IEEE TRANSACTIONS ON MAGNETICS, VOL. 52, NO.

9, SEPTEMBER 2016 2101806

Effects of Ga Addition on the Formability of Main Phase and

Microstructure of Hot-Deformed Ce–Fe–B Magnets
Ren-Quan Wang, Xin Shen, Ying Liu, and Jun Li
School of Materials Science and Engineering, Sichuan University, Chengdu 610065, China

The powders of Ce29.82 Fe69.18 B1.0 (CeFeB) and Ce29.82 Fe68.65 Ga0.53 B1.0 (CeFeGaB) (wt%) were prepared by melt spinning.
Microstructure and phase composition of the prepared powders were characterized by X-ray diffraction (XRD) and Mössbauer
spectrometry. The results indicated that the as-spun ribbons comprised multi-phases, including CeFe17 , Ce-rich phase, α-Fe phase,
and continuous phase. The proportion of the main phase (Ce2 Fe14 B) in the CeFeGaB ribbons increased as a result of Ga addition.
Then, the bulk samples were produced by hot pressing at 700 °C followed by hot deformation (HD) at 800 °C with a height reduction
of 75%, and then investigated by field emission scanning electron microscope, high resolution transmission electron microscope, XRD,
and vibrating sample magnetometer. The investigation showed a strong crystallographic texture in the HD CeFeGaB magnet and a
weak magnetic anisotropy in the HD CeFeB magnet, which could be attributed to the Ga addition that modified the microstructure
of grain boundary and the distribution of the Ce–Ga-rich phase.
Index Terms— CeFeB, Ga addition, high-resolution transmission electron microscope (HRTEM), hot-deformed magnets,
microstructure.

