Applied Surface Science 385 (2016) 28–33

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Applied Surface Science

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

Tuning the ITO work function by capacitively coupled plasma and its
application in inverted organic solar cells
Ming Fang a , Chunmei Zhang a,∗ , Qiang Chen a,b
a
Laboratory of Plasma Physics and Materials, Beijing Institute of Graphic Communication, Beijing, China
b
State Key Laboratory of Electrical Insulation and Power Equipment, Xi’an Jiaotong University, Xi’an, China

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

Article history: In this paper, we investigated the performance of inverted organic solar cells (OSCs) with plasma-treated
Received 17 November 2015 indium tin oxide (ITO) as the cathode for omitting an electron transport layer. The Ar plasma was produced
Received in revised form 13 May 2016 by capcitively coupled plasma setup under 20 Pa chamber pressure. For the device with the structure of
Accepted 14 May 2016
plasma-treated ITO/P3HT:PCBM/MoO3 /Ag, a power conversion efficiency (PCE) of 3.22% was achieved,
Available online 17 May 2016
whereas PCE of 1.13% was recorded from the device fabricated with the pristine ITO. The photovoltaic
performance was found to be dependent on the applied power of plasma. After analyzing by atomic
Keywords:
force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS), we concluded that the chemical
Organic solar cells
Plasma treatment
component variation of ITOs surface resulted in the decrease of ITO work function, which meant that the
Electron transport layer ITO Fermi level became shallow relative to the vacuum level. The low work function of ITO should be
ITO responsible for the improvement of inverted OSCs because of the better energy level alignment between
ITO and the photoactive layer.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction
Organic solar cells (OSCs) are being rapidly developed due
to its substantial advantages such as flexible substrates, light
weight, large area fabrication process and low-cost potential [1–6].
Recently, the bulk heterojunction organic solar cells with the con-
ventional structure have achieved high power conversion efficiency
[7]. However, the cathode with a low work function is easily oxi-
dized after the exposure in the air [8], which blocks the wide
application of OSCs. Additionally, the indium tin oxide (ITO) as
the anode can be corroded by hole transport layer, like poly (3,4
ethylenedioxylenethiophene): poly(styrene sulfonic acid) (PEDOT:
PSS) which shortens the lifetime of the device [9–11]. After adopt-
ing inverted device structure using ITO as cathode [12], the devices
demonstrate more stable properties compared to the conventional
solar cells. Unfortunately, the high work function of ITO cathode is
not suitable for electron collection in the inverted devices, espe-
cially for the cell based on the blend of poly (3-hexylthiophene)
(P3HT) as an electron donor and [6,6]-phenyl C61 butyric acid
methyl ester (PCBM) as an electron acceptor. In the inverted solar
cells, ITO is used as cathode to collect electrons. The work func-
∗ Corresponding author.
E-mail address: zhangchunmei@bigc.edu.cn (C. Zhang).
tion difference between the anode and the cathode is associated
with the built-in potential Vbi over the active layer (eVbi = Фanode −
Фcathode ). When 0 < V < Vbi (in the fourth quadrant of J-V curve, V is
the applied voltage), internal electric potential provides the driving
force for charge extraction. Then, either a decrease in the magni-
tude of ITO work function Фcathode or an increase in the magnitude
of anode work function Фanode can provide a bigger Vbi , which is
beneficial for the electron collection [13,14]. Moreover, the LUMO
level of PCBM (the acceptor in the active layer) is about −4.3 eV.
The low work function ITO can favor the Ohmic contact between
the cathode and PCBM. The electron injection barrier at the cath-
ode/organic interface can be formed when the value of ITO work
function is much higher than 4.3 eV, which can result in the lim-
ited open voltage and low injection current (in first quadrant of J-V
curve) [14]. Therefore, how to decrease the work function of ITO
for better energy level alignment or to improve the electron col-
lecting efficiency are the challenges for inverted OSCs. Currently,
the available way is to insert an electron transport layer between
ITO and the active layer, such as ZnO [15], TiOx [16], cesium car-
bonate (CsCO3 ) [17], Al2 O3 [18] polyethylene oxide (PEO) [19] and
so on to modify ITO.
In our previous study, using ITO with the low work function fab-
ricated by electron cyclotron resonation (ECR) plasma treatment in
high-vacuum environment, the performance of inverted solar cells
without electron transport layer was significantly improved [20].

