Thin Solid Films 311 1997.

1522

Giant magnetoresistance in granular AgCo films irradiated by excimer

laser
S. Luby

a,)

, E. Majkova a , M. Spasova a , M. Jergel a , R. Senderak a , E. DAnna b,

A. Luches b, M. Martino b, M. Brunel c
a
b

Institute of Physics, Sloak Acad. Sci., Bratislaa 842 28, Sloak Republic
Department of Physics and INFM, Uniersity of Lecce, Lecce 73100, Italy
c
Laboratoire de Crystallographie CNRS, Grenoble, France
Received 5 March 1997; accepted 29 May 1997

Abstract
A series of Ag 100yx Co x films x varying from 10 to 30 at.%. were codeposited by two electron beam sources in UHV system at the
SirSiO 2 substrate temperature F 408C. The Ag 75 Co 25 films were thermally processed by rapid thermal annealing RTA. at 500, 750 and
10008C for 30 s and by excimer laser irradiation at the fluences F s 0.1, 0.15 and 0.2 J cmy2 and number of pulses n varying from 1 to
100. The samples were analyzed by X-ray diffraction XRD. and grazing incidence XRD GIXRD.. The electrical resistance R H . was
measured up to 50 kOe with magnetic field perpendicular or parallel to the film plane and with current in plane of the sample, mostly at
4.2 K and 300 K. With increasing Co content in the film, a different degree of fcc Ag and fcc Co separation in the as-deposited films was
found, and for x 30%, small fcc Co peaks appeared. With RTA, a pronounced phase separation and increasing grain size with
increasing annealing temperature was observed. On the contrary, after laser irradiation, more random and less equilibrium structures with
smaller grain size and even negative temperature coefficient of the resistance developed. The giant magnetoresistance GMR. of
Ag 75 Co 25 films is f 74% at 4.2 K and 11.3% at 300 K in the as-deposited state. The GMR at 4.2 K can be increased by XeCl irradiation
to 82% at the most severe irradiation conditions F s 0.2 J cmy2 , n s 10. and to 13.213.5% at 300 K at the applied fluences. The
increase of GMR is ascribed to the formation of more random structure with smaller grain size. q 1997 Elsevier Science S.A.
Keywords: Excimer laser; Giant magnetoresistance; Granular Ag-Co films

1. Introduction
Since the initial reports of Berkowitz et al. w1x and Xiao
et al. w2x on giant magnetoresistance GMR. in CuCo
magnetic granular systems, many investigations have been
performed in this field. The highest GMR effect of granular systems reported so far has AgCo 25% at RT. w3x.
Granular magnetic films are heterogeneous immiscible systems which consist of magnetic particles granules., in a
non-magnetic matrix e.g., Cu, Ag.. Granular films are
easily prepared by various deposition techniques like sputtering or electron beam deposition, and they are considered
for applications as magnetic sensors and read heads w4x.
A granular structure is obtained as a result of phase
separation. During the deposition quenching process. the
phase separation may be suppressed, especially when the
substrate is held at room or lower temperatures. Under

Corresponding author.

these conditions, even metastable phases may be obtained.

A complete phase separation is achieved by post deposition heat treatment w5x.
The GMR effect arises from spin-dependent scattering
of conduction electrons, either within the single domain
magnetic particle, or at their interfaces with the non-magnetic matrix. For high GMR, small particles are favourable
because of their larger surfacervolume ratio w69x. The
size of particles and their separation must be smaller than
the spin-dependent electron mean free path w5x.. The size,
shape and distribution of magnetic particles strongly affect
the GMR. Generally, these parameters are predominantly
influenced by the deposition process and the post deposition heat treatment, which completes the precipitation.
Sometimes the GMR tends to increase with the initial heat
treatment, i.e., particle growth. Subsequent growth decreases it again w10,11x. On the other hand, heat treatment
is not necessary if the structure of the film is optimized by
substrate temperature and other deposition conditions cf.
w12x.. Moreover, heat treatment decreases roughness at the

