IEEE TRANSACTIONS ON MAGNETICS, VOL. 26, NO.
5, SEPTEMBER 1990
GRAIN S I Z E DEPENDENCE OF COERCIVITY AND PERMEABILITY
IN NANOCRYSTALLINE FERROMAGNETS
Vacuumschmelze GmbH, D-6450 Hanau, Fed. Rep. Germany
Abstract - Amorphous ribbons of composition
Fe74 5-xCuxNb3Si13 gBg (x=O,l at%) have been
annealed between about SOO'C and 9OO'C. This
produced a series of crystallized samples with
grain sizes between about lOnm and 300nm and
with coercivities HC and initial permeabilities
pi varying over several orders of magnitude.
The best soft magnetic properties (Hc=O.OIA/cm
and pi=80x103) were observed for the smallest
grain sizes of about 1 Onm. With increasing grain
size D coercivity steeply increases following
a D6-power law (up to DsSOnm). Hc then runs
through a maximum of Hc=30A/cm and decreases
again for grain sizes above 15Onm according to
the well-known l/D-law for poly-crystalline
magnets. The initial permeability was found to
vary in a similar manner, essentially being
inversely proportional to coercivity. The
variation of the soft magnetic properties with
the average grain size is discussed and compared
with the predictions of the random anisotropy
model and other theories for the magnetization
reversal-
INTRODUCTION
Recently Yoshizawa et al. [ l ] reported on new
ferromagnetic Fe-base alloys with ultrafine
grain structure, revealing excellent soft
magnetic properties. A typical example is
Fe73.5CUlNb3Si13.5Bg,(at%). Thematerial is cast
as an amorphous ribbon. A subsequent heat
treatment above the crystallization temperature
produces a homogeneous, ultrafine grain
structureof a - F e S i w i t h a t y p i c a l g r a i n d i a m e t e r
of D-lOnm. The formation of this nanocrystalline
structure is ascribed to the addition of Cu and
Nb 111.
The good soft magnetic properties of the new
material can only partially be understood by
the decrease of saturation magnetostriction to
near-zero being observed after crystallization
[ 1 1 . The combination of small grain size and
good soft magnetic behaviour seems to be at odd
with the classical rule of soft magnetic
engineering which states that soft magnetic
properties of poly-crystalline
deterioratewithdecreasing grain size (cf.[2]).
But, as a matter of fact, this rule only applies
as long as the grain diameter is larger than
the ferromagnetic exchange length. Otherwise
the magneto-crystalline anisotropy K1 of the
grains is suppressed due to the smoothing part
of ferromagnetic exchange interaction. This
mechanism seems to provide the basis for the
soft magnetic properties of the nanocrystalline
structure [3].
The situation resembles much the case of
amorphous alloys where it has become folklore
that atomic-scale local anisotropies are ran-
domly averaged out so that there would be no
anisotropy net-effect on the magnetization
process. The degree to which this mechanism is
effective has been successfully addressed by
Alben et al. (41 in terms of the so-called random
anisotropy model.
0018-9464/90/0900-1397$01.00'SI 1990 IEEE
1397
G. Herzer
We will adopt this model as well as the ones
for large scale poly-crystalline materials and
discuss their predictions with respect to the
new nanocrystalline material. In particular we
will focus on the grain size dependence of the
soft magnetic properties in crystallized
Fe74.~-~Cu~Nb3(SiB)22.5 for grain sizes from
about 10nm up to several 100 nm.
EXPERIMENTAL
Ribbons of Fe74.5-xC~xNb3Si13.5Bg(x=O, 1 at%)
and Fe73.5CuiNb3Si16.5B6 were prepared by
rapidly quenching from the melt in 15 mm width
and about 20 wm thickness. The material was then
crystallized by annealing for lh above its
crystallization temperature T,. In order to get
a series of samples with increasing crystallite
size the annealing temperature Ta was varied
from about 500°C up to 900°C.
Differential thermoanalysis (DTA) at 10 K/min
was used to characterize the crystallization
behaviour of the material. The structural
details after crystallization were studied by
transmission electron microscopy (TEM). Addi-
tional information about the constituent cry-
stalline phases and its volume fraction was
deduced from the temperature dependence of
saturation magnetization Js being measured in
a Faraday balance in a magnetic field of
H =6kA/cm.
The soft magnetic properties were measured at
room temperature on annealed toroidal wound
cores of 22mm outer and 16mm inner diameter.
Coercivity Hc was determined from the B-H-loops
recorded at about 0.1 Hz using an integrating
fluxmeter. The initial permeability Pi was
measured at 50 Hz with a driving field of
H=Hc/100.
RESULTS
Maanetic Proverties upon Annealinq
Fig.1 shows the coercivity HC of heat treated
magnets Fe74.5:xCuxNb3Si13.5Bg as a function of the
annealing temperature Ta. The behaviour of
initial permeability vi is given in Fig.2 and
reveals a similar behaviour being essentially
inversely proportional to Hc.
In the alloy without Cu coercivity increases
steeply with the onset of crystallization by
orders of magnitude and reaches a maximum of
more than 10A/cm at about 540'C. This is a rather
typical behaviour observed in many amorphous
alloys (cf.[5]). In comparison the crystallized
Cu-doped composition reveals a broad minimum of
H,=lOmA/cm within the same annealing window
between about 500'C and 560°C. Simultaneously
the initial permeability reaches a maximumvalue
of more than 80x1 03. A deterioration of the soft
magnetic properties is finally observed at about
6OO0C, i.e. at significantly higher annealing
temperatures than in the Cu-free alloy.
1398

