ISSN 10637826, Semiconductors, 2015, Vol. 49, No. 10, pp. 12531258. Pleiades Publishing, Ltd., 2015.

Original Russian Text E.P. Zaretskaya, V.F. Gremenok, A.V. Semchenko, V.V. Sidsky, R.L. Juskenas, 2015, published in Fizika i Tekhnika Poluprovodnikov, 2015, Vol. 49,
No. 10, pp. 12971303.

NONELECTRONIC PROPERTIES OF SEMICONDUCTORS

(ATOMIC STRUCTURE, DIFFUSION)

Structural Properties of ZnO:Al Films Produced

by the SolGel Technique
E. P. Zaretskayaa*, V. F. Gremenoka, A. V. Semchenkob, V. V. Sidskyb, and R. L. Juskenasc
a

Scientific and Practical Materials Research Center, National Academy of Sciences of Belarus, Minsk, 220072 Belarus
b
Gomel State University, Gomel, 246699 Belarus
c State Research Institute Center for Physical Sciences and Technology, Vilnius, LT01108, Lithuania
*email: ezaret@ifttp.basnet.by
Submitted January 12, 2015; accepted for publication February 5, 2015

AbstractZnO:Al films are produced by solgel deposition at temperatures of 350550C, using different
types of reagents. Atomicforce microscopy, Xray diffraction analysis, Raman spectroscopy, and optical
transmittance measurements are used to study the dependence of the structural, morphological, and optical
properties of the ZnO:Al coatings on the conditions of deposition. The optical conditions for the production
of ZnO:Al layers with preferred orientation in the [001] direction and distinguished by small surface rough
ness are established. The layers produced in the study possess optical transmittance at a level of up to 95% in
a wide spectral range and can be used in optoelectronic devices.
DOI: 10.1134/S1063782615100280

1. INTRODUCTION
Zinc oxide is a widegap semiconductor (Eg = 3.37 eV)
that possesses a unique combination of optical, acous
tic, and electrical properties and is extensively used in
a number of optoelectronic devices, such as converters
of surface acoustic waves (SAWs), solar cells, optical
waveguides, laser reflectors, broadband filters, and liq
uidcrystal displays (LCDs) [14]. To improve the
conductivity of zinc oxide, it is doped with aluminum,
gallium, and indium [57]. Most attention is given to
aluminumdoped zinc oxide (ZnO:Al) with the pur
pose of using it as a transparent conductive contact. In
fact, the transparency of ZnO:Al in the visible and
infrared (IR) regions is ~90%, and the resistivity is
102104 cm. The material ZnO:Al is more stable
to hydrogen plasma compared to other transparent
oxides and, in addition, can be used as an efficient
antireflection coating (the refraction coefficient is
~1.89) [8]. Aluminumdoped zinc oxide films are pro
duced by magnetronassisted evaporation [9], elec
tronbeam sputtering [10], and chemical and solgel
deposition [1114]. Of special interest is investigation
of the possibilities of the production of ZnO:Al films
with controllable physical characteristics by solgel
deposition [1517]. The solgel technique offers a
number of advantages for industrial application. These
are simplicity of the technological process of the dep
osition of largearea coatings, the low cost of equip
ment used in the process, and the large variety of
appropriate reagents.
Depending on the conditions of deposition,
ZnO:Al films produced by solgel deposition are dif
ferent in microstructure, which defines the different

