Original manuscript, Proceedings of 20th International Workshop on

RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________

Development of Composite/Nanocomposite Magnets

George C. Hadjipanayis1, Alexander Gabay1, Melania Marinescu2 and Jinfang Liu2

1
Department of Physics and Astronomy, University of Delaware, Newark, DE, USA
2
Electron Energy Corporation, Landisville, PA, U.S.A.

The paper reviews the recent efforts to fabricate composite magnets with hard and soft magnetic
components or with two hard magnetic components. Within the more traditional "top-down" approach,
the composite magnets were produced from isotropic nanocrystalline precursors. Texture was developed
through a hot plastic deformation. The explored systems included the Nd(Pr)-Fe-B, Sm-Co and Sm-Fe-N
hard magnetic components. The other, "bottom-up" approach consists of the assembly, alignment and
consolidation of separate hard and soft particles. Anisotropic Sm-Co nanoparticles can be produced via
surfactant-assisted high-energy milling. A uniform distribution of soft phase can be achieved via coating
of the hard magnetic particles with chemically synthesized Fe nanoparticles.

Keywords: nanoparticles, nanocomposites, coating, surfactant-assisted milling, hot deformation.

Contact author: George C. Hadjipanayis, University of Delaware, 217 Sharp Lab, Newark, DE 19716,
U.S.A., Fax: 1-302-831-1637, Phone: 1-302-831-6289, E-mail: hadji@udel.edu.

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 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
1. Introduction
Traditional magnets with a single magnetic
phase have nearly reached the limits of their
maximum energy product, (BH)max.
Furthermore, the demand for a higher
temperature stability leads to a sacrifice of a
considerable fraction of the room-temperature
properties. In principle, these two issues can be
addressed by combining two different materials
with high magnetization and high coercivity or
two materials with a good room-temperature
performance and high thermal stability. The
concept of nanocomposite magnets with
exchange-coupled high-coercivity (hard) and
high-magnetization (soft) phases [1,2] promised
at least doubled values of (BH)max. The practical
realizations of this concept so far fell short of
the expectations, and the highest room-
temperature (BH)max remains that of the
traditionally sintered Nd-Fe-B. The reasons for
this underachievement are fairly well
understood. Firstly, it is difficult to obtain a
uniform nanostructure with the size of the soft
elements not exceeding the exchange length.
Secondly, it is even more difficult to have such
nanostructure with a crystallographically
oriented hard phase. Finally, when dealing with
the not-as-high-as-predicted coercivity of the
nanocomposite magnet, one has to bear in mind
the Brown’s paradox, which refers to the
discrepancy which exists between the theoretical
nucleation field and coercivity of the real hard
magnetic materials.
In this paper, we review our recent efforts to
fabricate composite magnets with superior
room-temperature (BH)max and with enhanced
temperature stability. Two approaches have been
used. In the more traditional "top-down"
approach, the hard-soft composite magnets were
produced from isotropic nanocrystalline
precursors susceptible to the development of
texture via hot plastic deformation. In the other
approach (we may call it the "bottom-up"),
single-crystalline hard and soft particles have to
be arranged, crystallographically oriented and
then consolidated. Even though we did not yet
obtain breakthrough magnetic properties, it may
be worth it to discuss the strong and weak sides
2
of either approach and to point out the specific
difficulties associated with them.
2. Hot-deformed composite magnets
2.1. Hard-soft magnets based on R2Fe14B
The R-Fe-B systems with R = Pr and Nd
offer (in addition the R2Fe14B compounds with
their excellent hard magnetic properties) the
possibility to align the easy magnetization
directions of the 2:14:1 nanocrystallites through
a thermomechanical process (hot plastic
deformation) [3]. The alignment, however,
normally occurs only in the alloys enriched with
R, because of the presence of the liquid R-rich
grain-boundary phase [4]. In 2006, we reported
[5] that the moderately R-lean R-Fe-B
nanocrystalline alloys with approximately 15%
soft magnetic phase became susceptible for the
thermomechanical treatment if a small amount
of copper was added, as it is shown in Fig. 1(a).
More recently, we found that small additions of
indium generated a low-melting-temperature
phase in the Sm-Co alloys [6]. According to the
differential thermal analysis (DTA), a similar
effect takes place in the Pr-lean Pr-Fe-In-B
alloy: the Pr11Fe82In1B6 ingot exhibits what
seems to be a melting temperature of a minor
phase at 930 oC (see Fig. 2). This solidus
temperature, however, is significantly higher
than the one associated with the "usual" Pr-rich
Fig. 1. Demagnetization curves of (a)
Pr11.25Fe77.75Co5B6 (1), Pr11.25Fe76.75Co5Cu1B6
(2) and (b) Pr11Fe82In1B6 hot-deformed
magnets made from melt-spun alloys. Curves
were measured parallel and perpendicularly to
the pressure direction.
 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________