100
E
p

1
.-C 1
U W
I
I I

,x
.-
>
.-
U
5
0.

0.0
J
1 ; 5 : ; ! : ; I ' eF ,

0 a 1 at% Cu
0
0.00 'm
500 600 700 800 900
Annealing Temperature To in OC

Fig. 1 C o e r c i v i t y H , a s a f u n c t i o n of t h e
a n n e a l i n g t e m p e r a t u r e T, .
The arrows i n d i- Fig. 3 TEM b r i g h t f i e l d m i c r o g r a p h s o f
Fe73.5CulNb3Si13,gBg annealed a t Ta=540' C
cate t h e o n s e t o f c r y s t a l l i z a t i o n d e t e r m i n e d
by DTA a t 10 K / m i n . ( u p p e r l e f t ) and 900°C (lower r i g h t ) ,
Fe73.5CulNb3Si16.5Bg a n n e a l e d a t 5 4 0 ' C ( u p p e r
r i g h t ) a n d Fe74 g N b 3 S i 1 3 5Bg ( T a = 5 3 0 " C , lower
l e f t ) showing v a r i o u s s t a g e s o f crystalli-
z a t i o n . A n n e a l i n g t i m e w a s l h i n each c a s e .

100000
x
x
-e
.
.- 10000- the a-FeSi grains. Annealing above 600°C sig-
D nificantly increases the average grain size of
0 the a-FeSi-particles (cf. lower left in Fig.3).
Q,

E
Q,
1000- \

+ \
\
At the same time we find the Curie temperature
to increase towards Tc=700"C which proposes a
decrease of the Si-content in the a-FeSi. The