http://dx.doi.org/10.1016/j.apsusc.2016.05.077
0169-4332/© 2016 Elsevier B.V. All rights reserved.
 M. Fang et al. / Applied Surface Science 385 (2016) 28–33
Fig. 1. The schematic diagram of plasma setup.
Now we report another way (capacitively coupled plasma (CCP))
to treat ITO surface in low-vacuum environment. Comparing to the
ECR setup, the CCP did not need the expensive vacuum equipment
and had the scalability to larger areas and the possibility of continue
treatment. Ar plasma was introduced to treat ITO for 3 min before
assembling advices. The photovoltaic performance demonstrated
that without an extra electron transport layer between ITO and the
photoactive layer, the 3.22% PCE of the device with the structure
of ITO (Ar plasma-treating)/P3 HT:PCBM/MoO3 /Ag, was recorded.
The mechanism of the photovoltaic performance depending on the
applied power was analyzed in detail.
2. Materials and methods
2.1. Ar plasma treatment
Fig. 1 is the schematic diagram of capacitively coupled plasma
setup. The bottom plate was connected to the power electrode, and
the upper plate was grounded. Prior to plasma treatment, the ITO
films were cleaned in an ultrasonic bath with cleaning solution,
alcohol and deionized water sequentially for 10 min, respectively.
Then the films were dried by nitrogen stream. Those ITO films were
placed on the bottom plate. In the treatment process, first of all,
the vacuum chamber was pumped down to a pressure of ∼5 Pa.
Then the gas (argon) was introduced into the chamber via a mass
flow controller (MFC) up to a pressure of 20 Pa. After the pressure
became stable, the plasma was generated by the 13.56 MHz radio
frequency (RF) power source, and the RF power was applied var-
ied from 100 to 500 W. The time of plasma treatment was 3 min.
After plasma treatment, all samples were stored in ambient envi-
ronment.
2.2. Fabrication of organic solar cells
After exposed under Ar plasma for 3 min, the film was
transferred into a nitrogen atmosphere glove box. A 1,2-
dicholorobenzene (DCB) solution composed of P3HT (17 mg ml−1 ,
Rieke Metals) and PCBM (17 mg ml−1 , Nano-C) was spun onto the
ITO film at 800 rpm for 30 s. Then the samples were baked at 110 ◦ C
for 10 min. Finally, the MoO3 layer (10 nm) and Ag anode (100 nm)
were sequentially deposited onto the active layer by thermal evap-
oration. The area of device was 4.5 mm2 .
29
2.3. Characterization
The atomic force microscopy (AFM, Veeco DI-INNOVA) was
employed to characterize the ITO surface morphology. The
hydrophilicity of ITOs surfaces was investigated by water contact
angle measurement (DSA 100, Germany). The light transmit-
tance was obtained by ultraviolet visible spectrophotometer
(UV-2501PC). The current density-voltage (J-V) characteristics
were gained by a Keithley 4200 source meter under the simulated
light intensity of 100 mW/cm2 (ABET Technologies AM1.5). The
work function of ITO film was measured by Kelvin probe (SKP-5050,
KP Technology Ltd.). The surface chemical composition of pristine
and plasma treated ITO were characterized by X-ray photoelectron
spectroscopy (XPS) using ESCALAB 250 XPS Analysis System with
Al Ka monochromated X-ray source.
3. Results and discussion
Fig. 2(a) shows the self-bias voltage increased along with the
applied RF power. The negative self-bias DC voltage was established
between the RF-powered electrode and the grounded electrode due
to the accumulation of electrons on the RF-powered electrode after
dissociation of the Ar atoms during the plasma process. In our work,
the power electrode connected to the bottom plate was beneficial
to the plasma treatment of ITO because the self-bias voltage accel-
erates the ions with a higher kinetic energy to bombard the ITO
surface. Fig. 2(b) demonstrated that the electron temperature (Te )
varied from 3.5 to 5 eV, which was independent of the RF power.
Meanwhile, the plasma density (Ne ) increased with increasing the
RF power. This result was due to the exponential variation of impact
ionization rate coefficient (Kiz ) with Te which allowed the wide
variation of Kiz for the small variation of Te by particle conserva-
tion based on the Goble Model. The enhanced Kiz resulted in the
higher density of Ne [21].
Fig. 3 showed the AFM images of ITO substrates treated with
Ar plasma under various RF powers for 3 min. The surface of ITO
treated at 200 W showed a similar morphology as the untreated
ITO. When the applied power increased to 500 W, the ITO sur-
face exhibited less smooth. The values of root mean squares (RMS)
roughness of the pristine ITO, plasma-treated ITO at 200 and 500 W
were 1.68, 1.53 and 1.81 nm, respectively. It was known that the
RMS of ITO films could make a direct impact on the contact between
the active layer and the ITO cathode in the polymer solar cells, and
thus influenced the performance of the device [22]. In this work,
30 M. Fang et al. / Applied Surface Science 385 (2016) 28–33