electrical and optical parameters of the films. The

main problem lies in producing [001]oriented ZnO
films at low temperatures. According to the data
reported in publications, a major influence on the ori
entation of the solgel films in the [001] direction is
exerted by the composition and concentration of sol
vents and the sintering and annealing temperatures
[18, 19].
The purpose of this study is to understand how the
structural and optical characteristics of ZnO:Al films
depend on the conditions of solgel deposition and to
choose the optimal conditions for the formation of
ZnO:Al films of high crystalline quality.
2. EXPERIMENTAL
2.1. Deposition of Coatings
The precipitation of ZnO:Al coatings was per
formed by depositing a sol by centrifugal separation
(the spincoating procedure). To prepare the film
forming solution, the required amounts of zinc acetate
and aluminum nitrate were flooded with absolute iso
propyl alcohol (dimethyl formamide or 2methoxy
ethanol depending on the type of the sol) and mixed in
an ultrasonic bath for 30 min to obtain a homogeneous
solution. For aging, the solution was kept at the ambi
ent temperature (22 2)C for two or three days.
Monoethalamine was used as a catalyst that reduces
the period of aging of the solutions to two days and
provides their stability for a month. After the deposi
tion of a ~50nmthick seed sol layer onto glassy and
singlecrystal silicon substrates, the substrates were
placed into a thermostat and heated to a temperature

1253

1254

ZARETSKAYA et al.

002

Intensity, arb. units

Intensity, arb. units

002

no. 3
no. 2
no. 1
34

35
2, deg

100 101

004
no. 3
no. 2
no. 1

20

30

40

50

60

70

80
90
2, deg

Fig. 1. XRD patterns of ZnO:Al coatings produced by sol

gel deposition from solutions based on (1) 2methoxyeth
anol, (2) dimethyl formamide, and (3) isopropyl alcohol.

of 350C with a step of 20C over 10 min. The deposi

tion and drying process was repeated until the required
coating thickness was reached. After the cycle of dep
osition of the ZnO:Al films, their total thickness cal
culated from the scanning electron microscopy
(SEM) data was ~330 nm. During the final stage of the
process, the substrates with the deposited coating were
subjected to annealing via heating in stages to 550C
(with a step of 20C).
2.2. Investigation Methods
The phase composition and crystalline structure of
the deposited layers were studied by Xray phase anal
ysis (XPA) with a D8 Advance (Bruker AXS) diffracto
meter operating with CuK radiation ( = 0.1542 nm)
filtered by a multilayered Ni/graphite monochroma
tor. The voltage supplied to the tube was 40 kV, and the
current was 40 mA. Xray diffraction (XRD) patterns
were obtained at grazing incidence (GI) in the scan
ning mode of measurements with a step of 0.04 (on
the 2 scale) and a counting time of 5 s. The angle of
incidence of the primary beam was = 0.5. To adjust
the diffractometer, we used the certified SRM 606
standard (LaB6 powder) of the National Institute of
Standards and Technology (NIST), USA. The phases
were identified by comparing the experimentally
determined interplanar spacings d with data of the
Joint Council for Power Diffraction Standards
(JCPDS), 2013. The microstructural characteristics of
the films were studied by SEM using an H800 (Hita
chi, Japan) SEM microscope with a resolution of
0.2 nm. The elemental composition of the material of
the films was determined using an INCA 350 (Oxford