Fig. 2. DTA (heating) curves of Pr15Fe78In1B6

(1) and Pr11Fe82In1B6 (2) ingots. The Curie
temperature TC and solidus temperatures Tm Fig. 3. BSE SEM micrograph of a hot-
are shown. deformed magnet made from
(Nd,Dy)14Fe79.5Ga0.5B6 melt-spun alloy
phase (for Pr15Fe78In1B6 also shown in Fig. 2 blended with 10% Fe49Co49V2 melt-spun alloy.
that temperature was 660 oC). After the melt- Arrows indicate the pressure direction. Inset
spun and consolidated Pr11Fe82In1B6 alloy was shows a hot-pressed precursor.
deformed at 950 oC, it showed only a moderate
degree of texture and an intrinsic coercivity Hc
of less than 2 kOe, Fig. 1(b).
According to recent studies [7,8], die-upset
magnets made from blends of nanocrystalline R-
rich R-Fe-B alloys and coarse Fe(Co) powders
exhibit a uniform demagnetization behavior and
increased values of remanence Mr and (BH)max
parallel to the pressure direction. Backscattered-
electron (BSE) scanning electron microscopy
(SEM) image shown in Fig. 3 presents a vivid
example of such composite made from ground
Nd10.5Dy3.5Fe79.5Ga0.5B6 melt-spun ribbons and
the Fe-Co melt-spun ribbons cut into pieces as Fig. 4. Demagnetization curves of (a) hot-
large as 1 mm × 2 mm in size. Deformation at deformed (Nd,Dy)14Fe79.5Ga0.5B6 magnet and
900 oC arranges the Fe-Co inclusions into fairly Fe49Co49V2 ribbons and (b) hot-deformed
uniform layers perpendicular to the pressure magnet made from (Nd,Dy)14Fe79.5Ga0.5B6
direction. Fig. 4(a) presents the separate blended with 10% Fe49Co49V2. Broken lines
demagnetization curves of the different show weighted average calculated for the
components: those of the hot-deformed curves (a).
Nd10.5Dy3.5Fe79.5Ga0.5B6 magnet and Fe-Co
ribbons. The weighted averaged of these The small increase in 4πMr and (BH)max due
separate curves (the weight ratio 90/10) plotted to the Fe-Co addition to the above (Nd,Dy)-Fe-
in Fig. 4(b) has, of course, a distinct kink at zero Ga-B magnets (from 10.7 kG and 27.3 MGOe to
field. The M(H) curve of the composite magnet, 11.5 kG and 28 MGOe, respectively) may seem
however, reveals a perfect magnetic coupling disappointing. In fact, no increase at all should
between the hard and soft components. Without be expected in composites coupled only
doubt, in such coarse mixtures the coupling can magnetostatically [9]. The magnetostatic
only be of magnetostatic origin. coupling in layered composites like the one
shown in Fig. 3 should rather be seen as