a 100-
annealed l h at 1,
lo! ' '500' ' ' ' 550 ' ' '
Annealing Temperature T,
Pig. 2 I n i t i a l p e r m e a b i l i t y p i as a f u n c t i o n
o f the a n n e a l i n g t e m p e r a t u r e T,.
Microstructural Investiaations
Fig.3 shows some typical microstructures of
the crystallized material. The most striking
difference between the alloy compositions
without and with lat% Cu appears to be the
crystallite size after comparable heat treat-
ments in the lower temperature regime (cf. lower
left and upper part in Fig.3, respectively).
The constituent phase in the Cu-doped alloy
is a-FeSi [ 1,3,6]. The temperature dependence
of magnetization indicates its volume fraction
to be about 70-90% (cf.[3]) increasing with
annealing temperature. For annealing tempera-
tures Ta below about 580°C the crystalline
particles are embedded in a still amorphous
matrix [3] probably enriched with Nb, Cu and B
since these elements are known to be insoluble
in a-FeSi. The lattice parameter of 0.284 nm as
obtained by X-ray defraction [l] and the Curie
temperature of about Tc=600'C [3] suggest an
enhanced Si-content of about 20 at% (cf.[ 71 ) in
'
electron diffraction patterns further indicate
the formation of a second crystalline phase,
presumably FeNbB. This phase is also manifested
in a slight inflection of the temperature
' ' '
600 ' dependence of magnetization at around 420°C.
The situation is somewhat different in the
in OC Cu-free alloy. The thermomagnetic analysis
reveals a considerable amount of a-FeSi ( 5 0 - 8 0 % )
only in the very initial state of crystalli-
zation, i.e. in a small annealing window between
about 520'C and 540°C. Above Ta=540"C the
constituent phase changes to a FeB-compound,
presumably bct-FejB. This is indicated by the
X-ray diffraction patterns [1,6] as well as by
the thermomagnetic analysis which shows that
above Ta=540"C about 70-80% of the sample is
made up of a crystalline phase with a Curie
temperatureofTc=500"Cclosetothatofbct-Fe~B
(Tc=550'C, cf.18)). Yet there is still a small
amount ( 2 0 . 3 0 % ) of a second crystalline phase
with Tc=660"C corresponding to that of a-FeSi
with around 1 5 at% Si. The change in the con-
stituent phases from a-FeSi to FeB-compounds
runs along with a maximum in the average grain
size which first increases towards 540°C to
D-50-60nm and then decreases between about
Ta=540"C-600"C.The behaviour of coercivity
indicates that D finally increases again above
about Ta=600"C, although the development of
microstructure above Ta=600'C has still to be
investigated.
The different crystallization behaviour of the
alloys is also manifested in the DTA-traces.
While the Cu-free alloy shows a single crys-
tallization peak at TX(onset)=575"C, the
addition of Cu results in two peaks with
crystallization onsets at about 51 0°C and 660°C.
 1399

Obviously the Cu-addition promotes the THEORETICAL MODEL

nucleation of a-FeSi since Cu and Fe tend to
segregate. This is assumed to be the basic The magnetic properties of an assembly of small
mechanism [ 1 ] for the ultrafine grain structure grains depend strongly on the counterplay of
of a-FeSi obtained in a relatively wide anneal local magnetic anisotropy energy and ferro-
window between about 500’C and 560°C. magnetic exchange energy.
For large grains the magnetization can follow
cture the easy magneticdirectionsin the single grains
The correlation between the microstructural and domains can be formed within the grains.
and magnetic investigations is given in Fig.4, The magnetization process, thus, is determined
where Hc and pi have been plotted versus the by the magneto-crystallineanisotropy K1 of the
average grain size D. The most significant crystallites.
feature is the steep increase (decrease) of Hc For very small grains, however, ferromagnetic
(vi) by orders of magnitude for grain sizes exchange interaction more and more forces the
below about 50nm. Coercivity then runs through magnetic moments to align parallel, thus,
a maximum and tends to decrease again for grain impeding the magnetization to follow the easy
sizes of several 100 nm. Permeability varies directions of each individual grain. As a
accordingly. consequence the effective anisotropy for the
Fig.4 represents the central result of the magnetic behaviour is an average over several
present work. An interpretation of the grains and, thus, reduced in magnitude.
underlying physical mechanisms will be the The dividing line between these two cases is
subject of the following paragraph. given by the ferromagnetic exchange length
L:x = Jrn (1)
(A denotes the exchange stiffness) which is a

C 9
I
/.
I
I - - - - - -
*-*
-
basic parameter in domain wall theory (cf.[9])
representing a characteristic minimum scale over
which the magnetization can vary appreciably.
With the material parameters of a-Fe-20at%Si
(K1=8kJ/m3 [lo], A=lO-llJ/m [ll]) the exchange
length is estimated as Lex=35nm. This value
-- 100- ? roughly coincides with the grain size below that
U I we find a steep decrease of coercivity and a
I I F~74.5-x~uxNb3Si22.5-~ - corresponding increase of permeability (Fig.4).
,x 10-1-
.-
>
_- H without Cu. 9 at% B 1 G r a y o w Model)
U

0
10-2- +
0 0.0 1 at% Cu. 9 at% B
A& 1 at% Cu, 6 at% B
In order to interpret the behaviour of the
magnetic properties for very small grain sizes
0 we make use of the random anisotropy model
lo-’- I I . . . . I I * . . ’ originally proposed by Alben et al. [4] for
amorphous ferromagnets. The basic idea is
sketched in Pig. 5 and starts from an assembly
of ferromagnetically coupled grains of size D
with magneto-crystalline anisotropies K1
oriented at random.
The effective anisotropy affecting the mag-
netization process results from averaging over
the N= (Lex/D) grains within the volume V=Lex3
104- \
\
\
\
\
1 w- \

