Thin Solid Films 583 (2015) 158162

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Thin Solid Films

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

Structural and electrical properties of Au lms sputter-deposited on

HCl-doped polyaniline substrates
Rongying Huang, Yang Cao, Hong Qiu
Department of Physics, School of Mathematics and Physics, University of Science and Technology Beijing, 30 Xueyuanlu, Haidian District, Beijing 100083, China

a r t i c l e

i n f o

Article history:
Received 28 July 2014
Received in revised form 8 December 2014
Accepted 30 March 2015
Available online 6 April 2015
Keywords:
Au lm
HCl-doped polyaniline
Composite
Sputtering
Electrical property

a b s t r a c t
Au lms with a thickness of 14180 nm were sputter-deposited on HCl-doped polyaniline (HCl-PANI) substrates
at 300 K, forming the Au/HCl-PANI composites. The sputter-deposition is discontinuous in order to prevent from
heating the substrate during the deposition. The 14 nm- and 28 nm-thick Au lms have a network structure. The
Au lms with a thickness of 50180 nm have a continuous structure and consist of granular grains. A temperature
dependence of the resistance within 6280 K reveals the complex behavior of the Au/HCl-PANI composite as follows: (1) The composite with the 14 nm-thick Au lm shows the semiconducting behavior. (2) The composite
with the 28 nm-thick Au lm exhibits the metalsemiconductor transition with increasing temperature,
i.e., the composite shows the metallic conduction behavior at temperatures below the transition temperature
and the semiconducting behavior at temperatures over the transition temperature. (3) As the Au lm thickness
reaches and exceeds 50 nm, the composites only exhibit the metallic conduction behavior.
2015 Elsevier B.V. All rights reserved.

1. Introduction
The polymer nanocomposites containing metal nanoparticles were
mostly studied because of their functional applications [1]. Particularly,
the noble metal (Au and Ag) lms grown on polymers have attracted
considerable attention for their potential applications in functional devices, e.g., references [29]. Rufno et al. [2] sputter-deposited Au
lms on polystyrene (PS) and polymethylmethacrylate (PMMA) substrates. They observed that the Au lm evolved from hemispherical
islands to partially coalesced worm-like island, to percolation, and nally to a continuous and rough lm, with increasing deposition time. Furthermore, they annealed the Au and Ag thin lms grown on the PS and
PMMA substrates at temperatures over the glass transition temperature
of the polymer. They found the embedding of the Au and Ag nanoparticles in the PS and PMMA during annealing and obtained the activation
energy for the embedding process [3]. Kaune et al. [4] studied the
growth of the Au lm on the conducting polymer surface and suggested
the growth model. Takele et al. [5] prepared Teon- and Nylon-based
nanocomposite lms consisting of Au and Ag nanoparticles by coevaporating the metal and the polymer. They found that the resistivity
percolation thresholds were 0.42 and 0.32 for Teon- and Nylonbased nanocomposite lms, respectively. Torrisi et al. [6] deposited
Au/polymer multilayers on p-Si substrates to prepare the Schottky device. They found that the Schottky barrier height could be controlled
by the Au/polymer bilayer number. Rufno et al. [7] sputter-deposited
the Au micro-size square patterns on the PMMA layer by xing Cu
Corresponding author. Tel.: +86 10 62333786; fax: +86 10 62332993.
E-mail address: qiuhong@sas.ustb.edu.cn (H. Qiu).

http://dx.doi.org/10.1016/j.tsf.2015.03.069
0040-6090/ 2015 Elsevier B.V. All rights reserved.