I. I NTRODUCTION a strong crystallographic texture. In addition, the effects of Ga

D UE TO the extraordinary magnetic properties, materials
based on Nd2 Fe14 B are overwhelmingly favored in per-
manent magnet applications in which the rare earth elements
Nd and Dy are essentially critical to the high performance
of such permanent magnets [1]–[4]. However, the increasing
pressure on obtaining those diminishing rare earth resources
not only considerably elevated the cost of producing those
materials but also made it imperative to find a substitution for
Nd and Dy. Recently, cerium, as one of the most abundant rare
earth elements in nature, was found to be an ideal alternative
to Nd in Nd2 Fe14 B-based materials. Therefore, Ce2 Fe14 B has
gained growing interests from the researchers in past few
years [5]–[13].
Hot press (HP) and hot deformation (HD) had been proved
as an efficient method to produce fully dense anisotropic
NdFeB magnets, and has been used for the production
of these materials for many years [14]–[16]. Recently,
Pathak et al. [17]–[19] reported that the Ce, Co-doped
(Nd1-xCex)2Fe14-yCoyB compounds had excellent magnetic
properties both in bulk polycrystalline and rapidly solidified
nanostructured ribbon forms, which attracted considerable
interest on this method. To our knowledge, there is no study
about pure Ce–Fe–B magnets (Ce totally substituted Nd)
prepared by HP and HD, which has been reported so far.
In this paper, the pure CeFeB magnet and Ga added
CeFeGaB magnet were prepared by the above method. And,
it was found that the magnetic anisotropy was difficult to be
obtained for CeFeB sample even though the deformation ratio
was up to a height reduction of 75%. Nevertheless, with an
addition of 0.53 wt% Ga, the CeFeGaB magnet could obtain
Manuscript received September 10, 2015; revised December 2, 2015;
accepted May 10, 2016. Date of publication May 17, 2016; date of
current version August 17, 2016. Corresponding author: J. Li (e-mail:
abthonyli@163.com).
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/TMAG.2016.2569519
0018-9464 © 2016 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
addition on the ability of main phase forming as well as the
evolution of microstructure are studied in detail.
II. E XPERIMENTS
Alloys with the nominal composition of Ce29.82 Fe69.18
B1 (CeFeB) and Ce29.82 Fe68.65Ga0.53 B1 (CeFeGaB) (wt%)
were prepared by induction melting in argon atmosphere.
The ingots were broken into small pieces and melt spun
onto a molybdenum wheel from copper crucible at a surface
speed (Vs) of 28 m/s in argon atmosphere. This Vs corre-
sponds to a quench rate high enough to yield overquenched
as-spun ribbons, which are mostly amorphous or nanocrys-
talline. The ribbons were then crushed to under 100 mesh. The
isotropic bulk magnets were hot pressed in a tungsten carbide
mold of  15 mm for 2 min at the temperature of 700 °C and
a pressure ranged from 150 to 180 MPa. Then, still in vacuum,
with a height reduction of 75% and a strain rate of 10−2 s−1 ,
the anisotropic magnets were hot deformed at the temperature
of 800 °C and a pressure from 60 to 80 MPa.
The X-ray diffraction (XRD) information of both the
as-spun ribbons and the magnets was obtained on a
Fangyuan DX-2700 X-ray diffractometer with Cu Kα radiation
(λ = 1.5406 Å). For the further identification of the
phase composition of the as-spun ribbons, room tempera-
ture transmission Mössbauer spectrometry (MS) was con-
ducted with a 57 Co/Pd source. The morphology and the grain
size information of the as-spun ribbons were characterized
by the transmission electron microscope (TEM; JEL-2100).
In order to determine the HP temperature, differential thermal
analysis (DTA) was carried out on an SDTQ600 thermal
analyzer in ultra-highly pure Ar flow at a heating rate
of 10 K/min.
The cross-sectional morphology of the magnets was char-
acterized by a field emission scanning electron microscope
(Inspect F). And the further details about the magnets, such
as precipitates distribution and crystallographic information,
were investigated by a high-resolution TEM (HRTEM;
2101806
TABLE I
M ÖSSBAUER S PECTRA PARAMETERS OF THE CeFeB AND CeFeGaB A LLOYS
Fig. 1. XRD patterns of the melt-spun powders. (a) CeFeB. (b) CeFeGaB.
JEL-2100 and TECNAI F20) equipped with an EDX spectrom-
eter. The magnetic properties of the magnets were determined
by a vibrating sample magnetometer (LakeShore 7410) with
samples cut both parallel and perpendicular to the pressing
direction. The TEM samples were prepared by mixing the
Nd–Fe–B powders (30% in volume) with pure aluminum
powders, followed by blending, compacting into pellets,
rolling into flakes, punching, grinding, and ion-sputter
thinning [20].
III. R ESULTS AND D ISCUSSION
A. Melt-Quenching Ribbons
The phases of melt-quenching ribbons were examined by
XRD and MS. It could roughly determine the constituent
of melt-quenching powders by the XRD patterns in Fig. 1.
IEEE TRANSACTIONS ON MAGNETICS, VOL. 52, NO. 9, SEPTEMBER 2016
It can be seen that the magnetic hard phase Ce2 Fe14 B was
the dominant phase in the CeFeGaB alloy sample pattern, as
shown in Fig. 1(b), while it was not obvious in the CeFeB
alloy sample pattern shown in Fig. 1(a). Moreover, there were
some second phases coexisted (eg., Ce2 Fe17 phase) in both
two alloy samples. Further examinations by using Mössbauer
spectroscopy identified the phase composition in detail; the
volume percentage of each phase is shown in Fig. 2 and
listed in Table I. From the Mössbauer spectroscopy results,
it could be seen that, in the sample of CeFeB, the magnetic
hard phase Ce2 Fe14 B accounted for only 23.2% while the
continuous phase accounted for more than a half, 53.1%. Here,
the continuous phase is a mixture phase comprising a few
amorphous phases and some other Ce, Fe containing phases.
Because of the overlapping of the spectra, it was difficult to
distinguish those minor phases in continuous phase.
However, as a result of adding Ga to obtain CeFeGaB
alloy, the content of the magnetic hard phase Ce2 Fe14 B
increased to 56.3%, which was more than doubled compared
with the pure CeFeB, while the content of the continuous
phase decreased to 29.4%. It was noted in some previous
studies [21], [22] that the partial substitution of Ga atoms with
Fe atoms could lead to the swelling of crystal lattice, which
could make the crystal structure of Ce2 Fe14 B more stable.
As a consequence of making the structure of Ce2 Fe14 B more
stable by adding certain amount of Ga, the CeFeGaB contained
more of this magnetic hard phase than the CeFeB. Besides,
the Ce-rich phase and α-Fe phase were also detected in both
alloy samples. A similar result with various Ce contents of
Ce–Fe–B ternary ribbons was found in [23].
The bright-field (BF) TEM micrographs of melt-quenching
ribbons were shown in Fig. 3. The results show that the
grains of either ribbons’ sample are both in polygonal shape.
Compared with that of the pure CeFeB alloy, the grain size is
WANG et al.: EFFECTS OF Ga ADDITION ON THE FORMABILITY OF MAIN PHASE AND MICROSTRUCTURE 2101806