Instruments, UK) energydispersive Xray spectral

microanalyzer with a resolution of 1 m3 and a sensi
tivity of 0.1 at %.
The surface topography of the ZnO:Al layers was
studied using a SOLVER Pro 47 (NTMDT) highres
olution atomicforce microscope (AFM). The trans
mittance spectra of the ZnO films were studied in the
wavelength range from 0.19 to 3.00 m with a Cary
500 Scan (UVVisNiR Spectrometer, Varian, USA)
spectrophotometer.
The Raman spectra were recorded with a
Nanofinder High End spectrometer. For the excita
tion source, we used a solid laser emitting at a wave
length of 473 nm. All of the measurements were con
ducted at a temperature of T = 293 K in the backscat
tering geometry of recording in the spectral range from
150 to 3000 cm1.
3. RESULTS
3.1. Structural Properties of ZnO:Al layers Produced
in Different Reagents
The ZnO:Al coatings produced with different
thicknesses (150330 nm) in all types of reagents are
highly adhesive to glassy and silicon substrates and
physically stable and do not flake off upon heating to
temperatures above 550C.
According to the XPA data, the films are polycrys
talline singlephase hexagonal wurtzitestructured
materials (Fig. 1). In the XRD patterns of the ZnO:Al
layers, we can see a dominant reflection from the (002)
plane of ZnO at 34.37, lowintensity reflections from
the (100) and (101) planes, and the (004) second
order reflection from the (002) plane at 72.62. The
angular position of the reflections is in agreement with
the JCPDS data for nominally pure zinc oxide
(JCPDS, no. 361451). Irrespective of the type of ini
tial reagents used for the deposition of ZnO:Al films,
no foreign phases, such as Al or Al2O3 are detected in
the films. This suggests that the Al3+ ions substituting
Zn2+ ions do not disrupt the hexagonal wurtzitetype
structure of ZnO.
A substantial factor influencing the structural
ordering of the layers is the choice of reagent. The
ZnO:Al films produced using zinc acetate and alumin
ium nitrate in a solution of dimethyl formamide (series
no. 1) do not exhibit any pronounced texture. The
XRD patterns of these layers feature a very low inten
sity and a large full width at halfmaximum (FWHM =
0.42) of the (002) reflection, which is indicative of the
small grain size of the film coatings (see inset in Fig. 1).
The ZnO:Al films produced from zinc acetate and
aluminium nitrate in a solution of methoxyethanol
and monoethalamine (series no. 2) exhibit a higher
intensity and a smaller FWHM (0.36) of the (002)
reflection. The most pronounced texture in the [001]
direction is inherent in the ZnO:Al films produced
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438
574

1105
1158

330

Intensity, arb. units

E2(high)

Intensity, arb. units

using zinc acetate and aluminium nitrate in a solution

of isopropyl alcohol and monoethalamine (series
no. 3). The FWHM of the (002) reflection in these lay
ers is reduced to 0.21 (see inset in Fig. 1), and the pre
dominant [001]orientation factor calculated from the
relation I[001] = I(002)/(I(100) + (I(101) + I(110))is increased
from 2.07 (series no. 2) to 5.05, which is indicative of
improved structure and increased grain size.
The results of Raman spectroscopy of the coatings
are in good agreement with the XPA data. According
to group theory, in ZnO that crystallizes in the hexag
onal wurtzitetype structure with the spatial sym
metry C6v, there exist the following set of phonon
modes: 1A1(TO) + 1A1(LO) + 2B1 + 1E1(TO) +
1E1(LO) + 2E2 [20]. Among these, two modes of sym
metry B1 are inactive in the Raman spectra [21]. In
ZnO, phonon modes are observed at the following fre
quencies: E2(low) = 101 cm1, E2(high) = 437 cm1,
A1(TO) = 380 cm1, A1(LO) = 574 cm1, E1(TO) =
407 cm1, and E1(LO) = 583 cm1. If the incident beam
is strictly normal to the surface of the ZnO layer, only
the A1(LO), E2(low), and E2(high) vibrations are bound to
be observable, whereas other modes are forbidden by
selection rules. It is known that the intensity and fre
quency position of the E2(high) mode is heavily depen
dent on strains in the ZnO crystal lattice [22]. At the
same time, investigation of the spectral characteristics
of the A1(LO) vibration makes it possible to gain infor
mation not only on the chemical composition of the
ZnO:Al coatings, but on the presence of foreign
phases and locally ordered regions of the crystal lattice
as well.
In accordance with the data reported in [20], all of
the bands observable in the Raman spectra of the coat
ings (Fig. 2) can be attributed to scattering at phonons
of zinc oxide. In the Raman spectra of all of the
ZnO:Al films (series nos. 13), we observe the high
frequency E2(high) mode in the range 427439 cm1,
and the A1(LO) mode in the range 575582 cm1. The
330cm1 mode corresponds to a secondorder vibra
tion and is defined mainly by the vibrations of Zn
atoms [23]. The allowed E2(high) and A1(LO) modes cor
respond to the vibrations of oxygen atoms in a perfect
ZnO crystal and to local vibrations of intrinsic lattice
defects, such as oxygen vacancies and interstitial cat
ions [23].
The spectral positions, intensities and FWHMs of
the E2(high) and A1(LO) vibrations are substantially differ
ent for the ZnO:Al coatings produced in different
reagents. The E2(high) and A1(LO) modes observed in
samples of series nos. 1 and 2 are shifted from the stan
dard positions in ZnO to lower frequencies. The sig
nificant red shift ( 8 cm1) of the E2(high) mode is
caused by disorder of the crystal lattice and the non
uniform distribution of Al impurities and is indicative
of compression stresses in the coatings [24].