16

S. Luby et al.r Thin Solid Films 311 (1997) 1522

2. Experimental
The Ag 100yx Co x films 300 nm and 500 nm thick were
fabricated in a UHV apparatus with two e-beam sources
by coevaporation of Co and Ag onto the oxidized Si100.
substrates at room temperature. The thickness of thermal
SiO 2 was 300 nm. The vacuum prior to deposition was
1 = 10y7 Pa, and during the deposition, 1 = 10y6 Pa. The
substrates were heated to 5008C prior to deposition, and
during the deposition their temperature was F 408C.
The composition of Ag 100yx Co x layers was obtained by
setting the appropriate deposition rates of Co and Ag
elements prior to codeposition. The deposition rates of Co
and Ag were adjusted using the quartz crystal monitor, and
they were verified according to the measurements of the
thickness of the deposited Co and Ag layers by the hard
X-ray reflectivity and the times of deposition. Moreover,

Fig. 1. a. Temperature vs. time evolutions at the surface of Ag 300

nm.rSiO 2 300 nm.rSi and Co 300 nm.rSiO 2 300 nm.rSi samples
irradiated at various fluences F by one laser pulse. Tm : melting temperature. b. Depth of melting vs. time evolutions of Ag 300 nm.rSiO 2 300
nm.rSi sample irradiated at various fluences F by one laser pulse.

interfaces of magnetic particles, and this can also result in

an increase of GMR w13,14x.
Considering all these effects, the heat treatment of a
granular magnetic film should be intense enough to complete the phase separation, to optimize the particle size, to
decrease the roughness of the interfaces, and to ameliorate
the structure of the host matrix. From the other side, it
should be short enough to prevent very large growth of the
magnetic particles, which is most probably a result of the
diffusion-controlled process.
In this paper, we report the effect of pulsed excimer
laser irradiation of AgCo granular films. The advantage
of this type of heat treatment is the possibility to deposit
the required amount of heat energy into the volume of the
film without interaction with the substrate. In our previous
work, it was shown that new metastable phases were not
formed in the immiscible MoCu system under laser
melting and rapid solidification e.g., w15x.. As far as we
know, this type of heat treatment of systems with GMR
was not reported up to now.

Fig. 2. a. XRD spectra of as-deposited Ag 100yx Co x films 300 nm thick

with x s10, 15, 20 and 25 at.%. b. Detail showing the shifts of Ag
111. peak.

S. Luby et al.r Thin Solid Films 311 (1997) 1522

Table 1
The exact position of Ag 111. peak vs. Co content in as-deposited
Ag 100yx Co x films obtained by XRD and GIXRD
Co at.%.

Ag 111. 8.

10
15
20
23
25
27.4
30

38.52
38.69
38.70
38.67
38.61
38.59
38.54

the vapour composition and the deposition rates of Co and

Ag during the codeposition were controlled by the mass
spectrometer. The composition of as-deposited samples
was analyzed by inductively coupled plasma emission
spectroscopy ICP.. Samples with x between 10 and 30
at.% were prepared.
The samples were processed with a Lambda Physik
LPX 315i excimer XeCl laser with beam homogenizer in a
chamber evacuated down to 1 = 10y3 Pa. The laser fluences F were 0.1, 0.15 and 0.2 J cmy2 , the numbers of
pulses directed to the same irradiation spot were n s 1, 10,
20, 50 and 100. The pulse repetition rate was 10 Hz and
the pulse duration 30 ns. At F s 0.2 J cmy2 only n F 10
pulses were applied, since at n G 20 pulses, the samples
were damaged. For comparison, the samples were processed also using rapid thermal annealing RTA. at 500,
750 and 10008C for 30 s in a halogen lamp furnace
vacuum of 1 = 10y3 Pa.. The rise time of the temperature
was 12 s.
The samples were analyzed by X-ray diffraction XRD.
in the BraggBrentano symmetrical mode and at grazing
incidence GI.XRD with a position-sensitive detector. In
our experiments the standard Cu lamp, standard Fe lamp
and Cu rotation anode were used. With AgCo system
some problems could appear due to the large absorption
coefficient of Co and resulting fluorescence for Cu radiation. For standard Cu lamp, the graphite monochromator
was used in front of the detector to suppress the fluorescence of Co. According to our experience, the resolution
was not improved when Fe lamp was used instead of Cu.
The best results were obtained using the Cu rotation anode.
Here, the intensity of X-ray radiation was high enough,
and the Fe foil in front of the detector could be used to
improve the signal-to-noise ratio.
The electrical resistance R H . was measured as a
function of the applied magnetic field up to 50 kOe using a
standard 4-probe method with Ag contacts. Measurements
were performed in two geometries, magnetic field was
perpendicular H. or parallel 5. to the film plane. The
current was in the plane of the sample. The resistance was
measured at a variety of temperatures, mostly at room
temperature and 4.2 K.

