3472 JEEE TRANSACTIONSON MAGNETICS,VOL. 29, NO. 6.
NOVEMBER 1993
Pulse Annealing of FeSiB Amorphous Wires
S. Atalay, P.T. Squire and M.R.J.Gibbs
School of Physics, University of Bath, Bath BA2 7AY, UK
Abstmct The magnetic field dependence of
magnetization and Young's modulus of pubannealed
Fe,,,Si,,B,, are reported. Coercivity and anisotropy
energy density were measured as a function of annealing
current and the tensile stress applied during annealing. It
is shown that pulse annealing can remove the internal
stresses more effectively than furnace annealing.
Coercivity and anisotropy energy density fall by a few
percent for annealing currents up to 1 A. Currents
between 1 A and 1.5 A reduce both quantities by nearly
an order of magnitude. Higher annealing currents result
in sharp increases in the parameters , as crystallization
begins.
I. INTRODUCTION
It is well known that annealing of amorphous alloys can
remove the intemal stresses which are induced during the
solidification process. In previous work we have reported the
reduction of the intemal stresses in Fe,7,Si,,B,, wires by
current [l] and furnace [2] annealing. Interpretation of
elastic moduli data showed that neither treatment completely
removed the intemal stresses before the onset of
crystallization.
In contrast to fumace and steady current annealing, it has
been shown that pulsed current annealing, achieved by
passing a direct current through the sample for a short time,
can almost completely remove the intemal stresses in
Co-based amorphous ribbons [3] One of the advantages of
such a treatment is that it can achieve very high heating and
cooling rates. This allows the amorphous phase to be
retained at temperatures unavailable in conventional
treatments. In this paper we report a study of the reduction
of the intemal stresses in Fe-based amorphous wires by
pulsed current annealing. The effect of a tensile stress
applied during the annealing is also studied because this can
significantly modify the induced anisotropy.
We have shown [1,2] that measurements of Young's
modulus as a function of applied field can be used to test
various features of the domain structure in amorphous wires,
that are not accessible to direct study. It is shown in [4] that
for field annealed amorphous ribbons
--
E - 1
(1)
Es I+{hiEsF(O,H,o)lK) '
where E, is the saturation modulus, & is the saturation
magnetostriction, K is the anisotropy constant (proportional
Manusaipt received February 15,1993.
0018-9464/93$03.00Q 1993IEEE
to the anisotropy energy density EK), 8 is the easy axis
orientation to the axis of the applied field H and stress 0. F
is a function whose value varies between zero and 912. The
general features of the model are independent of sample
geometry and the detailed domain structure; therefore the
model can be used b interpret results for amorphous wires..
The nonnalised modulus ratio E/Es is shown in Fig. 1for
selected values of 0. Of particular significance are the
values of the ratio at H=O and the minimum, E-/Es. These
are determined mainly by 8 and the dimensionless ratio
p = A.: EslK . (2)
Equations (1) and (2), together with measurements of
coercivity and anisotropy energy, provide the basis for
discussing the effects of annealing.
DETAILS
11. EXPERIMENTAL
Fe,,,Si,,B,, wires with a diameter of 1 2 5 p were supplied
by the Unitika Corporation. Flash annealing was performed
as follows: An amorphous wire 10.6 cm long was clamped at
each end. A direct current pulse was passed through the
sample. The current was calculated from the voltage pulse
measured across a noninductive, zero-temperature-
coefficient resistor in series with the sample. Annealing was
done at currents ranging from 0 to about 1.5 A, and with
various tensile stresses applied. The pulse width was kept
constant at 100 ms. Further details are given in [5]. No
reliable method was available for determining the
temperature, so the pulse current has been used to specify the
annealing conditions.
1
a8 -
as -
1
0.4 i \ I
Fig. 1. Modulus ratios predicted by (l),(2) for various easy axis angles 9.
The value of fl is typicalof a well annealed Febased amorphous material.

1.5
1
I
-1.0
.......*
Fig. 2. M(H) loops of wires pulseannealed under 367 Mpa tensile stress
The magnetic field dependence of Young's modulus, E(H),
was measured by the vibrating reed method. The third mode
was excited, and the samples had a free length of 2.5 cm,
resulting in resonant frequencies in the range 1.5-2.5 kHz.
The M(H) loops were obtained using a dc digital system. The
coercivity H,was measured directly from the M(H) loops,
and the anisotropy energy density was estimated from the
area between the loops and the M axis.
111. RESULTS AND DISCUSSION
Fig. 2 shows the dc hysteresis loops of the pulse annealed
wires at currents between 0.5 A and 1.36 A. For this range
the Large Barkhausen Jump (LB J) characteristic of as-cast
wires [6] is observed, the increase in the remanence ratio
MJM, to almost one indicating the increase in core volume
as the stress in the outer shell is reduced. (At annealing
currents greater than 1.36 A the LBJ disappeared, consistent
with further reduction of intemal stress.)
Figs. 3 and 4 show that H, and % remain almost constant
until the annealing current reaches 1 A. Between 1.OA and
1.5 A both parameters drop sharply. Above 1.5 A both H,
and E, increase sharply, indicating that crystallization has
occurred. The application of tensile stress during annealing
affects H, more than E,. This is not altogether surprising ,
since it has been found that in amorphous ribbons H, is a
very sensitive indicator of intemal stress. For 0=367 MPa
the minimum Q was observed in the wire annealed at a
current of 1.36 A ; the value of 0.2 Alm is the lowest that
has been reported for Fe-based amorphous wires.
