Materials and Design 192 (2020) 108767

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Materials and Design

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

Property enhancement of bonded Nd-Fe-B magnets by composite

adhesive design
Wang Xi, Weiqiang Liu, Ruijin Hu, Yuxia Yin, Ming Yue ⁎
College of Materials Science and Engineering, Key Laboratory of Advanced Functional Materials, Ministry of Education of China, Beijing University of Technology, Beijing 100124, China

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Composite binder combines the advan-

tages of both epoxy and sodium silicate
to increase compatibility.
• The developed binder improved re-
markably application performance of
bonded magnets.
• The enhancement mechanism of com-
prehensive properties is revealed.

a r t i c l e i n f o a b s t r a c t

Article history: Bonded neodymium iron boron (Nd-Fe-B) magnets with excellent properties were prepared by using
Received 26 February 2020 waterborne-epoxy resin/sodium silicate composite binder (W-EP/SS). The results show that this composite
Received in revised form 28 April 2020 binder can endow the bonded magnets with high temperature resistance as well as strong corrosion resistance.
Accepted 29 April 2020
In addition, the compressive strength of W-EP/SS bonded magnet is higher than other types of bonded magnets.
Available online 4 May 2020
W-EP/SS composite binder has excellent homogeneity, which can coat the magnetic powders uniformly during
Keywords:
mixing and curing, and therefore forms a protective thin film on the surface of the magnet to prevent thermal
Bonded magnet oxidation under high temperature conditions as well as corrosion during chemical treatments. Moreover, the
Composite W-EP/SS composite binder, which combines the toughness of epoxy resin with the rigidity of sodium silicate, en-
Modification dows bonded magnets better mechanical properties. It is attributed to the co-existence of Si-O-Si and C-O-C net-
Epoxy resin work structure in the W-EP/SS. Therefore, it is expected that W-EP/SS composite binder will provide a broader
Sodium silicate application prospects for future bonded magnets.
© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction developed in the direction of miniaturization, complicated-shapes, and

The applications of small magnets continue to increase with the
growth of electronic consumer products; meanwhile the magnets are
⁎ Corresponding author at: 100 Pingleyuan, Chaoyang District, College of Materials
Science and Engineering, Beijing University of Technology, Beijing 100124, China.
E-mail address: yueming@bjut.edu.cn (M. Yue).
high-performance. Neodymium iron boron (Nd-Fe-B) based permanent
magnets with excellent magnetic performance are usually fabricated by
hot deformation, sintering, and bonding methods [1–5]. However, hot
deformation and sintering for complicated-shaped magnets would aug-
ment the manufacturing cost and result in much waste of energy and
rare earth resources due to the follow-up process of grinding or cutting
[6–12]. For comparison, the Nd-Fe-B magnets prepared by bonding