Fig. 2. (a) Variation of bias voltage as a function of RF power; (b) Variation of Te and Ne with RF power.

Fig. 3. AM images of the pristine ITO and treated ITO by Ar plasma for 3 min (a-pristine; b-200W; c-500W, respectively).

the increase roughness at the higher power should have an effect Table 1
The WCA change of ITOs treated by various power plasma versus aging time.
on the performance of the devices.
Fig. 4 shows the transmittance spectra of ITO treated by vari- Storage time (h) 0 8 16 24 48 120
ous RF power. The spectra showed that the transmittance of the
pristine ITO was about 80% over the visible wavelength range.
Pristine ITO <5◦ 10◦ 15.8 17 20◦ 38◦
When the power was less than 200 W, the light transmittance at
100 W, 3 min <5◦ <5◦ <5◦ 5◦ 8◦ 34.4◦
the wavelength range of 360–500 nm was slightly degraded. When 200 W, 3 min <5◦ <5◦ 11◦ 13◦ 13.6◦ 34.6◦
the power increased to 500 W, the transmittance of ITO decreased 300 W, 3 min <5◦ <5◦ 10.7◦ 12◦ 16◦ 34.3◦
in the range of visible wavelength range. A lower transmittance 500 W, 3 min <5◦ <5◦ 30◦ 32◦ 35◦ 35◦
means the less optical absorption of the active layer, resulting in
the decline of short-circuit current (Jsc ) of the device.
Table 1 shows the water contact angle (WCA) of the pristine all the samples were less than 5◦ , which indicated that the surface
and plasma-treated ITO as a function of the aging time. To evalu- was hydrophilic. The ␥lv of DCB is 35.7 mJ/m2 (ambient environ-
ate the dynamic behavior of the contact angle as a function of time ment at 20 ◦ C), which is smaller than that of water (72.7 mJ/m2 ).
elapsed after plasma treatment, the contact angles of the samples Complete wetting occurs when ␥lv ≈ ␥sv or ␥lv <␥sv , where ␥lv is the
were measured at 8, 12, 16, 24, 48 and 120 h after plasma treatment, liquid-vapor interfacial tension and ␥sv is the solid-vapor interfa-
respectively. After plasma treatment, the water contact angles for cial tension [23]. Thus for the same solid substrate, DCB will wet the
surface completely if water can. The contact angle of all the samples
 M. Fang et al. / Applied Surface Science 385 (2016) 28–33 31

Table 4
The work function of ITOs treated at different applied RF plasma power.