grid template on the PMMA surface. Some peculiar patterns of Au

were easily obtained by annealing because of the thermal-drivendewetting of the PMMA layer. The micro-patterns of Au lms can be applied to device applications.
Recently, Ni lms with a thickness of 45240 nm were sputterdeposited on HCl-doped polyaniline (HCl-PANI) substrates at 300 K,
forming the Ni/HCl-PANI composites. A temperature dependence of
the resistance (RT) within 5300 K revealed that all the Ni/HCl-PANI
composites exhibited the metalsemiconductor transition. The composite showed the metallic conduction behavior at temperatures
below the transition temperature and the semiconducting behavior at
temperatures over the transition temperature [10]. The parallel resistor
model was used to explain the metalsemiconductor transition of the
Ni/HCl-PANI composites [10,11]. Au has a high electrical conductivity
compared with Ni. Whether dose the Au/HCl-PANI composite have
the metalsemiconductor transition? Is the RT relationship of the Au/
HCl-PANI composite different from that of the Ni/HCl-PANI composite?
The answers to these questions are valuable and signicant for the fundamental viewpoint.
Polyaniline (PANI) is an important conducting polymer because of
its good environmental stability, low cost, ease of preparation and
high conductivity. Au is a noble metal widely used due to its high stability and high electrical conductivity. Au lms or Au nanoparticles grown
on PANI, forming the Au/PANI composite materials, have attracted considerable attention for their potential applications in catalyst, electronic
devices and sensors, e.g., references [1216]. As reported previously
[1216], the Au/PANI composites were prepared by the chemical
methods and their catalytic activities were mainly studied. On the
other hand, sputter deposition is the usual method to prepare thin

R. Huang et al. / Thin Solid Films 583 (2015) 158162

lms because it can easily control the composition, structure and physical property of the lms as well as can enhance the adhesion of the lm
to the substrate. Besides, the sputtered atoms have the high energy
when they arrive at the substrate surface or the growing lm surface.
These energetic adatoms can improve the structure of the lm
sputter-deposited at room temperature. Room temperature deposition
can eliminate the thermal stress in the lm and is suitable for the polymer substrates having a low decomposition temperature. Moreover, the
Ni/HCl-PANI composite has been successfully prepared by direct current
magnetron sputtering at room temperature [10]. Thus, in the present
work, Au lms are sputter-deposited on HCl-PANI substrates, forming
the Au/HCl-PANI composites. Structural and electrical properties of
the Au/HCl-PANI composites are studied as a function of the Au lm
thickness.
2. Experimental procedure
All the chemical reagents were purchased from Beijing Chemical
Works and were of analytical grade. Only aniline was doubly distilled
under reduced pressure and stored in refrigerator (at about 4 C) prior
to using. The other chemical reagents were used without further purication. HCl-PANI was chemically synthesized using the well-established
polymerization procedure [17]. The polymerization procedure is summarized as follows: (1) Aniline (0.1 mol) was dissolved in 100 mL aqueous hydrochloric acid (HCl, 1 mol/L) taken in a three-neck ask. The
mixture solution was cooled and stirred at 3 C by a magnetic stirrer.
(2) 51.5 mL ammonium persulfate solution (2.4 mol/L) in a constant
pressure funnel was slowly added into the mixture solution for 1 h in
order to avoid heating the reaction mixture. The reaction proceeded at
3 C for 8 h. (3) The nal solution was ltered. (4) The protonated
precipitate was washed with deionized water, acetone and ethanol
until the washing water, acetone and ethanol became colorless and
the pH was equal to 7. (5) The powder was dried at 50 C in oven for
two days. The HCl-PANI powder was obtained.
The HCl-PANI powder was compacted to pellets with 0.4 mm in
thickness and 13 mm in diameter. The HCl-PANI pellets were used as
the substrates. Au lms were deposited on the HCl-PANI substrates at
300 K by using a direct current sputtering system SCB-12 (KYKY) [18,
19]. The Au target (99.99% in purity) with 50 mm in diameter faced
the substrate. The distance between the target and the substrate was
40 mm. Prior to deposition, the working chamber was evacuated to a
pressure of 2 Pa by using the rotary pump. The sputtering was started
at an Ar gas (99.9995% in purity) pressure of 4 Pa and the sputtering
power applied to the target was xed at 1000 V 4 mA. The sputterdeposition is discontinuous in order to prevent from heating the substrate during the deposition. After the Au lm was sputter-deposited
for 10 s, the sputtering paused for 10 s and then continued to start.
The 10-second sputter-deposition and the 10-second pause were one
preparation cycle. The Au lm preparation required several cycles to obtain the desired lm thickness. The lm thicknesses ranging from 50 nm
to 180 nm were measured using eld emission scanning electron microscopy. The relationship between the lm thickness d and the deposition time t exhibits a linear dependence having a linear correlation
coefcient of 0.98. The deposition rate, which was obtained from the
dt relationship, was 9.4 nm/min. The lm thicknesses below 50 nm
were obtained by controlling the deposition time. The relative error in
the lm thickness came mainly from the surface roughness of the lm
and was around 10%.
Field emission scanning electron microscopy (FE-SEM) of SUPRA55
(Zeiss) was used to observe the structure of the Au lms. The acceleration voltage of electron beam was 10 kV. The electron beam did not inuence the surface morphology of the Au/HCl-PANI composite during
the FE-SEM observation. X-ray diffraction (XRD) of D/Max-RB (Rigaku)
was used to analyze the structure of the lms. The XRD measurements
were performed in a standard 2 scan using a Cu K radiation ltered
by a crystal monochromator (wavelength = 0.15406 nm). A