https://doi.org/10.1016/j.matdes.2020.108767
0264-1275/© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
2 W. Xi et al. / Materials and Design 192 (2020) 108767
Fig. 1. The preparation process of waterborne-epoxy resin/sodium silicate composite binder.
method exhibit significant advantages in shape diversity, and therefore
are widely used in electronics, new energy vehicles, etc. [13–20].
At present, the usual binder used in the industrial production of
bonded magnets is solid epoxy resin (EP) [21] due to its easy molding
and processing. However, the rapid development of motors for electric
cars brings specific requirements of high temperature resistance, anti-
corrosion, and high strength for bonded magnets [22–28]. However,
the poor high temperature resistance, corrosion resistance, and me-
chanical performance of the EP binders have limited the application of
bonded magnets in high-end fields. In recent years, many researchers
have focused on enhancing the high temperature resistance of bonded
magnets. Some researchers used high-melting-point polymer binders
such as polyamide (PA12) [22,23] and polyphenylene sulfide (PPS)
[25] to prepare bonded Nd-Fe-B magnets. The high temperature resis-
tance of PA12 and PPS bonded magnets has been improved. However,
the processing technic for PA12 and PPS bonded magnets is more diffi-
cult compared with other polymer binders. More importantly, the ther-
moplastic resins can be easily deformed in the high temperature
environments of over 150 °C. Therefore, there is a need for new adhe-
sives that could endow these magnets with excellent high temperature
magnetic properties, high mechanical properties, and corrosion resis-
tance simultaneously [29–31].
In our previous work, to solve the problem of temperature tolerance
of bonded magnets, we introduced sodium silicate (SS) binder into
bonded magnets [32,33] and obtained noteworthy enhancement of
their high temperature resistance [34]. Meanwhile, we also found that
sodium silicate binder was easy to absorb water. Thereafter, we
combined epoxy resin (EP) with SS to form a physical-composite binder
(EP/SS) used in bonded Nd-Fe-B magnets, which could prevent water
absorption and improve high temperature resistance and short-term
corrosion resistance [35]. Unfortunately, the physical-composite binder
has poor uniformity in bonded magnets due to the different hydrophi-
licity and hydrophobicity between EP and SS binders. Therefore, the me-
chanical properties of bonded magnets are undesirable. Moreover, the
corrosion phenomenon in EP/SS bonded magnets was still observed in
long-term corrosion resistance tests. Therefore, in this work, we modi-
fied the molecular structure of EP by introducing a hydrophilic group
to form waterborne epoxy resin (W-EP) with chemical methods,
which improved the compatibility of EP and SS binders. In this study,
we present our results from a systematic study on the magnetic proper-
ties, corrosion resistance, and mechanical properties of W-EP/SS bonded
magnets.
2. Experimental
2.1. Materials
(1) Isotropic Nd-Fe-B magnetic powders were purchased from
Magnequench Co., Ltd. (Tianjin, China). The magnetic properties of iso-
tropic Nd-Fe-B powders are as follows: Intrinsic coercivity (Hcj):
9.2–9.9 kOe; remanent magnetization (Br): 8.83–8.93 kG; maximum
magnetic energy product (BH)max: 14.8–15.8 MGOe. (2) Sodium silicate
was purchased from Gains Chemical Company, with the following pa-
rameters: modulus of 3.1–3.4, Baume degree of 40° ± 1; (3) The liquid
 W. Xi et al. / Materials and Design 192 (2020) 108767 3

Fig. 2. The synthetic reaction process of W-EP.

epoxy resin was purchased from Blue Star New Chemical Material Co.,
Ltd. with the model of E-51; (4) Maleic anhydride (MAH) and Polyeth-
ylene glycol 2000 (PEG-2000) was supplied by Gains Chemical Com-
pany. (5) Dicyandiamide was purchased from Tianjin Fuchen
Chemical Reagent Co., Ltd.
2.2. Preparation of water-epoxy resin/sodium silicate composite binder
In order to solve the compatibility between EP and SS, we adopt liq-
uid epoxy resin to modify it by chemical method. The preparation pro-
cess and reaction mechanism of waterborne epoxy resin/sodium
silicate (W-EP/SS) composite binder is shown in Figs. 1 and 2. The
mole ratio of PEG-2000, MAH and epoxy resin is 1:2:2. The acidic
value of the solutions is a critical issue for the preparation of W-EP.
PEG-2000 and MAH were mixed in a container with stirrer at
80–90 °C. The MAH undergoes esterification reaction with hydroxyl (-
OH) of PEG-2000 molecular chain, so both ends of PEG-2000 generate
carboxyl (-COOH) bond. At the moment, the MAH occurs in ring-
opening reaction, and the acidic value reduces with increasing the

Table 1
The magnetic properties at 20 °C and 200 °C of four types of bonded magnets.

Samples Br (kG) Hcj (kOe) BHmax (MGOe) Density (g/cm3)