Samples Pristine ITO 100 W 200 W 500 W

Work function (eV) 5.1 5.03 4.24 4.26

Table 5
The summary parameters of device fabricated with/without Ar plasma treated ITO
as cathode electrode.

Device Samples Jsc (mA/cm2 ) Voc (V) FF ␩ (%)

Without treatment 8.27 0.36 0.38 1.13

100 W 8.87 0.54 0.50 2.43
200 W 9.04 0.60 0.60 3.22
300 W 8.50 0.60 0.57 2.9
500 W 7.38 0.60 0.65 2.89

increased after Ar plasma treatments, which indicated the increase

of oxygen-deficient concentration [25].
Fig. 4. The transmittance spectra of treated ITO versus the applied power. Table 2 showed that the content of C-contamination decreased
after plasma treatment, especially when the sample was treated at
Table 2
200 W. The C contamination mainly came from the environmen-
Atomic concentration of the different elements (%). tal absorption and the residual detergent, such as ethyl alcohol,
isopropyl-ketone. Normally, the carbon contamination on the sur-
ITOs C O Sn In O/(In + Sn) In/Sn
face could be removed by Ar+ bombardment from ITO surface,
Pristine ITO 59.33 31.91 0.6 8.15 3.65/1 13.58/1 but the pollution in the air and the process of detecting XPS was
100 W 37.71 52.49 0.69 9.11 5.36/1 13.2/1
unavoidable, it was difficult to ablate C from the signals. In Fig. 6(a)
200 W 30.68 51.82 1.27 16.23 2.96/1 12.78/1
500 W 36.95 45.25 1.37 16.43 2.54/1 11.99/1 a small peak at 445.35 eV in In 3d5/2 spectra disappeared after
plasma treatment which was maybe the main reason leading to
the decrease of In element content, and in Fig. 6(b) the full width
Table 3 at half maximum of Sn 3d5/2 core was remarkably decreased along
The deconvolution of core O1s and its ratio. with the applied power. As shown in Table 2, the ratios of In/Sn
ITOs Oi Oii Oiii Oii /Oiii also decreased along the increase of applied power. The increased
Pristine ITO 0.450 0.277 0.273 1.015/1
concentration of oxygen-deficient and doped Sn could enhance
100 W 0.414 0.295 0.291 1.017/1 electron concentration, which may lead to the change of ITO elec-
200 W 0.368 0.329 0.303 1.086/1 trical property.
500 W 0.360 0.334 0.306 1.096/1 Kelvin Probe measurement was employed to detect the work
function of ITO substrate, and the result was shown in Table 4. The
work function of ITO was little reduced after plasma treatment at
increased slowly with increasing aging time. When the RF power 100 W (about 0.07 eV). Then the notable reductions were observed
was 100 W, the WCA value remained around a low value up to 24 h, after plasma-treatment at 200 and 500 W, which were 0.86 and
and then it increased and stabilized at ∼35◦ after 120 h aging. For 0.84 eV, respectively. The work function of ITO decreased after Ar
the samples treated by 200 and 300 W, the changes of WCA were plasma treatment, which was similar to the prior report [20]. As
almost the same which increased step by step from 5◦ to ∼35◦ . For known, the concentrations of oxygen vacancy and doped Sn dom-
the sample treated at 500 W, the WCA began to increase after the inate the carrier concentration [26]. The increase of the oxygen
aging time of 8 h. It was also stable at ∼35◦ 120 h later. Although the vacancy and doped Sn concentration could cause the upward shift
rates of WCA increments were different, the last value was similar. of the Fermi energy of ITO and decreased the work function of ITO.
The instability of the ITO surface was believed to arise from the re- Fig. 7 shows the current density-voltage (J-V) curves of the
organization of the plasma-created polar groups in the surface layer devices with the structure of ITO/P3HT:PCBM/MoO3 /Ag, and the
of the sample and the re-contamination of the surface by hydrocar- values of photovoltaic performance parameters are summarized in
bons in air [24]. Based on our previous work, the change of the WCA Table 5. The photovoltaic performance of assembled device was
has little effect on the performance of the device, and the influence obviously relying on the applied power. The devices with the pris-
of surface wettability on the device could be omitted [20]. tine ITO only exhibited a PCE of 1.13% due to very low open circuit
Since the chemical component of ITO surface may be the voltage (Voc ) and short circuit current density (Jsc ). When the RF
main factor to dominate the electrical characteristic, the XPS was power increased to 200W, it could be seen that Voc , Jsc , fill fac-
employed to analyze the pristine and plasma-treated ITOs. Fig. 5 tor (FF), and PCE all increased and reach to the maximum values
and Fig. 6 showed the core levels spectra of O 1 s, In 3d and Sn 3d, (Voc = 0.6 V, Jsc = 9.04 mA/cm2 , FF = 0.60 and PCE = 3.22%). The effi-
respectively. The corresponding atomic concentration and atomic cient cell performance was mostly because that the work function
ratios are summarized in Table 2. O 1s core level spectra was fitted of ITO was reduced. The low work function of ITO optimized the
based on Gaussian mode with peaks at 532.2 eV (Oi ), 531.2 eV (Oii ) energy level alignment at the interface between the ITO and the
and 529.9 eV (Oiii ). The peak at 532.2 eV is related to O H, O C or active layer, and favored the ohmic contact between LUMO of
O O bonds adsorbed on the ITO surface; the peak at 531.2 eV was PCBM. Moreover, the low work function of ITO made a large poten-
corresponded to the oxygen-deficient in the ITO matrix; and the tial difference between two electrodes, which could enhance the
peak at 529.9 eV was relevant to the oxide lattice without oxygen extraction efficiency of the photo-generated carriers. When the
vacancies [25]. In Fig. 5, we noticed that compared to the inten- ITO was plasma-treated using the applied power over 200 W, the
sity of peak Oiii , the intensity of peak Oii distinctly increased along increased applied power resulted in a decrease in Jsc from 9.04 to
the power. As shown in Table 3, the ratios of Oii /Oiii apparently 7.38 mA/cm2 , and the Voc remained unchanged. The variation in Jsc
32 M. Fang et al. / Applied Surface Science 385 (2016) 28–33