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 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
complementary to the exchange coupling, the Fig. 5(a)]. In a good agreement with the theory
way to relax the restrictions for the size of soft for magnetostatically coupled composites [9],
magnetic components. Unfortunately, the the Fe addition markedly increased the
magnetostatic interaction places high saturation magnetization, but not the remanence.
requirements for the coercivity of the hard While the reaction between the RCo5 and Fe
magnetic phase, which must be high enough to components must produce the Fe-rich (and
withstand the stray fields of the soft phase magnetically soft) R2(Co,Fe)17 phase, the
[9,10]. moderately hard Sm2Co17 phase forms at the
One underestimated problem with the die- boundaries of the Co inclusions in the
upset composites made from R-rich R-Fe-B SmCo5/Co composites, shown in Fig. 6. Such
alloys and Fe(Co) is that during the hot SmCo5/Sm2Co17/Co composite magnets exhibit
deformation the liquid R-rich phase readily an increased remanence [Fig. 5(b)], and they
reacts with the Fe(Co) phase changing both the may offer us at least two interesting
amount of the Fe(Co) phase and the average
composition of the R-Fe-B matrix [10]. When
the addition of 2 - 3 wt. % Fe (by deposition
through sputtering onto the hard particles)
reportedly increased 4πMr of the die-upset Nd-
Fe-B magnet from 13 to 15 kG [11], one should
attribute this not to the higher magnetization of
the Fe phase (3 wt.% Fe can add to the total
magnetization only about 0.25 kG) but rather to
changes in the Nd-Fe-B component.
The high reactivity of the R-rich phase also
makes it very susceptible to oxidation during
milling and, therefore, complicates refinement Fig. 5. Demagnetization curves of hot-
of the R-Fe-B component in the R-Fe-B / deformed magnets made from high-energy
Fe(Co) composites [10]. Though not critical for milled RCo5 powder blended with 10 wt. % of
the effective exchange coupling, the size of hard (a) 10 μm Fe powder (deformation at 800 oC)
magnetic elements ultimately determines the and (b) 30 μm Co powder (deformation at 950
o
volume ratio of the soft component. It is quite C). Inset is rendered from the BSE SEM
obvious that the present "(BH)max challenge" micrograph.
cannot be answered by a composite magnet with
only a few percent of a high-magnetization soft
phase.

2.2. Hard-soft magnets based on R-Co

Similarly to Nd-Fe-B, the RCo5
nanocrystalline alloys can develop texture
through hot plastic deformation [13-15]. The
RCo5/Co and RCo5/Fe anisotropic composite
magnets (R = Pr, Sm) were fabricated via
consolidation and deformation at 800 - 950 oC of
milled RCo5 alloys (the milling included a high-
energy step to assure a nanocrystalline structure Fig. 6. BSE SEM micrograph of hot-deformed
and a low-energy step to refine the powder) magnet made from high-energy milled SmCo5
blended with the Fe and Co powders. powder blended with 10% of 1.6 μm Co
The RCo5/Fe hot-deformed magnets featured powder. Arrows indicate the pressure
0.3 - 2.0 μm thick iron layers oriented direction.
perpendicularly to the pressure direction [see

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 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
opportunities. The microstructure of these
composites may be further optimized to take the
full advantage of the recently reported [16]
enhancement of the exchange coupling through
a graded interface. Moreover, if the emerging
2:17 phase follows the (partial) texture of the
parent 1:5 phase, the SmCo5/Co composites can
be developed into anisotropic Sm2Co17/SmCo5
magnets (the 2:17 phase itself is not susceptible
to the deformation-induced anisotropy [15]).