17

3. Calculation of temperature evolution

Since the direct measurement of temperature of the
laser-irradiated films is complicated due to very fast heating and cooling rates w16x, numerical computations were
performed. The details could be found in Ref. w17x. Calculation of the evolution of temperature for AgCo codeposits is complicated because thermal and optical parameters of Co and Ag reflectivity, thermal conductivity, etc..
are very different. This fact precludes the possibility of
averaging the parameters according to the film composition. Therefore, as a first approximation, temperature and
depth of melting evolution under laser irradiation were
simulated only for Co 300 nm.rSiO 2 300 nm.rSi and
Ag 300 nm.rSiO 2 300 nm.rSi systems. Some results
are shown in Fig. 1a,b.

Fig. 3. a. GIXRD spectra of as-deposited Ag 100yx Co x films 500 nm

thick with x between 2330 at.%. b. Detail showing the shifts of Ag
111. peak.

18

S. Luby et al.r Thin Solid Films 311 (1997) 1522

The melting temperature of SiO 2 is 2000 K and the

reaction of the AgCo film with the substrate during
irradiation can be neglected.

4. Results and discussion

4.1. XRD r (GI) XRD

Fig. 4. a. The effect of RTA on XRD spectra of Ag 75 Co 25 films 300 nm

thick. a: as deposited; b: 5008Cr30 s; c: 7508Cr30 s; d: 10008Cr30 s.
b. Detail showing the shifts of Ag 111. peak.

From Fig. 1a it follows that at the highest fluence

F s 0.2 J cmy2 only Ag film melts Tm s 1235 K.. The
time of melting is 260 ns and the film melts up to the
substrate. At F s 0.15 J cmy2 , Ag melts only superficially
Fig. 1b.. Co film Tm s 1768 K. does not melt even under
the highest fluence. Nevertheless, we expect that the melting of the Ag matrix is sufficient to influence the granular
structure of the film.
The calculations are valid only for the first laser pulse.
The cooling time of the sample is f 1 ms w18x, which is 2
orders of magnitude shorter than the time interval between
two successive laser pulses at the repetition rate of 10 Hz.
Thus, the laser pulses on the sample are thermally independent, and the accumulation of the heat in the samples
submitted to multipulse irradiation is not expected. Multipulse irradiation can affect the temperature profile if the
first pulse changes the surface reflectivity of the film. This
usually happens when F is high enough to melt the
surface layer.

