Thin Solid Films 518 (2010) 39453948

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Thin Solid Films

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / t s f

Morphological and structural investigations of CoMgF2 granular thin lms grown by

thermionic vacuum arc
V. Ionescu a, M. Osiac b,, C.P. Lungu c, O.G. Pompilian c, I. Jepu c, I. Mustata c, G.E. Iacobescu b
a
b
c

Ovidius University, 900527, Constanta, Romania

Faculty of Physics, University of Craiova, 200585, Craiova, Romania
National Institute for Laser, Plasma and Radiation Physics, Bucharest-Magurele, 077125 Romania

a r t i c l e

i n f o

Article history:
Received 3 June 2009
Received in revised form 1 February 2010
Accepted 12 February 2010
Available online 19 February 2010
Keywords:
Thermionic vacuum arc
Thin lms
CoMgF2 plasma

a b s t r a c t
CoMgF2 granular lms were deposited in thermionic vacuum arc plasma with simultaneous ignition of
plasma in Co and MgF2 vapours. The samples were investigated by transmission electron microscopy which
revealed Co grains of a few nm in diameter embedded in the MgF2 matrix. The crystalline phase for Co and
MgF2 was studied by electron diffraction after selecting a typical area of the sample. Low-angle x-ray
diffraction method was used to verify the bulk crystalline structure of the samples. The surface morphologies
of the lms were investigated by atomic force microscopy. The magneto-optical longitudinal Kerr rotation
spectra of the lms were also measured and compared.
2010 Elsevier B.V. All rights reserved.

1. Introduction
Combinations of metalnonmetal granular soft magnetic lms
such as CoAl2O3, CoMgO, FeSiO2, and FeSrF2 have attracted much
interest in the last years, due to their electrical and magnetic
properties, such as high electrical resistivity, low coercivity, low
effective magnetic anisotropy, and very weak inter-particle magnetic
interaction.
Good magnetic properties including susceptibilities of 10 3 up to
1
10 , electrical resistivity over 500 cm, saturation ux densities of
about 1 T, and coercivities as low as 10 A/m have been obtained [14].
For example, CoMgF2 granular system is used as thin lm inductor in
power converters for microprocessors, with fast response, high
efciency and small size. Magnesium uoride (MgF2) was chosen as
an insulating material because of its low evaporation point. This
material has a high resistivity due to the wider gap and smaller
dielectric constant than e.g. MgO and Al2O3, and it has a tendency to
get separated from the co-evaporated metal [5,6].
Networks of magnetic tunnel junctions are formed in ferromagnetic metal (FM)-insulator granular lms composed of metallic
nanodots embedded in the insulating matrix. The tunneling magnetoresistance effect due to spin-dependent tunneling between neighbouring FM dots has been intensively studied [79].
In the present study we propose the use of a thermionic vacuum
arc (TVA) deposition technique for coating smooth, nanostructured
CoMgF2 granular thin lms onto glass substrates. We investigated

Corresponding author.
E-mail address: m_osiac@yahoo.com (M. Osiac).
0040-6090/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.tsf.2010.02.035

two samples placed at two different positions relative to the anode of

the discharge that produces the Co plasma.
2. Experimental details
The method used here based on TVA for deposition of granular
lms was described in details elsewhere [10,11]. It uses two identical
set-ups which produce two separate electron beams emitted by
externally heated cathodes. Each cathode is made from a tungsten
wire with a diameter of 1 mm. The electron beams are accelerated by
high anodic voltages and bombard simultaneously the crucibles
placed at the anodes, as shown in Fig. 1. The crucibles contain each a
few grams of Co and MgF2, respectively. By applying a high voltage
between 1 and 6 kV on each of the anodecathode sets, two different
plasmas are formed in pure Co and MgF2 vapours. The chamber is
pumped down by mechanical and diffusion pumps until a pressure of
2.7 * 10 3 Pa is obtained.
Both plasmas expand in the high vacuum chamber and reach the
surface of the substrates of the samples, which are grounded.
The currents used to heat the cathode laments are between 40
and 55 A. The current of the discharge ignited in Co vapours is
Idisch = 0.7 to 0.8 A at a voltage Udisch = 400 V. In the case of the
discharge ignited in MgF2 vapours, the current and the voltage were
Idisch = 0.4 to 0.5 A and Udisch = 300400 V, respectively. The deposition rate rd and lm thickness d were measured and controlled in situ
using a FTM7 quartz microbalance. The thickness of the CoMgF2
coatings was 200 nm.
The lm substrates were rectangular pieces of industrial glass with
an area of 15 15 mm2. The studied thin lm samples were located at
P1 above and just in front of the Co crucible and P2 at mid-distance

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V. Ionescu et al. / Thin Solid Films 518 (2010) 39453948

Fig. 1. Experimental set-up for CoMgF2 thin lm deposition.