3%W-EP/SS 6.28 9.73 8.42 5.53

3%SS 6.25 9.40 8.26 5.46
3%EP 6.17 9.35 8.17 5.28
3%EP/SS 6.21 9.32 8.23 5.37
200 °C-3%W-EP/SS 4.88 4.82 4.73 –
200 °C-3%SS 4.77 4.54 4.47 –
200 °C-3%EP – – – –
Fig. 3. The acidic value of first step reaction (PEG-2000 and maleic anhydride) and second
200 °C-3%EP/SS 4.83 4.74 4.56 –
step reaction (adding E51 epoxy) at different time.
4 W. Xi et al. / Materials and Design 192 (2020) 108767
reaction time as shown in Fig. 3. When the reaction time extends to
2.5–3 h, the acidic value is invariant, indicating the first step reaction
is in equilibrium. Subsequently, the E-51 epoxy resin was added into
the mixed solutions. The epoxy groups of the epoxy resin occur ring-
opening esterification reaction with carboxyl, and the carboxyl bond
disconnects. Thus, the acidic value continues to reduce on the basis of
the first step. At 8 h, the acidic value becomes close to 0, indicating
that the second step reaction has completed. After cooling, W-EP was
obtained by adding 40 wt% distilled water. Subsequently, SS and W-EP
were mixed with the ratio of 1:9 to obtain the W-EP/SS composite
binder.
2.3. Preparation process of bonded Nd-Fe-B magnets
First, 96.9 wt% Nd-Fe-B powders, 3 wt% W-EP/SS binder and 0.1 wt%
dicyandiamide were mixed and stirred to obtain a uniform mixture and
the magnetic particles become dry. Second, the mixture was poured
into a mold to get a compact bulk by exerting pressure. Third, the bulk
was removed from the mold and subjected into isostatic pressing to
densify with a pressure of 240 MPa for 200 s. Finally, the W-EP/SS
bonded magnets were obtained by curing at 170 °C for 1 h. At the
same time, EP/SS bonded magnet, EP bonded magnet, and SS bonded
magnet were prepared by using the same magnetic powders and the
same binder content (3 wt%) for comparison.
2.4. Characterization
The magnetic properties of the bonded Nd-Fe-B magnets with the
size of 15.0 × 15.0 × 7.0 mm were characterized at 20 °C and 200 °C
by hysteresis loop instrument (NIM\\500C) based on the GB/T 24270-
2009 testing method.
The corrosion resistance of the bonded magnets was evaluated by
salt spray test at the room temperature in a 5 wt% sodium chloride
(NaCl) solution with pH value of 6–7.
The molecular structure and chemical group of the bonded magnets
were analyzed by Fourier Transform Infrared Spectroscopy (FTIR, Nico-
let 5700). The spectral range of spectral is from 400 cm−1 to 3500 cm−1.
The compressive strength of the bonded magnets with sizes of
14.0 × 7.0 × 7.0 mm was tested by electronic tensile testing instrument
(Zwick 050) based on the GB/T 7314. Microscopic morphology and en-
ergy spectrum analysis were performed using scanning electron micro-
scope (SEM-EDX, Tescan Vega II). The elemental distribution of the
internal structure of W-EP/SS bonded magnet was characterized by
Electron Probe Micro-Analyzer (EPMA, 1720H).
3. Results and discussion
3.1. Analysis of magnetic properties of the magnets
The magnetic properties of four types of bonded Nd-Fe-B magnets
are shown in Table 1 and Fig. 4. The magnetic properties among four
types of bonded magnets is similar because they adopt same magnetic
powders and binder content (3 wt%). The remanence of bonded mag-
nets is determined by the density of the bonded magnets. Comparing
with other three types of bonded magnets, the W-EP/SS bonded magnet
present slightly higher density and remanence. Thus, we infer that the
W-EP/SS bonded magnet possesses better structural regularity due to
the excellent homogeneity and the mobility of the W-EP/SS composite
binder. On the other hand, excellent coating homogeneity of binder
can prevent magnetic powders from oxidation, which is important for
maintaining high coercivity of the bonded magnets [21,34]. The high
curing temperatures will aggravate thermal oxidation of the Nd-Fe-B
powders and decrease the magnetic properties. The SS and W-EP/SS
bonded magnets exhibit slightly higher coercivity, indicating that SS
and W-EP/SS binders can prevent Nd-Fe-B powders from thermal oxi-
dation during high temperature curing. The reason could be that W-
EP/SS and SS can coat the magnetic powders evenly and thus reduce
the proportion of magnetic powder exposed to air, which decreases
thermal oxidation of Nd-Fe-B magnetic powders.
In our previous work [34], the magnetic data of the EP bonded were
not obtained since the epoxy could not keep the original shape of the
magnet at 200 °C. While in this work, W-EP/SS bonded magnet, EP/SS
bonded magnet, and SS bonded magnet still have usable magnetic prop-
erties at 200 °C. This suggests that SS can effectively improve the me-
chanical strength of magnets at elevated temperature.
3.2. Analysis of corrosion resistance of the magnets
Corrosion resistance is an important factor for the applications of
the bonded magnets. In this work, the corrosion mechanism of the
bonded magnets after the salt spray test was investigated by SEM-
EDX. In detail, the salt spray tests of the four types of bonded mag-
nets were carried out in 5 wt% NaCl solution for 72 h, and the cor-
roded morphology of the bonded magnets were observed every
24 h, as shown in Fig. 5.
The EP bonded magnet was the most corroded after 24 h, showing
brown rust on the surface. With increasing the test time to 48 h, corro-
sion phenomenon began to occur on the partial surface of EP/SS bonded
magnet and the corrosion area also increased. The corrosion phenome-
non was not observed on the surface of W-EP/SS and SS bonded magnet
even after testing for 72 h. We can infer that W-EP/SS and SS binder can
coat the magnetic powders uniformly during the process of mixing and
curing, which was verified by EDX observation in Fig. 6. The good coat-
ing substantially reduces the corrosion area of the bonded Nd-Fe-B
magnet.
In order to investigate the corrosion mechanism, the micromorphol-
ogy and compositions of four types of bonded magnets after salt spray
test were analysis, as shown in Fig. 6. Many needle-like substances
with high Fe and Nd content exist in the EP/SS and EP bonded magnets,
indicating that these two types of bonded magnets are easy to be cor-
roded. The high concentration Fe and Nd is derived from the exposed
magnetic powders due to the non-uniform coating of EP binder. On
the contrary, SS and W-EP/SS with good mobility can fully coat the mag-
netic powders to isolate the corrosive substances in salt spray corrosion
tests. Therefore, the EDX analysis data of SS and W-EP/SS bonded mag-
nets show low Fe and Nd content.
Fig. 7 displays the corrosion interface of EP/SS bonded magnet. It is
found that there are three regions with different morphological charac-
teristics in EP/SS bonded magnet. The region A represents SS area where
Fig. 4. The demagnetization curves of four types of bonded magnets at 20 °C and 200 °C.
 W. Xi et al. / Materials and Design 192 (2020) 108767 5

