Intermetallics 10 (2002) 317–321

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Structural and magnetic properties of Fe50Co50 system

M. Sorescua,*, A. Grabiasa,b
a
Duquesne University, Bayer School of Natural and Environmental Sciences, Physics Department,
Pittsburgh, PA 15282-0321, USA
b
Institute of Electronics Materials Technology, Wolczynska 133, 01-919 Warszawa, Poland

Received 1 September 2001; accepted 30 November 2001

Abstract
The Fe50Co50 alloys were prepared by mechanical alloying of the Fe and Co powders using a high-energy ball mill. The Fe50Co50
system was also obtained as a thin film by the pulsed laser deposition method. Both powder and thin film samples were character-
ized by X-ray diffraction and Mössbauer spectroscopy. The formation of the bcc-FeCo solid solution was investigated as a function
of milling time. Both Fe50Co50 systems reveal similar magnetic hyperfine fields of about 35 T. Typically, the powders have random
spin orientation, while the thin film shows an out-of-plane magnetic texture. # 2002 Elsevier Science Ltd. All rights reserved.
Keywords: A. Magnetic intermetallics; B. Magnetic properties; C. Mechanical alloying and milling; D. Microstructure; E. Spectroscopic methods

1. Introduction troscopy. The formation of the bcc solid solution is

It has been recognized that the mechanical alloying
technique can be successfully used for the preparation
of various metal–metal systems, including iron–cobalt
[1–5]. Mechanical alloying of the starting Fe100 xCox
powders leads to the formation of the bcc solid solution
for x up to about 70, while for higher cobalt content the
fcc structure is observed [1,5]. The formation of the
disordered crystalline solid solutions occurs due to the
interdiffusion of the elements induced by intensive ball
milling.
On the other hand, there is a growing interest in the
preparation of magnetic materials in thin film form,
including the FeCo system, which can be used as a
component of the sense layer in spin-valve read heads
[6]. Magnetic properties of Fe/Co multilayered systems
have also been investigated [7]. One of the advanced
methods for growing metallic thin films or multilayers is
pulsed laser deposition (PLD).
In the present work we obtained the Fe50Co50 alloy
by both mechanical alloying and PLD techniques.
Structural and magnetic properties of the FeCo systems
are studied by X-ray diffraction and Mössbauer spec-
* Corresponding author. Tel.: +1-412-396-4166; fax: +1-412-396-
4829.
E-mail address: sorescu@duq.edu (M. Sorescu).
0966-9795/02/$ - see front matter # 2002 Elsevier Science Ltd. All rights reserved.
PII: S0966-9795(02)00007-9
investigated as a function of milling time. The magnetic
hyperfine parameters of powder samples are compared
to those obtained for the thin film.
2. Experimental
Commercial Co and Fe powders with particle sizes of
1.6 and 10 mm, respectively, were milled using a vibra-
tory Spex 8000 mixer mill with steel vial and balls. The
Fe50Co50 composition was prepared. The high-energy
ball milling was performed in air for milling times up to
50 h. The FeCo thin film was obtained on a silicon
substrate by the pulsed laser deposition technique using
an Fe50Co50 commercial target. Lambda Physik pulsed
excimer laser with l=248 nm, pulse width of 8 ns and
repetition rate of 10 Hz was used for ablation.
Both powder and thin film samples were characterized
by X-ray diffraction and Mössbauer spectroscopy.
X-ray diffraction patterns were obtained with a Rigaku
powder diffractometer using CuKa radiation (l=1.5406
Å). Transmission Mössbauer measurements were per-
formed for powder samples, while for the thin film the
conversion electron Mössbauer technique (CEMS) was
used. All Mössbauer spectra were measured at room
temperature using a 25 mCi 57Co-in-Rh source and
analyzed with the NORMOS-SITE and-DIST pro-
grams.
318 M. Sorescu, A. Grabias / Intermetallics 10 (2002) 317–321

3. Results and discussion
3.1. Fe50Co50 powders
The X-ray diffraction patterns for the milled Fe50Co50
samples are shown in Fig. 1. After 2 h of milling, the
peaks originating from both elemental bcc-Fe and hex-
agonal Co powders are clearly seen in Fig. 1a. The pro-
gressive mixing of the starting elements due to the high-
energy ball milling can be observed with an increase of
the milling time. The peaks related to pure Co powder
vanish gradually (Fig. 1b and c) and disappear com-
pletely for milling times longer than 15 h. This indicates
the diffusion of Co into the bcc structure and the for-
mation of the disordered FeCo solid solution with the
bcc structure (Fig. 1d and e). At the same time, the
widths of the peaks related to the bcc phase increase
gradually with the milling time due to the decrease of
grain sizes and the formation of mechanical defects.
Transmission Mössbauer spectra of the selected
Fe50Co50 samples are shown in Fig. 2. All spectra were
fitted with two sextets: one with narrow lines and the
hyperfine field of about 33 T corresponding to the resi-
dual bcc-Fe particles, and the other with much broader
lines and larger hyperfine field representing the bcc-
FeCo phase formed due to ball milling of elemental