1255

no. 3
no. 2
no. 1

400
450
500
Raman shift, cm1

no. 3
no. 2
no. 1

500

1000

1500

2000

2500
3000
Raman shift, cm1

Fig. 2. Raman spectra of ZnO:Al coatings produced by

solgel deposition from solutions based on (1) 2metoxy
ethanol, (2) dimethyl formamide, and (3) isopropyl
alcohol.

As the crystal quality of the ZnO:Al coatings is

improved, the E2(high) and A1(LO) modes shift to higher
frequencies. At the same time, the intensity of these
vibrations increases, and their FWHM decreases (by 8
and 10 cm1 for the E2(high) and A1(LO) modes, respec
tively.) In the Raman spectra of the ZnO:Al films of
series no. 3, the peak related to the E2(high) vibration is
symmetric (see inset in Fig. 2), suggesting some order
ing of the crystal lattice [22]. For the series of ZnO:Al
coatings produced in a solution of isopropyl alcohol
and monoethalamine (series no. 3), the positions of
the E2(high) and A1(LO) vibrations shift to the standard
positions in ZnO. This means that the coatings of
series no. 3 are practically unstressed.
The fact that the E2(high) mode defined by vibrations
of oxygen atoms in the ZnO crystal lattice is more sus
ceptible to the effect of the fabrication conditions in
comparison with the E2(low) mode attributed to vibra
tions of the zinc sublattice implies that defects in the
oxygen sublattice are dominant. The increase in the
intensity of the E2(high) mode with improving crystal
quality of the coatings is indicative of ordering of the
oxygenanion sublattice in layers formed in the opti
mally chosen reagents and deposition conditions.
It should be noted that the A1(LO) mode observed in
the Raman spectra of the coatings at 574 cm1 is asym
metric (Fig. 3a). According to [25], the asymmetry of
the A1(LO) mode observed in the Al and Gadoped
ZnO films is attributed to local disorder produced in
the crystal lattice by oxygen vacancies and interstitial

1256

Intensity, arb. units

4000

2000

Intensity, arb. units

2500

2000

1500

ZARETSKAYA et al.

the superposition of LO modes and containing contri

butions of the secondorder modes 2E1(LO) at
1104 cm1 and 2A1(LO) at 1157 cm1 at the point of
574
(a)
the Brillouin zone (Fig. 3b) [22]. Ordering of the crys
557
tal structure of the coatings is accompanied by an
E1(LO)
increase in the intensity of the 2A1(LO) and 2E1(LO)
modes and by their shift to higher frequencies, specif
A1(LO)
ically, to 1140 cm1 for the samples of series nos. 1 and
2 and to 1154 cm1 for the samples of series no. 3. The
Raman spectra of the ZnO:Al coatings with the highly
dominant [001] orientation (series no. 3) feature clear
resolved 2A1(LO) and 2E1(LO) modes.
It should be noted that, in the vibrational spectra of
all of the ZnO:Al coatings, only the lines related to the
fundamental vibrations of the wurtzitestructured
ZnO host compound are evident. No additional vibra
tions relevant to phases of another type of symmetry
are observable. This suggests the lack of local struc
tural objects and the random distribution of defects in
550
600
650 the systems.
500
Raman shift, cm1
The XPA and Raman spectroscopy data are in good
agreement with the results of atomicforce micros
(b)
1104
copy (AFM) studies of the surface morphology of the
coatings. For comparison of the topographies of the
2LO
1157
ZnO:Al films deposited onto singlecrystal silicon
substrates with the use of different solvents, we chose
surface regions 98.287 m2 in area. As can be seen
from the AFM images (Fig. 4), the coatings produced
2A1(LO)
in all types of reagents are continuous, with no visible
984
pores or puncturing, and formed of pyramidal crystal
2TO
lites grown along the same direction orthogonal to the
substrate surface. The lowest surface roughness is
observed for the ZnO:Al layers produced with isopro
pyl alcohol as the solvent. The roughness of these lay
ers is 4.3 nm, and the average grain size is 19.3 nm. The
use of methoxyethanol and dimethyl formamide as the
solvents does not have any profound effect on the
topography of the surface of the ZnO:Al coatings;
however, the layers produced in the solution of dime
1000
1200
thyl formamide are smoother: their roughness is
Raman shift, cm1
6.5 nm.