102-

lo’!- - - ,
10 50
-I ‘.‘I
100
I .’..
500 1000
*\, I-
Grain Size D in nm

Fig. 4 Coercivity He and initial permea-

bility p i as a function of the average grain
-_I
size D. The dashed lines sketch the
theoretically expected behaviour and show
the variation H,, l / p i a D6 below 4 0 nm and Fig. 5 Schematic representation of the random
H e , l/pi a l/D above 150 nm. anisotropy model. The arrows indicate the
randomly fluctuating magneto-crystalline
anisotropies.
1400
of the exchange length. For a finite number, N,
of grains there will always be some easiest
direction determined by statistical fluctu-
ations. As a consequence the resulting aniso-
tropy density <K> is determined by the mean
fluctuation amplitude of the anisotropy energy
of the N grains, i.e.
In turn the exchange length Lex now is related
self-consistently to the average anisotropy by
substituting <K> for K1 in eq. (l), i.e.
(3)
This renormalization of Lex results from the
counterplay of anisotropy and exchange energy:
as magneto-crystalline anisotropy is suppressed
by exchange interaction the scale on which
exchange interactions dominate expands at the
same time and ,thus, the local anisotropies are
averaged out even more effectively.
The combination of eqs.(2) and (3) finally
yields
which holds as long as the grain size D is
smaller than the exchange length Lex. It should
be noted that this result is essentially based
on statistical and scaling arguments and,
therefore, is not limited tothe case of uniaxial
anisotropies (as may be anticipated from Fig.5)
but also holds for cubic or other symmetries.
The most significant feature of the above
analysis i s the strong variatior, of < K > with
the sixth power D6 of the grain size. If
coercivity and initial permeability are related
to <K> using the results for coherent spin
rotation (cf.[12]) we find
Accordingly the sensitive grain size dependence
of <K> should be also reflected in the soft
magnetic properties.
Indeed our experimental data for HC and ki
both are compatible with the expected D6 -de-
pendence (dashed line in Fig.4) for grain sizes
below about 40 nm (=Lex). A fit of the
corresponding data points to eq. (5) using the
material parameters of a-Fe-20 at% Si yields
pc=0.13 for coercivity and p,+=O.5 for permea-
bility, respectively. These fitted pre-factors
match surprisingly well with the results of fine
particle theory which are pc=O.64 and pP=O.33
for cubic particles oriented at random
(cf.[ 121 ) .
It should be finally noted that the above
results for Hc and ki are not bound to the case
of coherent magnetization rotation. Indeed, the
same final result can be derived assuming domain
wall pinning as the prevailing magnetization
mechanism (see appendix).
L a m e Grains
If the grain size exceeds the exchange length
the effective anisotropy <K> for the magnet-
ization process is given by the magneto-crys-
talline anisotropy K1 itself.
For D=Le!, coercivity and permeability approach
their maximum or minimum value, respectively,
given by
K,
Hc = P , z (6a)
With the material parameters of a-FeSi and
pc=0.64 and p =.33 for cubic particles we
estimate Hc=35 #/cm and pi=70 which is close to
the experimentally observed extreme values.
Finally, if the grain size exceeds the domain
wall width, GB=~L,,=T(A/K~ ) ll2, the magnetiz-
ation process is determined by domain wall
pinning at the grain boundaries. For that case
theory predicts [13,14]
with pre-factors being typically pc=6 (3) and
pk=O.l(0.2) for 180'(90") -domain walls in an
assembiy of randomly oriented cubic particles.
This l/D-law for Hc and l/pi is well-known for
poly-crystalline Ni-Fe [2] or MnZn-ferrites
~ 5 1 .
Our experimental data of Hc and l/pi indeed
seem to match with this theoretic result for
grain sizes above about 150 nm (=4(A/K1)ll2).
A fit of the data points to a 1/D law (dashed
line in Fig. 4) gives pc=2.6 for coercivity and
pP=0.05 for permeability which is in the order
of the theoretically expected values.
DISCUSSION
Fig. 6 compares the coercivities of nano-
crystalline FeCuNbSiB with other soft magnetic
alloys. The extrapolation of the 1 /D-law of the
nanocrystalline alloys to the km-scale gives
coercivities in between those of poly-crys-
talline FeSi6.5wt% (161 and 50wt?.Ni-Fe[2]. This
can be understood from the similar magnitude of
magneto-crystalline anisotropy Ki which is
22kJ/m3 for FeSi6.5 [lo] and 0.8kJ/m3 for
50wt%Ni-Fe [2). In comparison the Hc-level of
permalloy is significantly lower due to the
nearlyvanishing magneto-crystalline anisotropy
(K1<10J/m3). Amorphous alloys are located on
the quite opposite site of the scale. Hereby we
have assumed that the characteristic length
scale (analogous to D) is about 0.5nm corre-
sponding to the atomic volume of nearest
neighbours.
As schematically indicated in Fig.6 the
decrease of Hc with grain size in practice is
limited to a lower bound due to more long-range
inhomogenieties. Relevant to this are, for
example, magnetoelastic and induced aniso-
tropies or surface roughness. The resulting