Fig. 5. The deconvolution of O 1s in XPS spectra for treated ITO by Ar plasma for 3 min versus applied powers (a-without treatment; b-100W; c-200W and d–500 W).

Fig. 6. a- In-3d5/2 and b- Sn-3d5/2 in XPS for treated ITO by Ar plasma for 3 min versus applied power.

20 4. Conclusions

Control
15 In this paper, we used CCP plasma to treat ITO as cath-
100 W
200 W ode electrode for fabricating inverted organic solar cells with
10 300 W
ITO/P3 HT:PCBM/MoO3 /Ag structure. It was found that the Ar
J (mA/cm )

500 W
2

plasma treated-ITOs could successfully improve the OSCs photo-

5 voltaic performance. The inverted OSCs demonstrated 3.22% PCE
even without the electron transport layer. After detecting ITOs by
0 XPS and Kelvin probe measurement, it indicated that the chemi-
cal component of ITOs surface changed, including the increase of
-5
doped Sn and oxygen vacancy. Meanwhile the work function of ITO
decreased along with the RF power. After analyzing, it was clear
-10
-0.4 -0.2 0.0 0.2 0.4 0.6 0.8 that the increase of doped Sn and oxygen vacancy caused the work
Voltage (V) function decrease of ITOs surface, which explained the promotion
of devices.
Fig. 7. The J-V characteristics of the inverted organic solar cells fabricated with Ar
plasma-treated ITO.
Acknowledgements

This work is supported by BIGC Project (No.09000114/129,

may be due to the decrease of the ITO transmittance and the change 27170115004/043) and Science and technology project of Beijing
in the morphology of ITO surface. Municipal Education Commission (18190115/013).
 M. Fang et al. / Applied Surface Science 385 (2016) 28–33
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