Fig. 3. Raman spectra of ZnO:Al coatings produced by

solgel deposition from solutions based on isopropyl alco
hol (series no. 3): (a) Gaussian approximation of the
A1(LO) phonon mode; (b) Gaussian approximation of the
2LO phonon mode.

zinc atoms. Consequently, it can be concluded that the

higher intensity of the 557cm1 vibration in the
Raman spectra of the samples of series no. 3 is condi
tioned by the higher Al3+ concentration in these layers
compared to the Al3+ concentration in the samples of
series nos. 1 and 2.
At the same time, in the highfrequency region of
the Raman spectra (at frequencies about 1154 cm1,
we observe a broad asymmetric peak corresponding to

3.2. Effect of Annealing on the Properties

of ZnO:Al Layers
If the ZnO:Al layers produced in the solution
of isopropyl alcohol and monoethalamine
(HOCH2CH2NH2) (series no. 3) are recrystallized
in the temperature range from 350 to 600C, we
observe improvement in the structure with increasing
annealing temperature (Fig. 5). The inset in Fig. 5
illustrates the change in the FWHM of the (002)
reflection under variations in the recrystallization
temperature. As the annealing temperature is
increased from 350 to 500C, the FWHM of the (002)
reflection decreases from 0.4 to 0.16, and the predom
inant [001]orientation factor increases from 0.49 to
1.37, suggesting the formation of a ZnO:Al layer tex
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STRUCTURAL PROPERTIES OF ZnO:Al FILMS

X: 9.9 m Y: 9.9 m Z: 99.5 nm [33.9:1]
Ra: 4.8 nm Rq: 7.1 nm

002

X,

5.0
5.0
Y,
m

Z, mm

550C

Intensity, arb. units

90
72
54
36
18
0

Intensity, arb. units

9.9
9.9

1257

002

600C
500C
450C

350C
34

35
2, deg

100

101
102

103

110

0
X: 9.9 m Y: 9.9 m Z: 146.0 nm [17.7:1]
Ra: 9.3 nm Rq: 12.6 nm

30

X,
m

9.9
5.0
Y, m

X: 9.9 m Y: 9.9 m Z: 51.7 nm [55.6:1]

Ra: 2.5 nm Rq: 3.5 nm

Z, mm

135
108
81
54
27
0

X,

5.0
Y, m

45
36
27
18
9
0

Z, mm

5.0

9.9

9.9

Fig. 4. AFM images of ZnO:Al coatings produced by sol

gel deposition from solutions based on (1) 2methoxyeth
anol, (2) dimethyl formamide, and (3) isopropyl alcohol.

tured along the c axis of the hexagonal structure. As the

annealing temperature is increased to 600C, we
observe the opposite tendency: the predominant
[001]orientation factor decreases to 1.23. In the coat
ings, the grain size estimated from the FWHM of the
(002) reflection by the Scherrer formula D
0.9/cos (where = 0.1542 nm and is the FWHM
of the reflection in radians) increases from 8.1 to 21.0 nm,
as the annealing temperature is increased from 350 to
500C, and then decreases to 16.5 nm, as the anneal
ing temperature is increased further to 600C. The best
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50

60
2, deg

Fig. 5. XRD patterns of ZnO:Al coatings produced by sol

gel deposition from solutions based on isopropyl alcohol
(series no. 3) and subjected to recrystallization annealing.
The inset shows the (002) reflection peak on an enlarged
scale.