100, I I I I
I
--
:*
I
f tallite sizes of about 7nm and 20nm (no data
t are given in between these limits). This result
D6
I
I phenomenon from the studies of high coercive
I
i
I Good soft magnetic properties are also found
I
. - d
0.001 ! I I I I
1nm 1Crm
Grain Size D
Y (+) amorphous CO (Fe)-base
nanocrystalline Fe-Cu,,Nb,(SiB),
o Fe-Si 6.5 wtX
o 50 Ni-Fe
o Permalloy
Fig. 6 Grain size and coercivity H, for
various s o f t magnetic metallic alloys.
limitation for the soft magnetic properties is
obvious for amorphous metals and is also found
in the nano-crystallinematerial at small grain
'
sizes. As an example, .g
!
F 4 includes some data
for Hc and i~i as obtained when the sample is
slowly cooled after the isothermal treatment at
Ta. The higher coercivities and lower permea-
bilities in this case are due to induced
anisotropies during cooling. The effect is most
pronounced for the smallest grain sizes where
the induced anisotropy (typically 10- 20 J/m3)
exceeds the average structural anisotropy <K>
( = 5 J/m3 for D=lOnm) The problem has been . tostriction.
attacked theoretically by Alben et al. 1 4 1 who
found Hc to vary proportionally to D3 (instead
of D6) if Ku dominates over <K>.
The discussion so far aimed at the effect of
grain size. Comparing the Cu-free and the Cu-
dopedalloy composition itmust be still realized
that the two alloys reveal different constituent
crystalline phases after crystallization, i.e.
FeB-compounds and a-FeSi, respectively.
Actually the anisotropy constants K1 and K2 of
tetragonal crystalline Fe2B or Fe3B are in the
order of 100kJ/m3 (cf.[ 17,181) and, thus, one
order of magnitude higher than the one of a-FeSi.
However, K1 and K2 are negative at room tem-
perature and we rather deal with an easy c-plane
than with an easy direction. As a consequence
magnetization can be always easily reversed by
rotation within the easy plane. For an ideal
isotropic c-plane this would mean zero coer-
civity and infinite initial permeability. In
practice, however, the magnetization rotation
within the easy plane is certainly hindered by
a small amount of in-plane anisotropy K3. It is
suspected that this in-plane anisotropoy K3
lastly determines the magnetization reversal
and, that its magnitude is comparable to the
magneto-crystalline anisotropy of a-FeSi.
1401
I I I It is finally interesting to compare the
present work with other data for fine particles.
O'Handley et al. 1191 have made similar
observations in devitrified glassy CogqNbloBg.
They find a discontinuity in coercivity of more
than three orders of magnitude between crys-
is compatible with a D6-law. The decrease of Hc
atvery small particle sizes is also awell-known
materials(cf.(lO]).
in multilayered magnetic structures with layer
thicknesses on the nm-scale. Dirne et a1.1211,
for example, report an increase of permeability
I I I
I
and a corresponding decrease of coercivity in
1mm Fe/CoNbZr multilayers for Fe-layer thicknesses
D below about 50nm. However, the variation with
D in these lower dimensional structures is not
as pronounced as observed for the three-di-
mensional case. It rather corresponds to a
D2/3 -dependence which would be the prediction
of the random anisotropy model if generalized
to the one-dimensional case (for two dimensions
the result would be a DZ-dependence of Hc).
.. CONCLUSIONS
Nanocrystalline alloys offer an interesting
system to study magnetic interaction for the
case in which the structural correlation length
is comparable to the ferromagnetic exchange
length. The dramatic changes in coercivity and
permeability observed for very small grains can
be interpreted in terms of the smoothing part
of exchange interaction averaging out locally
fluctuating anisotropies so that there is only
a small anisotropy net-effect on the magnet-
izationprocess. Similar tothe caseof amorphous
alloys, this mechanism is the basis for the good
soft magnetic properties of the new nanocrys -
talline Fe-base alloys. In addition the high
silicon content of the constituenta-FeSi grains
leads to low or vanishing saturation magne-
There are only a few alloy systems which reveal
the combination of low anisotropy and low
magnetostriction: the Permalloys, Sendust,
Mn-Zn-Ferrites,the amorphous Co-based alloys
and, now, the nanocrystalline Fe-base alloys.
Among these the nanocrystalline alloys offer
the highest saturation polarizations of about
Js=1.2-1.3 T. This and further features like
low high frequency losses due to a high elec-
tricalresistivity, the possibility of tayloring
the shape of the hysteresis loop by magnetic
field annealing [22] as well as good thermal
stability make the nanocrystalline Fe-base
alloys a most promising candidate for soft
magnetic applications.
APPENDIX
Coercivity due to domain wall pinning basi-
cally results from spatial fluctuations of the
domain wall energy y ( 1 4 1 , i.e.
where L denotes the typical wavelength of the
effective anisotropy fluctuations.
1402