159

resistance of the Au/HCl-PANI composite was measured in the temperature range of 6280 K using the Cryogen-Magnet system of CFM-5TH3-CFVTI-1.6K-24.5 with the four-point probe (Cryogenic Inc.).

3. Results and discussion

Fig. 1 shows FE-SEM microphotographs of the 14 nm- and 28 nmthick Au lms sputter-deposited on the HCl-PANI substrates. Fig. 2
shows FE-SEM microphotographs of the 50 nm-, 100 nm- and
180 nm-thick Au lms sputter-deposited on the HCl-PANI substrates.
As can be seen from Figs. 1 and 2, the 14 nm- and 28 nm-thick Au
lms have a network structure while the lms with a thickness of 50
180 nm are continuous. The continuous lms do not consist of columnar
grains, i.e., the lms have a granular grain structure. It is considered that
the granular grain structure is attributed to the discontinuous sputterdeposition. Furthermore, the grain size increases with increasing lm
thickness. Rufno et al. [2] reported that the Au lm sputter-deposited
on the PS and PMMA substrates evolved from hemispherical islands to
partially coalesced worm-like island, to percolation, and nally to a continuous and rough lm, with increasing deposition time. Now, it is considered that the growth of the Au lm on the HCl-PANI substrate could
be also explained by the Au growth model reported by Rufno et al. [2].
Fig. 3 shows XRD pattern of the 50 nm-thick Au lm sputterdeposited on the HCl-PANI substrate. As shown in Fig. 3, only diffraction
peaks of Au are observed except for the diffraction peaks of the HClPANI substrate. A lattice constant of the Au lm is calculated by the
diffraction peak of Au(111). The lattice constant of the Au lm is

200nm

b
Fig. 1. FE-SEM microphotographs of the Au lms sputter-deposited on the HCl-PANI substrates; (a) 14 nm-thick lm and (b) 28 nm-thick lm.

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R. Huang et al. / Thin Solid Films 583 (2015) 158162

200nm

100nm

100nm

200nm

Fig. 2. FE-SEM microphotographs of the Au lms sputter-deposited on the HCl-PANI substrates; (a, b) 50 nm-thick lm, (c, d) 100 nm-thick lm, and (e, f) 180 nm-thick lm.

600
500

HCl-PANI

I (cps)

400

Au(111)

300
200

Au(200)
Au(220) Au(311)

100
0
10

20

30

40

50

60

70

80

90

2 (deg)
Fig. 3. XRD pattern of the 50 nm-thick Au lm sputter-deposited on the HCl-PANI
substrate.

0.40733 nm, which is almost equal to the lattice constant of the Au bulk
(0.40790 nm).
Fig. 4 shows a temperature dependence of the resistance of the Au/
HCl-PANI composites with different lm thicknesses. In Fig. 4, the resistance R at each temperature is normalized to the resistance R6 at 6 K.
The relative error in the resistance is mainly determined by the accuracy
of current control and voltage measurement and is below 1%. As can be
seen from Fig. 4, only the composite with the 28 nm-thick Au lm exhibits the metalsemiconductor transition with increasing temperature.
The transition temperature is around 70 K. The composite shows the
metallic conduction behavior at temperatures below the transition temperature and the semiconducting behavior at temperatures over the
transition temperature. The composite with the 14 nm-thick Au lm
exhibits the semiconducting behavior whereas the composites with
the 50 nm-, 100 nm- and 180 nm-thick Au lms show the metallic conduction behavior in the temperature range from 6 K to 280 K. A

R. Huang et al. / Thin Solid Films 583 (2015) 158162

1.20
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0.000

1.00
0.80

0.60
0.40

Table 1
The values of the Au lms with a thickness dF of 28180 nm at Tb = 10 K.

