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Materials Science and Engineering B 178 (2013) 225–230

Contents lists available at SciVerse ScienceDirect

Materials Science and Engineering B

journal homepage: www.elsevier.com/locate/mseb

FeNi3 /indium tin oxide (ITO) composite nanoparticles with excellent microwave
absorption performance and low infrared emissivity
Li-Shun Fu a , Jian-Tang Jiang a , Liang Zhen a,b,∗ , Wen-Zhu Shao a
a
School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001, China
b
MOE Key Laboratory of Micro-systems and Micro-structures Manufacturing, Harbin Institute of Technology, Harbin 150080, China

a r t i c l e i n f o a b s t r a c t

Article history: FeNi3 /indium tin oxide (ITO) composite nanoparticles were synthesized by a self-catalyzed reduction
Received 6 June 2012 method and a sol–gel process. The dependence of the content of ITO phase with the mole ratios of In:Sn
Received in revised form of different sols was investigated. The relation between the electrical conductivity, infrared emissivity of
12 September 2012
FeNi3 /ITO composite nanoparticles and the content of ITO phase was discussed. Electromagnetic wave
Accepted 28 October 2012
absorption (EMA) performance of products was evaluated by using transmission line theory. It was found
Available online 8 November 2012
that EMA performance including the intensity and the location of effective band is significantly dependent
on the content of ITO phase. The low infrared emissivity and superior EMA performance of FeNi3 /ITO
Keywords:
Microwave absorption
composite nanoparticles can be both achieved when the mole ratio of In:Sn in sol is 9:1.
Infrared emissivity © 2012 Elsevier B.V. All rights reserved.
Ferromagnetic metal
Indium tin oxide
Electrical conductivity

1. Introduction
In recent years, electromagnetic wave absorption (EMA) mate-
rials have attracted great interest because of their applications in
radar stealth and electromagnetic compatibility in the gigahertz
frequency range [1–7]. Ferromagnetic metal is a kind of impor-
tant EMA materials with higher complex permeability and higher
working frequency than ferrites [8–13]. However, the infrared
emissivity of ferromagnetic metal EMA materials is usually high,
which increases the possibility of being detected by infrared detec-
tor and limits their broad applications covering both the microwave
and infrared regions [14]. Combined with dielectric semiconductor,
ferromagnetic metal may exhibit better EMA performance due to
a large dielectric loss [15] and suppressing the eddy current effect
[3,16]. If the infrared emissivity of dielectric semiconductor is low,
low infrared emissivity of composites of ferromagnetic metal and
dielectric semiconductor can be achieved. Indium tin oxide (ITO) is
a kind of semiconductor with low infrared emissivity [17–19]. On
the other hand, the complex permittivity of the composites can be
tuned by the electrical conductivity [20–23]. Coating ITO on the sur-
face of ferromagnetic metal can adjust the electrical conductivity
∗ Corresponding author at: School of Materials Science and Engineering, Harbin
Institute of Technology, Harbin 150001, China. Tel.: +86 451 8641 2133;
fax: +86 451 8641 3922.
E-mail address: lzhen@hit.edu.cn (L. Zhen).
and infrared emissivity of the composites. The superior EMA perfor-
mance and low infrared emissivity will be simultaneously achieved
by adjusting the content of ITO phase in the composites.
In the present work, FeNi3 /ITO composite nanoparticles were
synthesized through a self-catalyzed reduction method and a
sol–gel process. The structure, morphology and composition of
FeNi3 /ITO composite nanoparticles were investigated. The electri-
cal conductivity and infrared emissivity were measured and their
relation to the content of ITO phase was discussed. The EMA perfor-
mance of coatings containing FeNi3 /ITO composite nanoparticles as
fillers was evaluated according to the transmission line theory.
2. Experimental
2.1. Synthesis of FeNi3 nanoparticles
FeNi3 nanoparticles were prepared with a self-catalyzed reduc-
tion method following our previous work [24]. Firstly, 0.06 mol
NiCl2 ·6H2 O, 0.02 mol FeCl2 ·4H2 O and 0.6 mol sodium citrate
(C6 H5 O7 Na3 ·2H2 O) were dissolved in 480 mL distilled water.
The solution was kept at 80 ◦ C in a water bath. Secondly,
80 mL N2 H4 ·H2 O (80% (v/v)) and 4 mol NaOH were mixed in 180 mL
distilled water. Under vigorous mechanical stirring, the mixture
solution of N2 H4 ·H2 O and NaOH was introduced to the water bath.
After 3 h, FeNi3 nanoparticles were magnetically separated from
the solution and then washed with distilled water and ethanol for
several times. The obtained products were dried at 60 ◦ C for 6 h.