4.1.1. Effect of Co content

The XRD spectra of Ag 100yx Co x 300 nm thick for
x s 10, 15, 20 and 25 at.% are shown in Fig. 2a,b. For all
compositions, the well-developed fcc Ag phase with the
set of peaks 111., 200. and 222. was observed the
220. peak is overlapped by the dominant Si 400. reflection of the substrate.. There is no clear crystallographic
evidence of the presence of pure hcp or fcc Co, although,
as it will be shown later, the Ag and Co phases are
separated. This is a typical problem of AgCo granular
systems with lower Co F 50 at.%. content w13x. The
reason is in the relatively large difference in numbers of
electrons of Ag and Co atoms. Consequently, the signal
coming from Co atoms is much weaker than those from
Ag atoms. Moreover, the granules of transition metal TM.
in TMAg codeposits with TM concentration F 30 at.%
are only poorly crystallized w19x, and their typical dimensions are between 5 and 20 nm w13x. The effect of large
absorption of Co for Cu radiation is discussed in Section 2.
The second problem is that the fcc Co 111. and Ag
200. reflections overlap. For our Co concentration range,
the Co 111. and Ag 200. reflection appears as a shoulder
slightly increasing with increasing Co content. According
to our data, the Ag 111. peak shifts towards higher angles
for x s 1020 at.%. For x s 25 at.% the Ag 111. peak
starts to move back to lower angles. It should be noted that
according to the crystallographic data for CuK a radiation,
the position of Ag 111. peak is 2Q s 38.116, whereas our
spectra give the values G 38.5 Table 1..
This trend was investigated in detail by GIXRD on the
set of Ag 100yx Co x films 500 nm thick for x s 23, 25, 27.4
and 30 at.% Fig. 3a,b.. Here, the Ag 111., 200., 220.,
311. and 400. reflections were found. For the sample
with 30 at.% of Co also small fcc Co 220. and 222.
reflections appear. The Ag 111. peak shifts towards lower
angles for x G 23 at.% Table 1.. Summarizing the XRD

Table 2
The exact position of Ag 111. peak vs. RTA conditions for Ag 75 Co 25
film
Annealing

Ag 111. 8.

As-deposited
5008Cr30 s
7508Cr30 s
10008Cr30 s

38.61
38.48
38.26
38.26

S. Luby et al.r Thin Solid Films 311 (1997) 1522

19

temperature is observed. After annealing at 10008Cr30 s

the fcc Co 200. and 311. reflections were identified.
With increasing temperature the shift of the Ag 111. peak
to lower angles closer to the Ag 111. bulk position. was
observed Fig. 4b, Table 2.. A gradual increase of the Ag
200. maximum indicates a pronounced phase separation
with increasing annealing temperature.

Fig. 5. a. The effect of XeCl laser irradiation on XRD of Ag 75 Co 25

films 300 nm thick F s 0.1 J cmy2 , ns 0, 1, 10, 50 and 100.. b.
Detail showing the shifts of Ag 111. peak.

and GIXRD data, the Ag 111. peak shifts to higher angles

with increasing Co content up to 2023 at.% reaching a
maximum of 2Q angle and then, with increasing Co
content, moves to lower angles again.
The Ag 200. and Co 111. peak slightly increases with
increasing Co content. These results correspond with the
data on Ag 100yx Co x x s 0100%. codeposits published
by Sang et al. w13x. Starting from the pure Ag film, the
authors observed a decrease of this peak up to x s 22 at.%
first, then a gradual increase and broadening. This behaviour is most probably a result of different degree of
phase separation in as-deposited samples with a different
Co content.
4.1.2. Effect of RTA
In Fig. 4a,b, the effect of RTA on XRD spectra of
Ag 75 Co 25 film is summarized. Here, a development of fcc
Ag phase and the increase of grain size with increasing