Fig. 2. Mössbauer spectra of (a) CeFeB and (b) CeFeGaB alloys.

Fig. 3. TEM micrographs of melt-quenching ribbons. (a) CeFeB.

(b) CeFeGaB.

much finer in the modified microstructure of the Ga containing

alloys. The powder particles of the Ga-free sample with a mean
grain size of about 100 nm could be clearly seen in Fig. 3(a).
However, fine and uniform particles of the CeFeGaB sample
with an average grain size of ∼40 nm could be seen in
Fig. 3(b). Thus, it could be concluded that the addition of Fig. 4. DTA curves of the CeFeB and CeFeGaB melt-spun powders.
a small amount of Ga to the ternary alloy is an effective way
to reduce the grain size of the magnets. In addition, according
to the literature [24], small grain size would be advantageous
for the deformation process.
B. Hot-Deformed Magnets
DTA measurements investigation gave information about the
melting point of the intergranular phase, which was observed
as an endothermic reaction. The melting temperature of the
grain boundary phase in the CeFeGaB and CeFeB alloys was
determined to be T = 953 K and T = 960 K (Fig. 4),
respectively. Therefore, the HP process temperature was set
as 973 K. The other two peaks at 738 K (or 724 K) and
1337 K (or 1335 K) are corresponding to the amorphous
transformation temperature and the melting point of Ce2 Fe14 B
in CeFeB and CeFeGaB samples, respectively.
Fig. 5(a) and (b) shows the cross-sectional morphology of
CeFeB and CeFeGaB HP magnets, respectively. Both of the
samples show the morphology of uniform distributed particles
of about 50–100 nm in diameter. Fig. 5(c) and (d) shows
Fig. 5. SEM micrographs of the fractured surface of HP and HD magnets.
the microstructure of the HD samples prepared from the (a) HP and (c) HD of CeFeB. (b) HP and (d) HD of CeFeGaB.
hot-pressed compacts. As can be seen, the cross-sectional
morphology of the HD CeFeB magnet sample is significantly equiaxed shape, instead the grains are in elongated shape.
different from that of the HD CeFeGaB magnet sample. The long axis of the elongated grain is perpendicular to the
It appears that the grains in CeFeGaB are no longer in compression direction [Fig. 5(d)]. On the contrary, it is noted
2101806
Fig. 6. XRD patterns of the HD magnets. (a) CeFeB. (b) CeFeGaB.
Fig. 7. Bright Field (BF) TEM images of the hot-deformed magnets of
CeFeB, (a) the morphology of deformed CeFeB magnets; (b), (c) and (d) the
distribution of the precipitates.
that the grains in CeFeB are still in an equiaxed polyhedron
shape and the grains’ size grow up to ∼2 μm [Fig. 5(c)].
Furthermore, there are many fine precipitates dispersed on the
surface of the large grains or surround them. This observation
indicates that the texture development during the HD may be
blocked by those precipitates. A further analysis was measured
by XRD and the results shown in Fig. 6(a) indicate that the
fine precipitates are α-Fe, CeFe2 , and Ce2 Fe17 . They all have
a high melting point [25] and play a role of a barrier during the
deformation process. Moreover, XRD studies were performed
in order to examine the crystallographic alignment of the
Ce2 Fe14 B grains in the HD magnets. Fig. 6 shows the XRD
patterns of the hot-deformed magnets, including: 1) CeFeB
magnet and 2) CeFeGaB magnet. The XRD pattern of the
pressed surface of the HD magnets shows the obvious c-axis
alignment of the CeFeGaB magnet, which is characterized by
the prominent (004) and (006) peaks [Fig. 6(b)]. However,
a weak crystallographic alignment is observed in the CeFeB
magnets, which is consistent with the SEM results.
Fig. 7 shows the BF TEM images of the hot-deformed
CeFeB magnet. It can be seen that after HD, the major phase
IEEE TRANSACTIONS ON MAGNETICS, VOL. 52, NO. 9, SEPTEMBER 2016
Fig. 8. HRTEM images corresponding to the regions marked by letters in
Fig. 7. (c) Inset of inverse fast Fourier transform indicates a lattice fringe
