi@(NiZn)Fe2O4 SMCs, two obvious problems:
low DC-bias property below 55% at H = 7960 A/m and high reaction
temperature of 80 ◦ C, are observed. As compared to the FeSi@(NiZn)
Fe2O4 SMCs, the C-SMCs insulated using inorganic material (SiO2 or
TiO2) show a better DC-bias over 75.5% and higher retain μ′ exceed 44.6
at H = 7960 A/m, and can be fabricated at room temperature with a
preparation time of 70 min, which is favorable for being widely used in
industry. Moreover, both the FeSi@SiO2 and FeSi@TiO2 SMCs exhibit a
much lower of Pcv of 1040.6 kW/m3 at 100 kHz for Bm = 0.1 T compared
with that of 1692.3 kW/m3 for R-SMCs. Based on the discussion above,
The inorganic insulating materials (such as SiO2 or TiO2) are recom­
mend to be the coating layer for SMCs for better meeting the further
developments of rated power, energy efficiency, and frequency band of
electronic devices in the near future as compared to the magnetic
coating material prepared using in-suit co-precipitation method.
4. Conclusions
The Fe-6.5 wt% soft magnetic composites coated with different

Table 2
Comparison of soft magnetic properties and coating preparation parameters for different powder cores under the same fabrication condition.
Powder cores μ′ @100 kHz μ′ @7960 A/m DC-bias @7960 A/m Pcv(kW/m3) Coating preparation parameters

50 kHz, 0.05 T 100 kHz, 0.1 T Total time, min Preparation temperature, ◦ C

FeSi@resin 69.4 40.4 59.4% 143.6 1692.6 about 15 Room temperature

FeSi@TiO2 59.6 44.5 75.5% 102.1 1040.6 70 Room temperature
FeSi@SiO2 60.2 45.0 75.1% 103.9 1048.6 70 Room temperature
FeSi@NiZn-ferrite 73.8 39.6 54.3% 87.8 921.7 40 80
FeSi@SiO2@NiZn-ferrite 66.4 47.1 71.2% 95.2 990.9 110 80

8
J. Wang et al.
insulating materials of organic resin, inorganic SiO2 and TiO2, magnetic
NiZn-ferrite, and composite coating layer of SiO2&NiZn-ferrite have
been successfully fabricated. The soft magnetic performances compari­
son for the FeSi SMCs above was carried out under the synchronous
consideration of coating process parameters. The main conclusions can
be draw from this work as below.
1. The easily magnetized NiZn-ferrite layer on surface of FeSi powders
is beneficial to evaluating the real-part permeability of FeSi SMCs,
but also to accelerating the magnetization process of SMCs under an
increasing DC superposition field, leading to a relative low DC-bias
property below 55% at H = 7960 A/m.
2. The FeSi@SiO2@(NiZn)Fe2O4 SMCs exhibit a favorable soft mag­
netic performance, including high μ′ of 67.4 at 100 kHz, good DC-
bias property of 72.4% at H = 7960 A/m, and low Pcv of 990.9
kW/m3 at 100 kHz, 0.1 T, but possess two obvious shortcomings of
long total preparation time exceed 110 min and high synthesis
temperature of 80 ◦ C.
3. As compared to the other insulation materials, the C-SMCs insulated
with inorganic material exhibit a better DC-bias over 75.5% and
higher μ′ @7960 A/m exceed 44.6, a relatively low total core loss of
1040.6 kW/m3 at 100 kHz, 0.1 T, and can be fabricated at room
temperature with a total preparation time of 70 min, which is
favorable for being widely used in industry.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This research was funded by the Guangdong Provincial Science and
Technology Program (Grant No. 2019A050510050), Guangdong Prov­
ince Key Project of Foundation and Application Foundation Research
Joint Fund (Grant No. 2019B1515120020), Characteristic Innovation
Projects of Universities in Guangdong Province (Grant No.
2019KTSCX194), Characteristic Innovation Projects of Universities in
Foshan City (Grant No. 2019XCC06) and Foshan Municipal Key Tech­
nology Tackling Program (Grant No. 1920001001392).
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