2.3. Hard-hard composite (hybrid) magnets

It has been recently suggested [17] that hot-
deformed composite magnets made from
blended R-Fe-B and R'-Co nanocrystalline
alloys may fill the gap in thermal stability
between the permanent magnets based on the R-
Fe-B and R'-Co systems. We would like to
emphasize that the results of combining these
dissimilar materials must be interpreted with
caution. Fig. 7 presents demagnetization curves
of the (Pr,Dy)-(Fe,Co)-B magnet and the
(Pr,Dy)-(Fe,Co)-B/(Pr,Sm)Co5 composite, both
deformed at 800 oC. One can see that the
favorable effect of the (Pr,Sm)Co5 addition is
more obvious at 25 oC than at 240 oC. This
seemingly puzzling result has a simple
explanation. According to the SEM observations
[Figs. 8(a,b)], the (Pr,Sm)Co5 phase rapidly
disappears during the hot pressing and hot
deformation processing. Its transformation starts
Fig. 7. Demagnetization curves of hot-
deformed magnets made from single
(Pr0.85Dy0.15)14Fe72Co7.5Ga0.5B6 melt-spun
alloy (1) and its blend with 10 wt. %
Pr0.75Sm0.25Co5 high-energy milled alloy.
Fig. 8. BSE SEM micrographs of (a) hot-
pressed and (b) hot-deformed blends of melt-
spun (Pr,Dy)14(Fe,Co)79.5Ga0.5B6 alloy with
10% high-energy milled Pr0.75Sm0.25Co5 alloy.
(C) hot-deformed blend of the same melt-spun
alloy with 10% high-energy milled Sm2Co17
alloy; also shown is Sm elemental map for
marked area. Arrows indicate the pressure
direction.
in the areas adjacent to the triple junctions
between the R-Fe-B particles, most likely due to
the abundant supply of the (liquid) R-rich phase.
By the end of the hot deformation, almost all the
added 1:5 phase transformed into the "R'-rich"
[in this case, R'(Co0.9Fe0.1)2] phase. Thus, the
major reason for the observed improvement of
magnetic properties was the increased amount of
the rare-earth-rich phases leading, in particular
to a better texture in hot-deformed magnet.
One would expect the Sm2Co17 addition,
which can accommodate any amount of Fe, to
be more resistant to the above transformation.
Indeed, in the (Pr,Dy)-(Fe,Co)-B/Sm2Co17
composite magnet deformed at the same 800 oC,
the 2:17 phase was found to be mostly intact
[Fig. 8(c)]. However, the Sm2Co17 addition did
not improve the magnetic properties of the
composite magnet: its own properties were not
high enough and it could not develop texture via
hot deformation [15] [in fact, as Fig. 8(c) shows,
the 2:17 phase was not even deformed].