Fig. 5 shows the magnetic field dependence of Young's
modulus, normalised to the value E, at saturation, for wire
annealed without tension. As explained in the Introduction,
the ratio E-Es is determined mainly by 8 and K. For wires
annealed below 1.15 A this ratio is almost equal to that for
as-cast wire. This can be understood by the constancy of E,
(Fig. 4) and therefore of K below this current. It also
indicates that the easy axis distribution is not significantly
changed. Above 1.15 A K starts to decrease, so the ratio
E,@, increases; finally K increases again, as
crystallization sets in, leading to a rapid increase in E&E,
3473
0 a=367 MPa
0.0 0.5 1.o 1.5 2.0
I (A)
Fig. 3. Coercivity as a function of annealing current at zero and 367 MPa
tensile stress.
towards unity. The minimum ratio E-ES =0.4 ,
corresponding to the greatest modulus change, was obtained
for the wire annealed at 1.51 A. Although very low
anisotropy energies were obtained by this method of
annealing, the modulus changes were found to be less than
those in furnace-annealed wires [l]. This suggests that the
easy axis distribution following pulsed current annealing is
less favourable for a large AE effect Comparison of Figs. 1
and 5 indicates that for the optimum annealing current of
1.51 A the easy axes are at close to 45' to the wire axis,
whereas for optimum AE effect they should be near 90°.
The application of tensile stress during annealing has a
pronounced effect on the modulus ratios (Fig. 6). Under
these conditions plastic flow could be induced. For currents
below 1.36 A the permanent axial strain was no more than
1.5%. For higher currents this increased to as much as lo%,
with a corresponding decrease in diameter of 5%. This
deformation induces a mechanical anisotropy in the easy
axis direction, which tends to align the magnetic moments
along the wire axis. There is thus the possibility of an
interplay between opposing mechanisms for determining
the easy axis directions. The sensitivity of the resulting
behaviour to annealing conditions is evident in Fig. 6. For
an annealing current of 0.67 A the field dependence of EE,
is very like that of the low-current, zero-stress annealed
samples (Fig. 5). At 1.31A E,,,&, for the stress-annealed
" , i i 2
500
05 1.0 1.5
I (A)
Fig. 4. Anisotropy energy density as a function of annealing current at
zero and 367 MPa tensile stress
 3414
LLY
\ 0.6
W W
0.4 y 0 1=1.54 A
0.2 f I I I I I
0 0.5 1.0 1.5 2.0 2.5
H (kA/m)
Fig. 5. Normalised Young's modulus as a function of applied field for Wires
annealed at zero stress.
samples is close to its minimum value, and occurs at lower
H. This shows that the easy axis direction has been pulled to
near 45' . At the slightly higher current of 1.36 A there is
hardly any AE effect at all, in spite of the low anisotropy.
This can only be explained by assuming that the easy axis is
very close to the wire axis ( 8 4 9 , consistent with anisotropy
dominated by the mechanical component. At the higher
current of 1.54 A E-ES falls again, showing that 8 is
between 45' and 90° . This can be attributed to the now
stronger, competing effect of crystallization.
Such pronounced changes of anisotropy direction under the
combined influences of stress and current during the
annealing process show how delicate may be the balance
between the various competing sources of anisotropy. The
elastic modulus ratio is a sensitive indicator of these
changes; taken in conjunction with M(H) curves it can be
used to deduce important information about the anisotropy
magnitude and direction.
One of the main motives for this study was to inhibit
crystallization by using a short, high temperature anneal.
The evidence from X-ray data supports the assertion, based
here on the magnetic and magnetoelastic behaviour, that
significant crystallization does not occur below an annealing
current of 1.51 A . Comparison with the effect of fumace
annealing [2] c o n f i i s the success of the pulse annealing
method.
The results reported here are selected from a much more
extensive data set. In particular, the annealing current pulse
length and annealing stress were varied. The values chosen
for this report represent the best results that were obtained.
However, the trends reported could be reproduced under
different conditions, so we believe the main effects to be
reproducible.
IV.CONCLUSIONS
Pulsed current annealing is a convenient method of
improving the magnetic and magnetoelastic properties of
0.8
0 1=0.67 A
A 1=1.31 A
0 1=1.36 A
0 1=1.54 A
0.2
0 0.5 1.o 1.5 2.0 2.5
H (kA/m)
Fig. 6. Normalised Young's modulus as a function of applied field for
wires annealedunder 367 MPa of tensile stress.
amorphous wires. It can remove most of the casting stress,
and can reduce the anisotropy energy by an order of
magnitude. The simultaneous application of tensile stress
during annealing enables the coercivity to be decreased even
more, resulting in a value as low as 0.2 Nm. Its effect on the
elastic modulus is complicated by the competing effects of
mechanically induced anisotropy and crystallization.
ACKNOWLEDGEMENT
The authors thank Del Atkinson for helpful discussions, and
Mike Harriman for technical help.
REFERE"
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dependence of Young's modulus and shear modulus in Fe-based amorphous
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