0921-5107/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.mseb.2012.10.027
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226 L.-S. Fu et al. / Materials Science and Engineering B 178 (2013) 225–230
2.2. Synthesis of FeNi3 /ITO composite nanoparticles
FeNi3 /ITO composite nanoparticles were prepared via a sol–gel
process. In(NO3 )3 ·4.5H2 O was dissolved in acetylacetone, and then
the solution was maintained at 80 ◦ C for 8 h. The color of the
solution changes from light yellow to dark reddish-brown. Then
SnCl4 ·5H2 O was diluted with absolute ethanol. The two solutions
were mixed and aged at room temperature for 12 h to form sol. The
molar concentration of indium ion was 0.23 mol/L and the mole
ratios of In:Sn were 50:1, 30:1, 9:1 and 2:1, respectively. 1.2 g FeNi3
nanoparticles were dispersed in 480 mL distilled water by ultra-
sonic treatment for 30 min. Under vigorous mechanical stirring,
the mixture was added with 12 mL sol and 12 mL ammonia sub-
sequently. The products were obtained after 2 h, then washed with
distilled water and ethanol for several times and dried at 60 ◦ C for
6 h. The dried products were annealed at 500 ◦ C for 3 h in Ar atmo-
sphere in a tubular furnace. The FeNi3 /ITO composite nanoparticles
prepared with different sols were named in turn as R50, R30, R9 and
R2, respectively.
2.3. Characterization
The phase contents and crystal structure of products were ana-
lyzed by X-ray diffraction (XRD, Rigaku D/max-␥B, Cu K␣ ). The
morphology of products was observed on a scanning electron
microscope (SEM, FEI Quanta 200F) and a transmission electron
microscope (TEM, Philips Tecnai 20). The elemental composition
of products was identified by energy disperse X-ray spectrome-
try (EDS) attached to SEM. The electrical conductivity of pressed
bulk specimen was measured using a four-probe technique at room
temperature.
The infrared emissivity value of products at the wavelength of
8–14 ␮m was measured using IR-2 Infrared Emissometer (Shanghai
Institute of Technological Physics, Chinese Academy of Sciences).
All values were obtained by averaging over the data measured from
Fig. 1. SEM images of FeNi3 nanoparticles (a) and FeNi3 /ITO composite nanoparticles (b). TEM images of FeNi3 nanoparticles (c) and FeNi3 /ITO composite nanoparticles (d).
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six different regions of each coating (the maximum and minimum
data were removed before averaging).
The electromagnetic parameters of the composites containing
products and paraffin were measured on a vector network ana-
lyzer (VNA, Agilent N5230A) using transmission/reflection mode
in the 2–18 GHz band. 70 wt.% products and 30 wt.% paraffin were
mixed thoroughly to obtain a random distribution. The mixture was
pressed into a mold to fabricate VNA specimens. The VNA spec-
imens are coaxial toroidals with outer diameter of 7 mm, inner
diameter of 3.04 mm, and thickness of 3–3.5 mm. EMA performance
of the coatings containing products as fillers can be calculated from
the measured electromagnetic parameters according to the trans-
mission line theory [20],
  1/2   2fd  
r
Zin = Z0 × tan h j (r εr )1/2 (1)
εr c
 