For large grains L corresponds to the average [ 1 1 ] K.Huller, "The Spin Wave Excitations and
grain size D and we readily end up with the the Temperature Dependence of the Magnetization
well-known 1 /D law of large scale poly-crys - in Iron, Cobalt Nickel and Their Alloys", J.
talline alloys. Magn. Magn. Mat., vo1.61, pp.347-358, 1986.
For grains smaller than the ferromagnetic [12] R.M.Bozorth, Ferromagnetism, Prince-
exchange length, Lex, eq.(Al) only makes sense ton,N.J.: D. Van Nostrand, ch. 18, pp.811-837,
if we look at it on the renormalized scale of 1951
Lex. Hence, the effective wavelength of ani- [ 131 A.Mager, "Uber den Einflup der Korngrope
s o t r o p y f l u c t u a t i o n s i s g i v e n n o w b y t h e exchan e
length itself. Similarly the wall energy (AK)
is rather determined by the effective anisotropy
y2 auf die Koerzitivkraft", Annalen der Physik,
vol. 1 1 , Heft 1 , 1952
<K> than by the magneto-crystalline anisotropy [14] , M. Kersten, "Zur Theorie der ferro-
K1 in that case. Putting the corresponding magnetischen Hysterese und der Anfangsper-
expressions (eqs.(3) and (4)) into eq. (Al) leads meabilitat", Z. Phys., vo1.44, pp. 63-77, 1943
to same functional form of coercivity as given [ 15] W.Kampczyk and E.R o p , Ferritkerne,
in eq. (5a) and as originally derived starting Berlin,Munchen: Siemens AG, ch.B2.3, pp.94-99,
from rotational processes. 1978
A corresponding argument for initial per- [16] K.I.Arai, H.Tsutsumitakae and K.Ohmori,
meability essentially follows the same line, "Grain Growth of Rapid Quenching High
starting e.g. from eq.(7b). Silicon-Iron Alloys, IEEE Trans.Magn.,
VOl.MAG-20, pp.1463-1465, 1984
ACKNOWLEDGEMENTS
(171 G.A.Jones and P.J.Grundy, "The Magnetic
The author is indebted to J. Nahm who performed Domain Structure of Partially Crystallized
the TEM investigations, to M. Stadtmuller for Amorphous Fe-B Alloys by Electron Microscopy",
her assistance in the magnetic measurements and J.Mag.Magn.Mat., vol. 23, pp.200-208,1981
to K.Emmerich and H.R. Hilzinger for stimulating (181 M. Takahashi and C.Oh Kim, "Temperature
discussions. Dependence oftheMagnetic Anisotropy inFe81B1g
Alloy", Japan J.Appl.Phys., vol. 16, pp.
2061-2062, 1977
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