image and (f) selected area diffraction patterns of the GBP in (e).
Ce2 Fe14 B grains, with an average grain size of 300 nm,
remained the polygonal shape. As shown in Fig. 7(a) and (d),
there are some extremely fine precipitates located on the grain
boundary of some well-developed Ce2 Fe14 B grains, or inside
them. Some researchers mentioned that those Ce, Fe con-
taining continuous phases were metastable transition phases,
which would be easily decomposed at an elevated tempera-
ture [24], [25]. Therefore, it was assumed that these extremely
fine particles were precipitated during the HD process at
elevated temperature from the Ce, Fe containing continuous
phases. The continuous phases are metastable state and they
would decompose CeFe2 and a-Fe phase under a high temper-
ature, which could inhibit the formation of the c-axis texture
during HD. The precipitates marked by letters in Fig. 7 will
be further examined by the HRTEM.
As shown in Fig. 8, the HRTEM images are corresponding
to the phases marked by different letters in Fig. 7. Fig. 8(a)
indicates that the well-developed grains in Fig. 7 are the main
phase of Ce2 Fe14 B. Moreover, the precipitates lettered by
B–D are the Fe2 B, Ce-rich phase, and CeFe2 , respectively.
Especially, a wide grain boundary (lettered E) about 50 nm
is shown in Fig. 7(d). A further analysis by the HRTEM
[Fig. 8(e)] and selected area electron diffraction [Fig. 8(f)]
shows that it mainly consisted of a-Fe. Those results are well
in agreement with the XRD analysis. And these dispersed
extremely fine precipitates contributed most to the retardation
of the deformation of the CeFeB alloy, which was assumed to
be the reason that the CeFeB magnet was difficult to attain a
texture.
Fig. 9 shows the HRTEM images of hot-deformed
CeFeGaB magnet. The platelet shape grains were observed
in Fig. 9(a). Ultra-thin (about 1.4 nm) Ce-rich amorphous
layers were observed on the interface of elongated grains
WANG et al.: EFFECTS OF Ga ADDITION ON THE FORMABILITY OF MAIN PHASE AND MICROSTRUCTURE
Fig. 9. HRTEM images of the hot-deformed magnets of CeFeGaB and
EDX spectra showing the existence of intergranular Ce-Ga-rich phase, (a) the
morphology of deformed CeFeGaB magnets; (b) a Ce-rich phase in grain
boundary; (c) and (e) the HRREM images of Ce-oxide; (d) a step-like grain
boundary and (f) a straight thin grain boundary about 1.4 nm; (g) and (h) the
EDX results of the phase in grain boundary.
in the CeFeGaB magnet [see Fig. 9(f)]. Previous studies
revealed that these Ce–Ga-rich phase magnetically insulated
the grains and promoted the texture development, and believed
that these Ce, Ga rich phases should be responsible for the dra-
matic difference in microstructure between Ga added and free
Ga samples [27]–[29]. The intergranular phase was investi-
gated by EDX, as shown in Fig. 9(g) and (h). The result
confirmed the assumption that Ga is responsible for the
improvement of hot workability in CeFeGaB magnets in
comparison to the ternary alloy of CeFeB. Furthermore,
Fig. 9(d) shows a large step of 5 nm and the two Ce2 Fe14 B
grains are in direct contact with this particular boundary, and
some Ce-oxide phases were found in the trigonal grains in
Fig. 9(c) and (e). It consumed a lot of Ce-rich phases and
resulted in the deficiency of Ce-rich between the main phases.
The magnetic properties of the hot-deformed samples were
measured both parallel and perpendicular to the pressing direc-
tion, and the results were shown in Fig. 10. From Fig. 10(b),
it can be seen that the remanence Br of the c-axis parallel
direction (6.8 T // c-axis) of CeFeGaB magnet is much higher
than that of the c-axis perpendicular direction (2.8 T ⊥ c-axis),
indicating a strong crystallographic texture [Fig. 10(b)]. This
could be assigned to the formation of the deformation texture