 Zin − Z0 
RL = 20 lg   (2)
Z +Z
in 0
where r is the complex permeability, εr is the complex permittiv-
ity, f is the frequency of electromagnetic wave, d is the thickness of
the coating, c is the velocity of light in free space, Z0 is the impedance
of free space, and Zin is the input impedance of the absorber.
3. Results and discussion
SEM images of FeNi3 nanoparticles and FeNi3 /ITO compos-
ite nanoparticles are shown in Fig. 1a and b, respectively. FeNi3
nanoparticles have an average diameter of about 270 nm. The sur-
face of FeNi3 /ITO composite nanoparticles is rougher than that of
FeNi3 nanoparticles due to the ITO coating. TEM image of FeNi3
nanoparticles is shown in Fig. 1c. ITO phase are distributed among
FeNi3 nanoparticles in the form of small particles in FeNi3 /ITO
composite nanoparticles, as shown in Fig. 1d. The size of ITO
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L.-S. Fu et al. / Materials Science and Engineering B 178 (2013) 225–230 227

800

Electrical conductivity (S/cm)

FeNi3
ITO 600
Intensity (a.u.)

400

(b)
200

(a)
0
20 30 40 50 60 70 80 90 R50 R30 R9 R2

2θ (º) Fig. 4. Electrical conductivity of FeNi3 /ITO composite nanoparticles prepared by sols
with different In:Sn ratios.
Fig. 2. XRD patterns of FeNi3 nanoparticles (a) and FeNi3 /ITO composite nanopar-
ticles (b).
Table 1, as shown in Fig. 3. As shown in Fig. 3a, the total content
of In and Sn elements first increases and then decreases with the
Table 1
EDS results of FeNi3 /ITO composite nanoparticles prepared by sols with different decrease of mole ratio of In:Sn in sols, indicating that the content of
In:Sn ratios. ITO phase in FeNi3 /ITO composite nanoparticles first increases and
then decreases with the decrease of In:Sn mole ratio of sol. The con-
Elements R50 R30 R9 R2
tent of ITO is the largest when the mole ratio of In:Sn in sol is 9:1.
wt.% at.% wt.% at.% wt.% at.% wt.% at.% It can be seen that In:Sn ratios in FeNi3 /ITO composite nanopar-
O 2.20 7.79 1.54 5.52 2.74 10.07 4.05 13.98 ticles decreases with the decrease of mole ratio of In:Sn in sol in
In 6.26 3.09 6.50 3.26 15.52 7.94 5.16 2.48 Fig. 3b, which indicates that the mole ratio of In:Sn of ITO phase
Sn 0.28 0.13 0.35 0.17 1.42 0.70 5.64 2.62 in FeNi3 /ITO composite nanoparticles decreases with the decrease
Fe 21.46 21.74 21.30 21.99 17.76 18.68 18.89 18.66
Ni 69.79 67.25 70.31 69.06 62.56 62.61 66.26 62.27
of In:Sn mole ratio of sol. It is noticeable that the mole ratios of
In:Sn in ITO phase are different from those in corresponding sols.
This may be related to different hydrolysis and condensation rates
nanoparticles is about 10–20 nm. It may be just a simple contact of indium and tin of different sols in sol–gel process.
between FeNi3 and ITO phase without conversion zone. The electrical conductivity of FeNi3 /ITO composite nanoparti-
XRD patterns of FeNi3 nanoparticles and FeNi3 /ITO composite cles prepared with different sols is shown in Fig. 4. It can be seen
nanoparticles are shown in Fig. 2. The obtained FeNi3 nanoparti- that the electrical conductivity of FeNi3 /ITO composite nanoparti-
cles are a solid solution phase with a face-centered cubic structure cles first decreases and then increases with the decrease of mole
(JCPDS 04-0850). The average grain size of FeNi3 nanoparticles ratio of In:Sn in sols. The electrical conductivity of samples R50,
was calculated from full width at half maximum (FWHM) of the R30, R9 and R2 is 601, 473, 211 and 707 S/cm, respectively. It is
strongest XRD peak (3 1 1) using the Debye–Scherrer formula. noticeable that the electrical conductivity of FeNi3 is 1622 S/cm,
The calculated result shows that the average grain size of FeNi3 which is higher than that of all FeNi3 /ITO composite nanoparti-
nanoparticles is about 8.8 nm. It can be seen that XRD peaks of cles prepared in this paper. Therefore, the electrical conductivity of
FeNi3 /ITO composite nanoparticles match those of FeNi3 (JCPDS 04- FeNi3 /ITO composite nanoparticles is mainly related to ITO phase.
0850) and In2 O3 (JCPDS 06-0416). The XRD analysis shows that Sn It can be found that the more the content of ITO phase is, the lower
element is completely soluted into the In2 O3 lattice and no other the electrical conductivity of FeNi3 /ITO composite nanoparticles is,
phase containing Sn element is observed. as shown in Figs. 3a and 4. So the content of ITO phase is the main
The EDS analysis shows that FeNi3 /ITO composite nanoparti- controlling factor in electrical conductivity of FeNi3 /ITO compos-
cles contain iron, nickel, indium, tin and oxygen elements. The EDS ite nanoparticles. It is known that the electrical conductivity of ITO
results of R50, R30, R9 and R2 are shown in Table 1. The total con- phase first increases and then decreases with the decrease of In/Sn
tent (wt.%) of In and Sn elements and In:Sn ratios (at.%) in FeNi3 /ITO ratio [25]. When Sn4+ to In3+ ratio increases, the free carrier concen-
composite nanoparticles were obtained by calculating the data in tration increases, resulting increase of the electrical conductivity.