Fig. 5. The corrosion morphology of different bonded magnets after salt spray test for different times.

corrosion does not occur, while the region C represents EP area where
corrosion has occurred previous. The region B represents the transition
area between region A and C. Combined with EDX analysis, we can infer
that the corrosion has occurred at the more concentrated location of EP.
The EP could not coat the magnetic powders ideally and results in the
exposure of magnetic powders, which react with O2 or Cl− to form
oxide or chloride in NaCl solution. As a result, the EP region contains
needle-like substances, and presents high Fe content. However, SS
with good mobility can fully coat the magnetic powders to isolate the
corrosive substances in NaCl solution. Therefore, the SS region in EP/SS
bonded magnet exhibits a smooth surface and low Fe content. The rea-
son for this phenomenon is that the physical mixing of EP/SS binder has
poor compatibility, which could not coat on the surface of the magnetic
powders uniformly, and the exposed magnetic powders are easy to ox-
idize or corrode in NaCl solution. As a result, we modified the molecular
structure of EP by introducing a hydrophilic group to form waterborne
epoxy resin (W-EP), which improved the compatibility of EP and SS
binders, and thus enhance the corrosion resistance of the bonded
magnets.
3.3. Analyses of Fourier transform infrared spectrometer of the magnets
The molecule structure and group in EP and W-EP/SS bonded mag-
nets are illustrated by Fourier transform infrared spectrometer, (FTIR)
as shown in Fig. 8. The peaks of Si-O-Si and C-O-C have been marked
in the figure. The peak positions at 1033 cm−1, 804 cm−1, and
6 W. Xi et al. / Materials and Design 192 (2020) 108767

Fig. 6. Micromorphology and energy spectrum analysis of different bonded magnets after salt spray test. a: SS; b: W-EP/SS; c: EP/SS; d: EP.

460 cm−1 correspond to Si-O-Si asymmetric stretching (as-s), symmet- W-EP/SS magnets combine Si-O-Si and C-O-C chemical bonds simulta-
ric stretching (s-s), and Si-O-Si bending vibration (b), respectively neously. It can be expected that combination between Si-O-Si and C-
[33,34]. On the other hand, the peak position of 1510 cm−1 and O-C chemical bond could benefit to the heat resistance and mechanical
1450 cm−1 corresponds to C-O-C structure. FTIR analysis shows that properties of bonded magnets.

Fig. 7. The corrosion mechanism of EP/SS bonded magnet.