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 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
3. Hard-soft magnets based on Sm2Fe17Nx
The Sm2Fe17Nx compound has a saturation
magnetization almost as high as Nd2Fe14B, but a
significantly higher Curie temperature and a
stronger magnetocrystalline anisotropy.
However, because it is less stable than the
mixture of SmN and Fe, the Sm2Fe17Nx can only
be obtained via nitrogenization of Sm2Fe17 and it
cannot be exposed to a temperatures greater than
600 oC. In reference [12], we pointed out that in
composite magnets made from Sm2Fe17Nx and a
soft magnetic phase, the latter may
simultaneously serve as a metal binder. The hot-
pressed Sm2Fe17Nx/Fe0.65Co0.35 composites
indeed showed considerably higher absolute and
relative densities.
We have found that certain Co-substituted Fe
nitrides may provide nitrogen for synthesis of
Sm2Fe17Nx in such composites during
consolidation. The thermal gravimetric (TG)
scans in Fig. 9 show that decomposition of the
Sm2.1Fe17N2.7 alloy starts at 600 oC (Sm2Fe17N≈3
releases 1/3 of its N atoms when it dissociates
into SmN and Fe), whereas the
(Fe0.65Co0.35)89N11 alloy releases N at 450 oC
(the Co-free Fe89N11 does this only at 670 oC).
Thus, in the Sm2Fe17/(Fe0.65Co0.35)89N11
composite, the N atoms released during
decomposition of (Fe0.65Co0.35)89N11 can
interstitially modify the Sm2Fe17 compound.
Fig. 10 shows the microstructures of the
Sm2Fe17Nx/Fe-Co composite obtained through
Fig. 9. TG (heating) scans for ground Sm-Fe-
N alloy and mechanically alloyed Fe-N and
Fe-Co-N powders.
6
Fig. 10. BSE SEM micrograph of Sm2Fe17Nx /
Fe65Co35 composite consolidated at 570 oC
from blended Sm2.1Fe17 and (Fe0.65Co0.35)89N11
powders. Location of nitrogen was found with
XRD and TMA.
the in situ nitrogenization. The more ductile Fe-
Co phase fills the space between the hard
Sm2Fe17Nx particles, resulting in a dramatic
increase of the density [12]. Of course, this
merely demonstrates the concept; a much finer
microstructure and a textured hard phase are
required for the development of advanced
permanent magnets.
4. Nano-assembled composite magnets
4.1. Coating hard magnetic particles with high-
magnetization nanoparticles
It is rather difficult to form thin continuous
layers of a soft magnetic phase by simply
blending the hard magnetic powders with the
much finer soft particles: distribution of the
smaller particles will be determined by the voids
between the larger particles. The natural solution
to this problem would be to form the desired
thin layers in advance, by coating the particles
while they are still separate. Different coating
techniques have been suggested for the
fabrication of nanocomposite magnets [11,18-
20]. We focus our efforts on coating the hard
magnetic particles with the Fe(B) nanoparticles
synthesized by chemical reduction of FeCl2 with
NaBH4 [20].
To perfect the coating technique we used the
model systems of Cu particles coated with the
Fe nanoparticles. Cu powders with particle sizes
ranging from 1 to 100 μm were immersed in the
reaction bath during the synthesis of Fe
 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
Fig. 11. BSE SEM micrographs of model hot-
pressed composites made from (a) coarse and
(b) fine Cu powders coated by Fe
nanoparticles. Also shown are Fe elemental
maps for marked areas.
nanoparticles. The best results were achieved
after the dried-up powder was additionally
agitated. The large Cu particles (~ 100 μm) were
uniformly coated by Fe nanoparticles after a few
minutes of the "low-energy" hand shaking, but
the high-energy agitation in a SPEX-8000 mixer
was necessary for the Cu particles of a few
microns. Fig. 11 shows the microstructures of
two model composites obtained by consolidation
of the Cu-core/Fe-shell powders at 500 oC.
Following the above procedure, the
Sm(Co0.757Fe0.1Cu0.11Zr0.033)7 sintered magnet
was finely milled and the powder was dispersed
in the FeCl2 solution prior to the reduction. As a
result, the Sm-Co particles were only partially
coated with Fe particles, Fig. 12(a). A followed
high-energy agitation for 1 h led to complete and
seemingly uniform coating, Fig. 12(c). These
Fe-coated Sm-Co particles were consolidated at
500 oC into a composite magnet with the
uniform submicron Fe layers, Fig. 12(c).
4.2. Anisotropic Sm-Co nanoparticles by
surfactant-assisted milling
The high-performance nano-assembled
composite magnets will require anisotropic hard
7
Fig. 12. Particles of milled Sm(Co,Fe,Cu,Zr)7
magnet (a) coated with Fe nanoparticles and
(b) additionally shaken with SPEX mixer. (C)
BSE SEM micrograph of composite magnet
made from the shaken core/shell powder.
magnetic particles not much greater than the
soft particles, with a size no more than few tens
of nanometers. At this moment, the surfactant-
assisted milling seems to be the only technique
capable for producing so small metallic
nanoparticles with the rare-earths [21,22]. The
very promising results have been obtained
recently at the University of Delaware [23]. The
homogenized Sm2(Co0.8Fe0.2)17 and SmCo5
alloys were subjected to a high-energy ball
milling in heptane with a small amount of oleic
acid. After several hours of milling the powders
preserved their crystal structure and were
anisotropic (Fig. 13). The high-resolution
transmission electron microscopy (TEM, Fig.
14) revealed a very narrow particle size
distribution with the average size of 5.5 nm.
Due to the uniform size, the particles were self-
assembled into a two-dimensional lattice.
Evolution of the particles coercivity with the
milling time (Fig. 15) resembles that for the
low-energy milling: the coercivity inversely
follows the particle size rather than going
through a maximum followed by amorphization.
The surfactant-milled anisotropic
nanoparticles may serve as a perfect hard
magnetic component in nano-assembled
composite magnets.
Acknowledgements
This work was supported by DOD, DARPA,
 Original manuscript, Proceedings of 20th International Workshop on
RARE EARTH PERMANENT MAGNETS AND THEIR APPLICATIONS, Sept. 8-10, 2008, Crete, Greece
__________________________________________________________________________________________________
ONR, DOE and NSF.
Fig. 13. XRD scans of Sm2(Co0.8Fe0.2)17 alloy
after homogenization (1), surfactant-assisted
high-energy ball milling for 4 h (2) and
additional orientation by magnetic field (3).
Fig. 14. Bright field TEM image of
Sm2(Co0.8Fe0.2)17 powder after 4 h of
surfactant-assisted high-energy ball milling.
8
Fig. 15. Coercivity of Sm2(Co0.8Fe0.2)17 and
SmCo5 powders vs. time of surfactant-assisted
high-energy ball milling.
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