20
(a) 25 (b)
16
Total content (wt.%)

20
In:Sn ratios

12
15

8
10

4 5

0 0
R50 R30 R9 R2 R50 R30 R9 R2

Fig. 3. The total content (wt.%) of In and Sn elements (a) and In:Sn ratios (at.%) (b) in FeNi3 /ITO composite nanoparticles prepared by sols with different In:Sn ratios.
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228
1.0
Infrared emissivity
0.9
0.8
0.7
0.6
R50 R30
Fig. 5. Infrared emissivity of FeNi3 /ITO composite nanoparticles prepared by sols
with different In:Sn ratios.
When Sn4+ to In3+ ratio increases further, the electrical conductivity
decreases. This is because doping ion itself is a kind of lattice defect
which has strong scattering effect to electron. Excessive doping ions
can affect the mobility of electrons and cause the lattice distor-
tion, so that the electrical conductivity decreases [25]. The role of
In/Sn ratio on the electrical conductivity of FeNi3 /ITO composite
nanoparticles and that of the content of ITO phase is the opposite
with the decrease of mole ratio of In:Sn in sols. However, the role
of the content of ITO phase is larger than that of In/Sn ratio, that is,
the role of the content of ITO phase on the electrical conductivity
just weakens but does not reverse.
Fig. 5 shows the infrared emissivity of FeNi3 /ITO composite
nanoparticles prepared with different sols. The infrared emissiv-
ity of FeNi3 /ITO composite nanoparticles first decreases and then
increases with the decrease of mole ratio of In:Sn in sols. The
infrared emissivity of R50, R30, R9 and R2 is 0.952, 0.870, 0.802 and
0.895, respectively. Obviously, the infrared emissivity of FeNi3 /ITO
composite nanoparticles is the lowest when the mole ratio of In:Sn
in sol is 9:1. In addition, the infrared emissivity of all FeNi3 /ITO
composite nanoparticles prepared in this study is lower than that of
FeNi3 nanoparticles (0.958). It can be found that the more the con-
tent of ITO phase is, the lower the infrared emissivity of FeNi3 /ITO
composite nanoparticles is, as shown in Figs. 3a and 5. More-
over, ITO is a kind of semiconductor with low infrared emissivity.
Thus, the content of ITO phase is also the main controlling factor
in infrared emissivity of FeNi3 /ITO composite nanoparticles. It is
known that the infrared emissivity of ITO phase first decreases and
then increases with the decrease of In/Sn ratio [26]. The reason
28 (a) R50
R9
24
Complex permittivity
20
16
12
8
4
0
0 2 4 6 8 10
Frequency (GHz)
Fig. 6. Complex permittivity (a) and complex permeability (b) of composite specimens containing FeNi3 /ITO composite nanoparticles prepared by sols with different In:Sn
ratios.
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L.-S. Fu et al. / Materials Science and Engineering B 178 (2013) 225–230
is that semiconductor carrier concentration changes with the
decrease of In/Sn ratio [26]. The role of In/Sn ratio on IR emissivity
of FeNi3 /ITO composite nanoparticles and that of the content of ITO
phase is the same with the decrease of mole ratio of In:Sn in sols.
The complex permittivity of the composite specimens contain-
ing FeNi3 /ITO composite nanoparticles prepared with different sols