between the anodes as illustrated in Fig. 1. The distance between the

Co crucible and P1 sample was 250 mm, while the distance between
the Co crucible and P2 sample was 275 mm. The substrates were
maintained at T = 300 K during deposition.
The transmission electron microscopy (TEM) analyses were
carried out using a Philips CM120ST microscope operating at 100 kV
with Cs = 1.2 mm and 2 resolution. The x-ray diffraction (XRD)
patterns were obtained using a Shimadzu model 6000 diffractometer
operating with Cu K radiation (40 kV, 30 mA). The atomic force
microscopy (AFM) data were recorded in non-contact mode using a
Park XE-100 equipment (silicon tip with conical shape). The AFM
scans were taken over the area 5 5 m2. We used the horizontal line
by line attening as planarization method.
Finally, the magnetic properties of the lms were investigated via
longitudinal Magneto-Optic Kerr Effect (MOKE), using p-polarized,
633 nm HeNe laser light (10 mW power) as an incident light. The
incident beam was modulated with an electro-optic-modulator.
The magnetic eld was applied parallel to the lms and lays in the
incidence plane of HeNe laser.
3. Results and discussion
The TEM image of P1 sample, presented in Fig. 2(a) shows a
network-like structure of nanoscale grains of Co (dark areas) and
thin intergrain boundaries of MgF2 (light areas). The grain size is
about 34 nm in diameter with intergrain regions of 36 nm width.
The TEM image of P2 sample presented in Fig. 2(b) shows the presence
of some very ne dark spots (Co) xed in a lighter area surface (MgF2

Fig. 2. Cross-sectional TEM images for: a) sample P1; b) sample P2; and c) SAED pattern
for sample P1.

Fig. 3. XRD patterns of: a) sample P1; and b) sample P2.

V. Ionescu et al. / Thin Solid Films 518 (2010) 39453948

3947

For sample P1 the well dened diffraction rings shown in SAED

pattern (Fig. 2(c)) correspond to the interplanar distances of
0.212 nm and 0.194 nm. These values t well with the distances of
the (100) and (101) diffraction planes for the hexagonal-close-packed
(hcp) phase of Co. This measurement proves the presence of
crystalline structure of Co grains in the MgF2 matrix of sample P1.
Low-angle XRD analyses were performed to establish the presence
of crystalline phases in the coatings. In the XRD patterns of both
samples P1 and P2 the 2 diffraction peaks can be assigned to (110),
(111), (210), (211) and (301) crystalline planes of MgF2 tetragonal
phase (Fig. 3). In Fig. 3(a), we can see for sample P1 the smooth slope
of the XRD curve in the 4447 range. The Co lines inserted from the
database JCPDSInternational Centre for Diffraction Data, which
overlap this angle range, allowed us to assign this slope to the
presence of Co in the MgF2 matrix. Fig. 3(b) shows that by XRD
measurements it is not possible to detect the presence of Co in sample
P2.
The topographical AFM images and subsequent statistical data
analysis, including the calculation of the root mean square roughness
(Rq), gave detailed information about the surface morphology. The
morphological AFM images of samples P1 and P2 are presented in
Fig. 4(a) and (b), respectively. The Rq values are 3.8 nm for P1 and
4.7 nm for P2. The in-plane size of the surface asperities was found to
be almost uniform for both samples, only a small number of these
asperities being higher than 10 nm for P1 and higher than 20 nm
for P2. Similar results were reported by Hosoya et al. [1] in the case of
FeSrF2 co-evaporated granular lms deposited onto MgO substrates.
In Fig. 5 we present the MOKE hysteresis loops (longitudinal
mode) at room temperature for samples P1 and P2. It can be observed
that the saturation magnetization for sample P1 is about two times
higher than that of the P2 sample; the coercivities resulting from
MOKE measurements are: 0.038 T for P1 and 0.054 T for P2.
4. Conclusions
In order to obtain CoMgF2 composite thin lms in plasmas
generated in the vapours of Co and MgF2 materials employing the TVA
technique the substrates are usually placed at 250275 mm above the
evaporating anodes. From the SAED pattern obtained by TEM analysis
we could reveal the presence of hcp crystalline phase of Co and of
nanometrical Co grains embedded in the MgF2 insulating matrix, only
in the lm placed just above the anode which produces the Co plasma.
The XRD patterns in the bulk of the same lm revealed a random
orientation of Co in the MgF2 crystalline matrix. This sample has a low
surface roughness with crack-free and densely packed microstructure.
The best magneto-optical properties are obtained for the lm with the

Fig. 4. AFM top view for a scan area of 5 5 m2 in a) sample surface P1; and b) sample
surface P2.

structure). We could not notice the existence of Co nanograins

embedded in MgF2 matrix in this case. Coonley et al. [6] reported a
similar structure for a granular soft magnetic CoMgF2 lm prepared
by evaporative co-deposition onto glass substrate, with 41% volume of
Co. In their study, the Co grain size was between 2.7 nm and 3.7 nm in
diameter, and the intergrain region widths in the range of 1 to 2 nm.

Fig. 5. MOKE measurements on samples P1 and P2 at room temperature.

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V. Ionescu et al. / Thin Solid Films 518 (2010) 39453948

Co nanograins xed in the MgF2 structure. The CoMgF2 granular thin

lm with the thickness of about 200 nm was deposited onto glass
substrates placed within the Co plasma.
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