Herzer Soft Magnets1
Herzer Soft Magnets1
Herzer Soft Magnets1
G. Herzer
Vacuumschmelze GmbH, D-6450 Hanau, Fed. Rep. Germany
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- electron diffraction patterns further indicate
the formation of a second crystalline phase,
annealed l h at 1, presumably FeNbB. This phase is also manifested
in a slight inflection of the temperature
lo! ' '500' ' ' ' 550 ' ' ' ' ' '
600 ' dependence of magnetization at around 420°C.
The situation is somewhat different in the
Annealing Temperature T, 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-
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 zation, i.e. in a small annealing window between
o f the a n n e a l i n g t e m p e r a t u r e T,. 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
Microstructural Investiaations above Ta=540"C about 70-80% of the sample is
made up of a crystalline phase with a Curie
Fig.3 shows some typical microstructures of temperatureofTc=500"Cclosetothatofbct-Fe~B
the crystallized material. The most striking (Tc=550'C, cf.18)). Yet there is still a small
difference between the alloy compositions amount ( 2 0 . 3 0 % ) of a second crystalline phase
without and with lat% Cu appears to be the with Tc=660"C corresponding to that of a-FeSi
crystallite size after comparable heat treat- with around 1 5 at% Si. The change in the con-
ments in the lower temperature regime (cf. lower stituent phases from a-FeSi to FeB-compounds
left and upper part in Fig.3, respectively). runs along with a maximum in the average grain
The constituent phase in the Cu-doped alloy size which first increases towards 540°C to
is a-FeSi [ 1,3,6]. The temperature dependence D-50-60nm and then decreases between about
of magnetization indicates its volume fraction Ta=540"C-600"C.The behaviour of coercivity
to be about 70-90% (cf.[3]) increasing with indicates that D finally increases again above
annealing temperature. For annealing tempera- about Ta=600"C, although the development of
tures Ta below about 580°C the crystalline microstructure above Ta=600'C has still to be
particles are embedded in a still amorphous investigated.
matrix [3] probably enriched with Nb, Cu and B The different crystallization behaviour of the
since these elements are known to be insoluble alloys is also manifested in the DTA-traces.
in a-FeSi. The lattice parameter of 0.284 nm as While the Cu-free alloy shows a single crys-
obtained by X-ray defraction [l] and the Curie tallization peak at TX(onset)=575"C, the
temperature of about Tc=600'C [3] suggest an addition of Cu results in two peaks with
enhanced Si-content of about 20 at% (cf.[ 71 ) in crystallization onsets at about 51 0°C and 660°C.
1399
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
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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