14nm Au

dF (nm)
104 (K1)

0.20

50

100 150 200 250 300 350

0.00
0

50

100

150

200

250

300

161

350

1.10

28
7.1

50
8.1

100
8.5

180
9.2

where F is the resistivity of the Au lm, S is the resistivity of the HClPANI substrate, dF is the Au lm thickness and dS is the HCl-PANI
substrate thickness. A constant value of 3.31 is determined by the
four-point probe instrument. As it is well known, a temperaturedependence of resistivity of the metallic lm is linear and can be
expressed as
F b  1  TTb 

28nm Au

R/R6

0.88
where b is a reference resistivity of the lm at a reference temperature
Tb. is a temperature coefcient of resistance of the lm, also related to
Tb. T is a temperature. On the other hand, for the HCl-PANI substrate, the
carrier transport mechanism is three-dimensional variable range
hopping and a temperature-dependence of resistivity follows the
relation [2022]

0.66
1.03
1.02

0.44

1.01
1.00

0.22

0.99
0

20

40

60

80

0.00
0

50

100

150

1.80

200

250

300

350

180nm Au

"
1 #
T0 =4
S 0 exp
T

where T0 is the Mott characteristic temperature and 0 is the resistivity

at T = . According to Eqs. (3) and (4), Eq. (2) can be written as [11]

1.60

100nm Au
1.40

RC

50nm Au

1.20

b  1  TTb   0 exp

 1 
T0 =4
T


 1  :
=
3:31  dS  b  1  TTb  d F  0 exp TT0 4
5

1.00

50

100

150

200

250

300

350

T (K)
Fig. 4. Temperature dependence of the resistance of the Au/HCl-PANI composites. The
arrow represents the transition temperature.

temperature coefcient of resistance (TCR) increases with increasing

lm thickness in the temperature range of the metallic conduction.
For the composite with the 14 nm-thick Au lm, the Au lm has the
network structure and the network connect is broken in some regions
as shown in Fig. 1a. Therefore, the temperature dependence of the resistance of the Au/HCl-PANI composite with the 14 nm-thick Au lm could
be dominated by the HCl-PANI substrate, i.e., the resistance of the composite decreases with increasing temperature and it is similar to a semiconductor [2022].
For the composites with the Au lms thicker than 14 nm, the simple
parallel resistor model is used to analyze the resistancetemperature
(RT) characteristic of the composite within 6280 K [10,11]. Both the
Au lm and the HCl-PANI substrate are conductive. Thus the resistor
of the Au/HCl-PANI composite is a parallel of the two resistors of the
Au lm and the HCl-PANI substrate. The resistance RC of the composite
is expressed as [10,11]
RC

R F  RS
R F RS

where RF and RS are the resistance of the Au lm and the resistance of

the HCl-PANI substrate, respectively. Eq. (1) can be written as
RC

F  S
3:31  dS  F d F  S

As shown in Eq. (5), the resistance of the Au/HCl-PANI composite is a

function of the temperature.
Based on the experimental results, T0 = 5.93 106 K, 0 =
8.22 106 cm [22]. The HCl-PANI substrate thickness dS is equal
to 0.4 mm. The reference temperature Tb is 10 K. The resistivity b of
the Au lm is estimated to be 1 105 cm. The values of the Au
lms with a lm thickness dF of 28180 nm are summarized in
Table 1 [23]. According to Eq. (5) and the parameters mentioned
above, the calculated RT characteristic of the Au/HCl-PANI composite
can be obtained within 10280 K. Fig. 5 shows the calculated RT relationship of the Au/HCl-PANI composite in which the Au lm has a thickness of 28180 nm. In Fig. 5, the resistance RC at each temperature is
normalized to the resistance RC10 at 10 K. As can be seen from Fig. 5,
the composite with the 28 nm-thick Au lm exhibits markedly the
metalsemiconductor transition whereas the composites with the

1.40
1.30

RC/RC10

0.80

180nm Au
100nm Au
50nm Au

1.20
1.10

28nm Au
1.00
0.90

100

200

300

400

T (K)
Fig. 5. Calculated RT relationship of the Au/HCl-PANI composites with a Au lm thickness
of 28180 nm. The arrow represents the transition temperature.