Fig. 1. X-ray diffraction patterns of the Fe50Co50 samples milled for different times.
 M. Sorescu, A. Grabias / Intermetallics 10 (2002) 317–321
powders. In Fig. 2 one can see a significant broadening
of the absorption lines with increasing milling time. This
is also an indication of the distribution of hyperfine
fields related to a random substitutional solid solution.
The hyperfine field of the bcc-FeCo sextet increases
from 33.60 T after 15 h of milling (Mössbauer spectrum
in Fig. 2a) to 36.46 T after 35 h of milling (Fig. 2c). The
latter value of the hyperfine field is similar to that
obtained for the disordered FeCo phase in the Fe50Co50
system prepared by mechanical alloying and determined
by the fitting of the Mössbauer spectra with three
Fig. 2. Mössbauer transmission spectra of the Fe50Co50 samples mil-
led for 15, 25 and 35 h.
319
sextets (one related to the remaining Fe and two corre-
sponding to the disordered FeCo phases) [3]. The
increase of the magnetic hyperfine field at iron nuclei in
Fe–Co alloys with the bcc structure as compared to
bulk Fe is well evidenced [2,5,8]. The intensity of the
starting bcc-Fe component decreases gradually with
increasing milling time. Its hyperfine field also increases
to 34.33 T after 35 h of milling (Fig. 2c), strongly sug-
gesting that this phase is not pure iron any more, but
there are some Co atoms soluted in the bcc structure.
The powders exposed for longer milling times can be
fitted using the hyperfine field distribution method [2].
Fig. 3 shows the Mössbauer spectrum recorded for the
sample collected after 35 h of milling fitted with this
method. The distribution of the hyperfine fields extrac-
ted from the spectrum consists of one well defined, nar-
row peak with the average value of 35.65 T. This means
that after 35 h of milling, a relatively homogeneous
solid solution was formed. The average hyperfine field
calculated for our sample is slightly larger than that
reported in literature for the Fe50Co50 prepared by
mechanical alloying [2,4,5]. This is probably due to a
small contribution of iron introduced into the processed
Fig. 3. Mössbauer spectrum of the Fe50Co50 sample milled for 35 h
fitted using the hyperfine field distribution method.
320 M. Sorescu, A. Grabias / Intermetallics 10 (2002) 317–321

FeCo mixture during the intensive ball milling. The
small increase of iron content in the parent Fe50Co50
powder results in a change in composition, which
increases the hyperfine field of the new, iron-rich bcc-
FeCo phase [2,5].
The formation of the bcc-FeCo phase can be followed
in Fig. 4, which presents the relative abundance of two
bcc phases determined by the relative areas of the two
relevant sextet components in Mössbauer spectra. The
constant increase of the relative content of the FeCo
solid solution with milling time is associated with a
similar decrease of the starting bcc-Fe phase. After 35 h
of milling, the iron content in the sample is about 11%,
however, it has to be mentioned that this component is
not the pure iron, but it is being transformed gradually
with increasing milling time into the bcc phase contain-
ing more and more Co atoms. This is confirmed by the
gradual increase of the hyperfine field of the bcc-Fe
component as compared to that of the bulk Fe, as well
as by the hyperfine field distribution fittings, which do
not show any separate peaks characteristic for the iron
particles.

Fig. 4. Relative content of the bcc phases present in the Fe50Co50 powder samples as function of the milling time.

Fig. 5. X-ray diffraction pattern of the Fe50Co50 thin film deposited on Si substrate.
 M. Sorescu, A. Grabias / Intermetallics 10 (2002) 317–321
Fig. 6. Conversion electron Mössbauer spectrum of the Fe50Co50 thin
film.
3.2. Fe50Co50 thin film
The X-ray diffraction pattern for the laser ablated
thin film from the Fe50Co50 target is shown in Fig. 5.
The narrow diffraction peaks corresponding to the
FeCo phase with bcc structure are indicated. Beside two
large peaks related to the Si substrate, there are some
small peaks which correspond to the FeO phase. The
X-ray diffraction pattern is good evidence that the bcc-
FeCo phase was obtained by the PLD method.
The conversion electron Mössbauer spectrum recor-
ded for the same thin film can be fitted using only one
sextet with the hyperfine field of 34.80 T (Mössbauer
spectrum in Fig. 6). This result is in perfect agreement
with the data obtained for the Fe50Co50 alloys prepared
by mechanical alloying [2,4,5]. The linewidths of the
sextet related to the bcc-FeCo in the thin film Möss-
bauer spectrum are, however, significantly narrower
than those observed in powders. Thus, the FeCo thin
film is more homogeneous than powder alloys from the
compositional point of view.
For thin samples it is possible to calculate from the
Mössbauer spectrum the average angle between the
magnetization axis and the direction of the incident
gamma ray, , from the following relationship: R21=
4sin2/3(1+cos2), where R21 is the ratio of the relative
areas of the second to the first lines of the Zeeman sex-
tet. In case of our thin film, the R21 parameter equals
0.58, indicating a tendency to the out-of-plane spin
orientation. The angle  calculated for the FeCo thin
film obtained by the PLD method is 51 , giving an angle
321
of 39 between the average magnetic moment orienta-
tion and the film plane. The dependence of the spin
orientation on the thickness of Fe60Co40 films obtained
by electron-gun deposition was studied by Mössbauer
spectroscopy in [9]. It was observed that spins preferred
in-plane orientation when the film thickness was well
below 100 nm, and then rotated perpendicularly to the
film plane as the thickness increased. The FeCo film
obtained in our experiment is about 100 nm thick. For
comparison, bulk FeCo alloys prepared by mechanical
alloying have typically a completely random spin orien-
tation.
4. Conclusions
The Fe50Co50 alloys were prepared by mechanical
alloying and in a thin film form by pulsed laser deposi-
tion. The bcc-FeCo solid solution was identified by both
X-ray diffraction and Mössbauer spectroscopy. The
hyperfine field of the bcc-FeCo phase is significantly
larger than that of bulk Fe and is about 35 T. The thin
film is chemically more homogeneous than powders,
which reveal a hyperfine field distribution. The magnetic
moment orientation of the thin film shows a tendency to
be out-of-plane, while powders posses a random spin
orientation.
Acknowledgements
This work was supported by the National Science
Foundation.
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