 W. Xi et al. / Materials and Design 192 (2020) 108767
Fig. 8. The Fourier transform infrared spectrometer curve of bonded magnets with EP and
W-EP/SS binders.
3.4. Analyses of compressive strength of the magnets
Fig. 9 shows the compressive strength of four types of bonded mag-
nets at 20 °C. The compressive strength of SS bonded magnet (78 MPa)
is larger than that of EP bonded magnet (27 MPa). SS binder has a good
bonding ability, which can increase the compressive strength by
forming the Si-O-Si network structure [34]. EP/SS binder prepared by
physical mixing method exhibits non-uniform feature due to the unde-
sirable compatibility between EP and SS. Therefore, EP region and SS re-
gion could be distinguished in EP/SS bonded magnet, as shown in Fig. 7.
As a result, EP with poor compressive strength brings negative effect for
the compressive strength of EP/SS bonded magnet. The mechanical
properties of EP/SS bonded magnet fall in between the EP and SS
bonded magnets. On the other hand, the chemical modification could
improve the compatibility between W-EP and SS, which can make the
W-EP/SS binder to form a uniform and stable structure. W-EP/SS binder
combining the toughness of EP with the rigidity of SS can play a syner-
gistic effect on the bonded magnet, so its compressive strength can
reach 95 MPa, which is 79.2% higher than that of EP/SS bonded magnet.
Fig. 10 displays the compressive strength of the four types of bonded
magnets at 200 °C. The EP bonded magnets exhibit poor strength due to
poor heat-resistance. However, the W-EP/SS boned Nd-Fe-B magnets
still have high compressive strength at 200 °C which is 59% higher
than that of EP/SS boned magnets.
Fig. 9. The compressive strengths of bonded magnets with different binders at 20 °C.
7
Fig. 10. The compressive strengths of bonded magnets with different binders at 200 °C.
3.5. Analysis of internal microstructure of W-EP/SS bonded magnets
To further explore the bonding mechanism, SEM and EPMA were ap-
plied to verify the role of W-EP/SS composite binder in the system. As
shown in Fig. 11, the morphology of magnetic powders presents neatly
a brick-type structure. The composite adhesive has good fluidity, so
magnetic particles can rotate to form a tightly arranged structure during
the prepressing process. It reveals that the improvement of internal reg-
ularity endows the bonded magnets with good mechanical and mag-
netic properties simultaneously.
In addition, the distributions of Nd, Si, and C elements in W-EP/SS
bonded magnet reveal that most binders are concentrated in the gap be-
tween the magnetic particles. Meanwhile, the results also confirm that
EP and SS have excellent compatibility by chemical modification. More-
over, we can find that the Si and C distribute at the same position. Given
that W-EP/SS bonded magnet combine Si-O-Si and C-O-C chemical
bond simultaneous in Fig. 8, we speculate that the co-existence of Si-
O-Si and C-O-C network structure in the W-EP/SS bonded magnet
plays a synergistic effect on the enhancement of the compressive
strength.
4. Conclusion
Bonded Nd-Fe-B magnets have been prepared with chemical modi-
fication by a composite W-EP/SS binder. The magnetic properties, me-
chanical properties, corrosion resistance, and microstructure have
been systematically investigated. The excellent compatibility of W-EP/
SS composite binder by chemical modification could endow the mag-
nets with outstanding performance, including high temperature resis-
tance, strong corrosion resistance, and high mechanical properties.
The excellent compatibility and mobility of W-EP/SS composite binder
protect the bonded Nd-Fe-B magnet from thermal oxidation under
high temperature conditions and corroding in chemical conditions. In
addition, W-EP/SS composite binder has synergistic effect between EP
and SS with Si-O-Si and C-O-C chemical bonds on increasing the com-
pressive strength of the bonded magnets and high temperature resis-
tance of the binders. Therefore, W-EP/SS composite binder system has
excellent synthesizing properties and has the prospect for a wide
application.
CRediT authorship contribution statement
Wang Xi: Data curation, Writing - original draft. Weiqiang Liu:
Writing - review & editing. Ruijin Hu: Software, Validation. Yuxia Yin:
Software, Validation. Ming Yue: Writing - review & editing.
8 W. Xi et al. / Materials and Design 192 (2020) 108767
Fig. 11. SEM and EPMA image of W-EP/SS bonded magnet.
Declaration of competing interest
The authors declared that they have no conflicts of interest to this
work.
We declare that we do not have any commercial or associative inter-
est that represents a conflict of interest in connection with the work
submitted.
Acknowledgements
This work was supported by the National High-tech Research and
Development Program of China (2012AA063201), National Natural Sci-
ence Foundation of China (51001002, 51371002, 51331003), Interna-
tional S&T Cooperation Programme of China (2015DFG52020), the
2011 Cooperative Innovation Center of Beijing University of Technology,
Program of Top Disciplines Construction in Beijing under Grant
PXM2019_014204_500031.
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