as fillers is shown in Fig. 6a. The real part (ε ) and imaginary part
(ε ) of complex permittivity of FeNi3 /ITO composite nanoparti-
cles based specimens both first decrease and then increase with
the decrease of mole ratio of In:Sn in sol. It can be observed that
the higher the electrical conductivity, the higher the permittivity
of FeNi3 /ITO composite nanoparticles, as shown in Figs. 5 and 6a.
The dielectric properties in microwave frequency range are mainly
determined by the movement of free charges at the interfaces
R9 R2 between the filler and insulating matrix. The increase in electri-
cal conductivity can intensify the interface polarization that brings
about the high permittivity [20]. As shown in Fig. 6a, obvious
dielectric relaxation can be observed in all FeNi3 /ITO composite
nanoparticles based specimens in this study, which is related to
interfacial polarization.
Fig. 6b shows the complex permeability of the composite speci-
mens containing FeNi3 /ITO composite nanoparticles prepared with
different sols as fillers. No obvious changes can be observed in
FeNi3 /ITO composite nanoparticles with the decrease of mole ratio
of In:Sn in sol. The real part of permeability ( ) of FeNi3 /ITO com-
posite nanoparticles based specimen decreases quickly from 2.0
to 1.2 in the 2–7 GHz, levels off at 1.2 in the 7–12 GHz, and then
decreases slowly from 1.2 to 0.8 in the 12–18 GHz with the increase
of measuring frequency. The imaginary part of permeability ( )
of Fe microflakes based specimen decreases from 0.6 to 0 in the
2–18 GHz band.
EMA performance of the coatings containing FeNi3 /ITO com-
posite nanoparticles as fillers was evaluated by calculating the
reflection loss (RL) according to transmission line theory, as shown
in Fig. 7. A maximum reflection loss (RLmax ) of −73.6 dB was
obtained at 6.2 GHz with a thickness of 2.92 mm for the paraffin
composites containing R30 as fillers, as shown in Fig. 7b. For sam-
ples containing R9 as fillers, the RLmax of −64.2 dB was observed
at the frequency 6.56 GHz with matching thickness of 3.04 mm,
which can be seen in Fig. 7c. However, Fig. 7a and d shows that
the RLmax of only −14.9 dB and −15.3 dB was found at the frequency
2.19 GHz and 2.29 GHz with the thicker matching thickness of 5 mm
for composites containing R50 and R2, respectively. An effective
EMA band (RL < −10 dB) covering frequency range of 10.2–18 GHz
with bandwidth of 7.8 GHz can be achieved in a coating containing
R30 with a thickness of 1.71 mm, as shown in Fig. 7b. For com-
posites containing R9 as fillers, an effective EMA band covering
ε', ε" R30 ε ', ε" (b) R50 ε ', ε" R30 ε ', ε"
ε ', ε" R2 ε ', ε" ε ', ε" R2 ε ', ε"
2.0 R9
Complex permeability
1.6
1.2
0.8
0.4
0.0
12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 20
Frequency (GHz)
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L.-S. Fu et al. / Materials Science and Engineering B 178 (2013) 225–230 229

Fig. 7. Calculated EMA performance of the coating containing 70 wt.% FeNi3 /ITO composite nanoparticles prepared by sols with different In:Sn ratios as fillers with different
coating thicknesses. (a) R50; (b) R30; (c) R9; (d) R2.