4.1.3. Effect of laser irradiation

Also for laser irradiation studies the Ag 75 Co 25 film was
used, because, according to our preliminary results, the
highest GMR ratio at room temperature in as-deposited
state was obtained for this composition cf. w20x.. The
effect of laser irradiation with F s 0.1 J cmy2 and n s 1,
10, 50 and 100 on the XRD spectra is summarized in Fig.
5a,b. The shift of the Ag 111. peak with increasing
number of pulses is summarized in Table 3.
While for the as-deposited sample the Ag 111., 200.,
and 222. peaks were found, after laser irradiation, 220.
and 311. peaks also appear. This means that the grain
orientations are more random. Also the shape of the Ag
200. and Co 111. shoulder indicates the different degrees
of phase separation c.f. w13x.. From Table 3, it follows
that the Ag 111. peak shifts to higher angles, apart from
Ag 111. bulk position.
The XRD spectrum of the Ag 75 Co 25 sample irradiated
with the highest fluence F s 0.2 J cmy2 and 10 pulses is
compared with the spectrum of the as-deposited sample in
Fig. 6a,b. As it will be shown later, this sample also
possess the highest GMR ratio after irradiation. For the
irradiated sample a split Ag 111. maximum with positions
2Q s 38.25 close to the value for pure Ag. and 38.74 was
observed, and the Ag 200. shoulder is significantly suppressed.
From Figs. 5 and 6 it follows that in Ag 75 Co 25 film, a
structure with smaller Ag grain size develops due to laser
irradiation. The origin of splitting of the Ag 111. peak is
not clear. Considering that the laser treatment is a nonequilibrium solidification process, a formation of some
metastable phases cannot be excluded c.f. w21x.. On the
other side, the shift of Ag 111. peak pointing at the
decrease of Ag lattice parameters could originate due to
strains at the boundaries between Ag and Co crystallites
w19x.

Table 3
The exact position of Ag 111. peak vs. number of laser pulses for
Ag 75 Co 25 films
Number of pulses

Ag 111. 8.

as-deposited
1
10
50
100

38.61
38.81
38.81
38.82
38.75

F s 0.1 J cmy2 .

20

S. Luby et al.r Thin Solid Films 311 (1997) 1522

Table 4
RT and LHe resistivities of Ag 75 Co 25 films irradiated by XeCl laser
Thermal processing

r RT, m V cm.

r 4.2 K, m V cm.

As-deposited

18.9

17.4

0.1 J cmy2
1 pulse
10
50
100

20.4
20.4
20.4
21.75

20.25
18.80
18.8
20.10

0.15 J cmy2
1 pulse
10
50
100

21.75
21.75
21.75
21.75

19.88
19.38
19.00
19.70

0.2 J cmy2
1 pulse
10

19.0
19.0

20.5
19.83

Zero field cooled samples.

splitting of Ag 111. peak could hint at the presence of

some AgCo phase beside the pure Ag.

4.2.2. GMR
The representative GMR curves of the as-deposited
Ag 75 Co 25 film 300 nm thick is shown in Fig. 7. It should
be noted that the resistance is not saturated at 50 kOe. The
curves show hysteresis. The maxima of GMR 74%. occur
at the coercive field Hc 5 s 1570 Oe. Our results are similar
to those published for Ag 100yx Co x films e.g., w10,22x..
Fig. 6. a. The effect of XeCl laser irradiation on XRD of Ag 75 Co 25
films 300 nm thick F s 0.2 J cmy2 , ns 0 and 10.. b. Detail showing
the shift of Ag 111. peak.

4.2. Resistiityr GMR

4.2.1. Resistiities of irradiated samples
The resistivities of Ag 75 Co 25 films 300 nm thick irradiated by XeCl laser at various conditions are summarized in
Table 4. These values are lower than the resistivity f 40
m V cm reported in Ref. w10x for dc magnetron sputtered
films with 25 at.% Co. The difference may be due to
different structure and content of gases in evaporated and
sputtered films.
The TCR of as-deposited sample is positive as it is
typical for crystalline metallic systems. The same sign of
TCR was found for all irradiated samples. Only samples
irradiated with the highest fluence F s 0.2 J cmy2 with 1
and 10 pulses reveal negative TCR. This could imply, that
after the most severe irradiations, the structure of AgCo
film becomes more disordered. As mentioned above, the

Fig. 7. GMR curves of the as-deposited dots. and irradiated at F s 0.2 J

cmy2 , ns10 full line. Ag 75 Co 25 film 300 nm thick measured with
magnetic field parallel to the film plane.