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R. Huang et al. / Thin Solid Films 583 (2015) 158162

50 nm-, 100 nm- and 180 nm-thick Au lms show the metallic conduction behavior. The calculated RT relationship is in qualitative agreement with the experimental RT relationship. Thus it is considered
that the simple parallel resistor model could be used to qualitatively
explain the temperature dependence of the resistance for the Au/HClPANI composites. The difference between the experimental RT relationship and the calculated RT relationship could be attributed to
these two facts: (1) the parameters used in Eq. (5) is inaccurate,
and (2) the current does not distribute throughout the thickness
of the lm/substrate sample during the RT measurement [24]. For
example, the and b values are related to the lm preparation condition. Therefore, these parameters used in Eq. (5) are different from the
practical parameters of the Au lms prepared in this work, resulting in
the difference between the calculated resistance and the measured
resistance.
As shown in Fig. 4, the TCR value increases with increasing lm
thickness in the temperature range of the metallic conduction. The
TCR of the metallic lm can be given by [25]

c  0
c v i g

where c is the resistivity of bulk material at a reference temperature

Tm. 0 is the TCR of bulk material, also referred to Tm. v, i and g are
the temperature-independent resistivities caused by vacancies, impurities and grain boundaries in the lm, respectively. In the present work, it
is considered that the i and v are same for all the Au lms because the
background pressure, Ar gas pressure, deposition temperature and deposition rate are same during the deposition. On the other hand, the
grain size increases with increasing lm thickness as shown in Figs. 1
and 2. As a result, the g value decreases with increasing lm thickness.
According to Eq. (6), the TCR value increases with increasing lm
thickness.
For the metal-lm/HCl-PANI composite, we dene the maximal
transition thickness as the lm thickness over that the metalsemiconductor transition of the composite will disappear, i.e., the composite
only exhibits the metallic conduction behavior with increasing temperature. Moreover, we dene the transition thickness range as the lm
thickness range in which the composite shows the metalsemiconductor transition with increasing temperature. In comparison with Refs.
[10,11], the maximal transition thickness of the Au/HCl-PANI composite
is thinner than that of the Ni/HCl-PANI composite and the transition
thickness range of the Au/HCl-PANI composite is narrower than that
of the Ni/HCl-PANI composite. It should be attributed to the fact that
the conductivity of Au is larger than that of Ni. According to the parallel
resistor model [10,11], only when the resistance of the metal lm
matches the resistance of the HCl-PANI substrate, the current can ow
the lm and the substrate, leading to the metalsemiconductor transition behavior of the composite. For the Au and Ni lms, when they
have the same resistance, the thickness of the Au lm is thinner than
that of the Ni lm. As a result, the maximal transition thickness of the
Au/HCl-PANI composite is thinner than that of the Ni/HCl-PANI composite. For both the Au/HCl-PANI and Ni/HCl-PANI composites, the current is more limited in the Au lm compared with the Ni lm.
4. Summary
The Au lms with a thickness of 14180 nm were sputter-deposited
on the HCl-PANI substrates at 300 K, forming the Au/HCl-PANI composites. The 14 nm- and 28 nm-thick Au lms have the network structure.
The lms with a thickness of 50180 nm are continuous and have the
granular grain structure. The temperature dependence of the resistance
within 6280 K reveals the complex behavior of the Au/HCl-PANI
composites. The composite with the 14 nm-thick Au lm shows the
semiconducting behavior. The composite with the 28 nm-thick Au
lm exhibits the metalsemiconductor transition with increasing

temperature. As the Au lm thickness reaches and exceeds 50 nm, the

composites only exhibits the metallic conduction behavior. The parallel
resistor model could be used to explain the RT relationship of the
composites.

Acknowledgment
The authors would like to thank Prof. J. P. He of the State Key Laboratory for Advanced Metals and Materials for FE-SEM observations. The nancial support from the Fundamental Research Funds for the Central
Universities No. 8220 is gratefully acknowledged.

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