Table 2
EMA performance of FeNi3 /ITO nanoparticles–paraffin composites and other reported composites.

Sample Maximal RL value (dB) d (mm) (RL < −10 dB) Bandwidth (RL < −10 dB) Maximal RL fm (GHz) Reference

FeCo/Al2 O3 −30.8 1.2–4 5.5–17 11.4 [27]

Ni/polyaniline −22 2–6 4.2–18 5 [28]
Fe/Fe3 B/Y2 O3 −33 3–6 2.2–8 4.5 [29]
Fe/ZnO −57.1 1.5–5 5.9–18 7.8 [3]
R50 −14.9 2.05–5 2.19–6.98 2.19 Present work
R30 −73.6 1.28–5 3.24–16.63 6.2 Present work
R9 −64.2 1.34–5 3.55–16.87 6.56 Present work
R2 −15.3 0.96–5 2.29–18 2.29 Present work

a frequency range of 10.8–18 GHz with bandwidth of 7.2 GHz can
be achieved with a thickness of 1.73 mm, which can be seen
in Fig. 7c. Nevertheless, as can be seen in Fig. 7a and d, nar-
rower effective EMA bandwidth of 0.8 GHz and 3.5 GHz at the
frequency ranges of 2.6–3.4 GHz and 14.5–18 GHz can be achieved
with thickness of 3.87 mm and 1.08 mm for the samples containing
R50 and R2 as fillers, respectively. In addition, the RL values less
than −10 dB were observed in the 2.19–6.98 GHz, 3.24–16.63 GHz,
3.55–16.87 GHz and 2.29–18 GHz with the thickness of 2.05–5 mm,
1.28–5 mm, 1.34–5 mm and 0.96–5 mm for composites contain-
ing R50, R30, R9 and R2 as fillers. The effective absorption band
locates at S-band (2–4 GHz) for R50, C-band (4–8 GHz) and X-band
(8–12.4 GHz) for R30 and R9, and S-band, C-band, X-band and Ku -
band (12.4–18 GHz) for R2. It can be seen that the content of ITO
phase in FeNi3 /ITO composite nanoparticles significantly influences
the intensity and the location of effective band. The EMA per-
formance of some recently reported composite nanoparticles are
summarized in Table 2. It is noting that R30 and R9 exhibit higher
RLmax and broader bandwidth of effective absorption with thinner
absorber matching thickness.
4. Conclusions
FeNi3 /ITO composite nanoparticles were prepared through a
sol–gel process on precursory FeNi3 nanoparticles. The content of
ITO is the largest when the mole ratio of In:Sn in sol is 9:1. The elec-
trical conductivity and infrared emissivity of FeNi3 /ITO composite
nanoparticles can be mainly controlled by the content of ITO phase.
The infrared emissivity of FeNi3 /ITO composite nanoparticles is
the lowest when the mole ratio of In:Sn in sol is 9:1. Further-
more, the permittivity of FeNi3 /ITO composite nanoparticles in
microwave band can be controlled by the electrical conductiv-
ity. In addition, a significant effect of the content of ITO phase
was observed on the EMA performance of FeNi3 /ITO composite
nanoparticles, such as the intensity and the location of effective
band. The effective absorption band locates at S-band for R50, S-
and X-bands for R30 and R9, and S-, X-, C- and Ku -bands for R2.
When the mole ratio of In:Sn in sol is 9:1, FeNi3 /ITO composite
nanoparticles possess both the lowest infrared emissivity and supe-
rior EMA performance, which is suitable for both infrared and radar
camouflage.
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230 L.-S. Fu et al. / Materials Science and Engineering B 178 (2013) 225–230

Acknowledgements
This work was financially supported by Program of Excellent
Team at Harbin Institute of Technology. L.S. Fu thanks Dr. Yong
Yang and Prof. Yuming Zhou at Southeast University for help with
infrared emissivity measurements.
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