S. Luby et al.r Thin Solid Films 311 (1997) 1522

21

Table 5
GMR and coercive field Hc of Ag 75 Co 25 film vs. laser irradiation conditions
DGMR %. H H , 300 K

Irradiation

GMR %. H 5 , 4.2 K

Hc 5 Oe.

GMR %. H H , 4.2 K

Hc H Oe.

GMR %. H H , 300 K

As deposited

74

1570

74.3

1730

11.3

F s 0.1 J cmy2
1 pulse
10
50
100

71
71.1
69
68.8

1650
1470
1620
1570

74.3
72
70.9
69.9

1680
1750
1740
1640

12.2
11.5
12.2
13.2

0.9
0.2
0.9
1.9

F s 0.15 J cmy2
1 pulse
70.6
10
66.6
50
y
100
70.3

1500
1580
y
1614

72
68.2
71.9
68.8

1600
1440
1430
1620

13.08
12.17
13.28
13.5

1.78
0.87
1.98
2.2

F s 0.2 J cmy2
1 pulse
73.8
10
82

1520
1180

76.2
81

1850
1700

12.1
13.46

0.8
2.16

DGMRs GMR irradiated sample y GMR as-deposited sample .

Results from films irradiated by laser at various conditions

are summarized in Table 5.
In Table 5, the effect of laser irradiation on the GMR at
4.2 K and at 300 K can be seen. At 4.2 K, the increase of
GMR due to laser irradiation appears only at the most
severe irradiation conditions Fig. 7.. At 300 K, the increase is systematic, although with fluctuations. It should
be noted that the RT resistance was measured only up to
15 kOe and, thus, the RT GMR is roughly evaluated.
Nevertheless, the absolute values of DGMR DGMRs
GMR irradiated sample y GMR as-deposited sample . are 1.92.2%
for irradiations with n s 100 pulses at various fluences,
and the relative increase of GMR DGMRrGMR. is between 16 and 19% at the same conditions.
The different behaviour of GMR at 4.2 K and 300 K
will be studied in more details later. We hope that our
results give a good preliminary evidence that GMR of
Ag 100yx Co x films can be improved by laser irradiations,
which form more disordered granular structure with smaller
grain size.
For comparison, we have measured also the GMR of
RTA processed and standard furnace annealed Ag 75 Co 25
films 300 nm thick. Using RTA, it was possible to obtain
values DGMRf q2% for 5008Cr30 s annealing conditions. At 7508Cr30 s, GMR decreased y7%.. After
furnace annealing at 4008C and 5008C during 10 and 30
min, GMR decreased systematically DGMR s y3
13.%.. The increase of GMR after annealing at 5008Cr30
s can be attributed to the improved phase separation and
annealing out of defects.
Obviously, the structure of the film influences the GMR
in Ag 75 Co 25 film considerably. It can be assumed that
GMR can be increased by changing the as-deposited structure to a more disordered laser irradiation. or ordered one
RTA.. However, if the grains are too large, the GMR
decreases because of decreasing the interfaces between

magnetic particles and non-magnetic matrix and probability of electron spin-dependent scattering. TEM investigations can explain these effects in a more straightforward
way.
5. Conclusions
From our experiments, it follows that by the pulse XeCl
laser irradiation with fluences F s 0.10.2 J cmy2 , it is
possible to influence the granular codeposited Ag 75 Co 25
film considerably. After laser irradiation, the structure of
the film is more random with smaller grain size, and the
negative TCR hints on some level of structural disorder.
Under these conditions, the absolute increase of GMR
from 74 to 82% was observed at 4.2 K and from 11.3 to
13.5% at 300 K after irradiation. The corresponding relative increase of GMR is 10.3% and 19%, respectively.
Similar increases of GMR were obtained by rapid thermal
annealing of the films. We conclude that GMR can be
increased by changing the as-deposited structure of the
film to a more disordered laser irradiation. or ordered, to
some extent RTA., state.
Acknowledgements
Authors acknowledge the support of this work by Scientific Grant Agency, Bratislava grant 5305r476..
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