caused by HD process in which the magnetization easy axis
aligned parallel with the pressing direction. And the conclusion
deduced from the hysteresis loops of the CeFeGaB magnet
2101806
Fig. 10. Hysteresis loops of hot-deformed (a) CeFeB and (b) CeFeGaB
magnets.
is well consistent with the analysis of XRD patterns as well
as the observation of micrographs. However, a weak c-axis
alignment can be observed in the hysteresis loops of the CeFeB
magnet, as shown in Fig. 10(a), for the Br difference between
the two directions is fairly small, 3.7 and 2.9 T parallel and
perpendicular to the c-axis direction, respectively. The poor
magnetically anisotropy of the CeFeB magnet could be mainly
contributed by the irregularity of microstructure and phase
composition. Due to the relatively large grain size in both
magnet samples, the coercivity (Hci) parallel to the c-axis is
very low, only 635 and 600 A/m in CeFeB and CeFeGaB
magnets, respectively.
IV. C ONCLUSION
This paper focused on the effects of gallium addition on the
hot-deformed CeFeB magnet. In order to cover all the detailed
information during the whole preparation of magnet, two melt-
spinning alloy ribbons had been designed and made prior to
the ultimate magnets that were compacted by HP and HD.
The XRD, MS, DTA, SEM, TEM, and the study of magnetic
properties were successively applied in the whole progress to
reveal that the influences of Ga addition existed throughout
the process, from the as-spun ribbons to the ultimate magnets.
Based on the experimental and analytical results, the following
conclusions can be drawn.
During the preparation of the melt-spinning ribbons, the
formation of the main phase, Ce2 Fe14 B, could be facilitated
by a small amount of Ga addition (0.53 wt%), which led the
content of the main phase in Ga added sample increase by
33.1%–56.3% compared with the Ga free sample. Beyond that,
the addition of Ga also caused an obvious grain refinement
in CeFeGaB ribbon sample according to the TEM micro-
graphs. The average grain size of the CeFeGaB ribbon sample
decreased to about 40 nm from about 100 nm of the CeFeB
ribbon sample. Either more main phase or finer grain size
would benefit the following process.
During the preparation of the ultimate products, the mag-
netically anisotropy of the magnets was highly dependent on
the Ga addition. The pure CeFeB magnet could hardly obtain
magnetically anisotropy even when the deformation degree
reached 75% in height reduction. While with the addition
of 0.53 wt% Ga, the CeFeGaB magnet could attain fairly
good texture with the same process condition. Moreover, the
CeFeGaB magnet had a much superior magnetic performance
to its free Ga counterpart. These dramatic differences between
the Ga added and the free Ga CeFeB magnet could be ascribed
to the following three reasons: 1) the formation of the texture
2101806
in the pure CeFeB magnet was impeded by those extremely
fine dispersed precipitates that precipitated from 53.1% of
the continuous phase in the pure CeFeB magnet; 2) the
formation of the texture in the CeFeGaB magnet was benefited
from the ultra-thin platelet Ce–Ga-rich phases, which mainly
located on the grain boundary of the main phase; and 3) the
superior magnetic properties of the CeFeGaB magnet could be
attributed to the increased quantity of main phase, Ce2 Fe14 B,
with the addition of 0.53 wt% Ga.
Finally, the addition of 0.53 wt% Ga into the CeFeB could
cause a prominent improvement on the magnetic properties of
CeFeGaB magnet, (BH)max = 2.2 MGOe, Br = 0.68 T, and
Hci = 600 A/m.
ACKNOWLEDGMENT
This work was supported in part by the National Natural
Science Foundation of China under Grant 51171122 and in
part by the Sichuan Province Science and Technology Support
Program under Grant 2013GZX0164, Grant 2013GZ0056, and
Grant 2014GZ0090.
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