9.9

5.0

40

crystal structure is obtained for the samples annealed

at temperatures of 500550C. Within the limits of
experimental error, the lattice parameters of these
ZnO:Al layers are slightly smaller than those for nom
inally pure ZnO: according to the JCPDS no. 00036
1451, the lattice parameters of ZnO are a = 3.24982
and c = 5.20661 and the average lattice parameters
of ZnO in the deposited ZnO:Al layers are a =
3.231(69) and c = 5.185(39) .
The Al dopant impurity is incorporated into ZnO
by the substitution of Al3+ ions with Zn2+ ions in the
ZnO lattice and by the formation of interstitial Al
defects. Since the Al3+ion radius (0.53 ) is smaller
Zn2+
than the Zn2+ion radius (0.74 ), the Al3+
substitution is bound to yield a decrease in the lattice
parameters. At the same time, it can be thought that
interstitial Al defects are bound to increase the lattice
parameters. The observed decrease in the lattice
parameters of doped ZnO:Al layers is attributed to the
fact that, as the annealing temperature is increased,
the relative content of Al atoms incorporated though
Zn2+ statistical
the prevailing mechanism of Al3+
substitution increases. Studying the elemental compo
sition of the ZnO:Al films shows that the Al content in
these layer is about 0.4%.
The optical transmittance of all of the ZnO:Al lay
ers produced in the study is higher than 80% in the vis
ible spectral region (Fig. 6). However, the ZnO:Al lay
ers annealed at recrystallization temperatures above
500C feature transmittance increased to 95% in the
spectral range from 400 to 800 nm and a sharper
absorption edge around 380 nm, which is close to the
intrinsic band gap of ZnO (3.2 eV).

1258

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REFERENCES

Transmittance, %
100
80
Baseline, %
350C
450C
500C
550C
600C

60
40
20
0
200

400

600

800
1000
Wavelength, nm

Fig. 6. Optical absorption spectra of ZnO:Al coatings pro

duced by solgel deposition from solutions based on iso
propyl alcohol (series no. 3) and subjected to recrystalliza
tion at temperatures of 350, 450, 500, 550, and 600C.

From the above data, it follows that the most rea

sonable temperature conditions of annealing corre
spond to the range from 450 to 500C. These temper
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500800C reported in previous publications [18].
4. CONCLUSIONS
As a result of this study, procedures for the solgel
deposition of polycrystalline singlephase wurtzite
structured ZnO:Al films with the use of different types
of solvents are developed. Studying the structural and
morphological characteristics shows that the optimal
reagent for the production of ZnO:Al layers with the
highest degree of dominant orientation in the [001]
direction and with the lowest surface roughness
(4.3 nm) is isopropyl alcohol. From analysis of the
Raman spectra of all of the coatings under study, it is
found that, in the ZnO:Al layers, there are no local
structural agglomerates and the defect distribution is
random. The ZnO:Al layers produced at the optimally
chosen conditions of deposition feature a high degree
of ordering of the anion sublattice. It is shown that
recrystallization of the ZnO:Al layers at an annealing
temperature of 450550C provides a means for fabri
cating coatings of high structural quality, with an opti
cal transmittance of up to 95% in the spectral range
400800 nm. Such coatings are suitable for use in
optoelectronic devices.
ACKNOWLEDGMENTS
The study was supported by the Belorusian Republi
can Foundation for Basic Research, project no. T14ARM.

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Translated by E. Smorgonskaya
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