Optics and Laser Technology 101 (2018) 85–90

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Optics and Laser Technology

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

Full length article

Facile solution-processed aqueous MoOx for feasible application in

organic light-emitting diode
Qinghong Zheng a, Disui Qu a, Yan Zhang a, Wanshu Li a, Jian Xiong a, Ping Cai a, Xiaogang Xue a, Liming Liu b,⇑,
Honghang Wang b, Xiaowen Zhang a,⇑
a
School of Materials Science and Engineering & Guangxi Key Laboratory of Information Materials, Guilin University of Electronic Technology, Guilin 541004, PR China
b
Zhongshan Branch of State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Zhongshan Institute, Zhongshan
528402, PR China

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

Article history: Solution-processed techniques attract increasing attentions in organic electronics for their low-cost and
Received 14 August 2017 scalable manufacturing. We demonstrate the favorite hole injection material of solution-processed aque-
Received in revised form 24 October 2017 ous MoOx (s-MoOx) with facile fabrication process and cast successful application to constructing efficient
Accepted 8 November 2017
organic light-emitting diodes (OLEDs). Atomic force microscopy and X-ray photoelectron spectroscopy
analysis show that s-MoOx behaves superior film morphology and non-stoichiometry with slight oxygen
deficiency. With tris(8-hydroxy-quinolinato)aluminium as emitting layer, s-MoOx based OLED shows
Keywords:
maximum luminous efficiency of 7.9 cd/A and power efficiency of 5.9 lm/W, which have been enhanced
OLED
Solution process
by 43.6% and 73.5%, respectively, in comparison with the counterpart using conventional vacuum ther-
MoOx mal evaporation MoOx. Current-voltage, impedance-voltage, phase-voltage and capacitance-voltage char-
Hole injection acteristics of hole-only devices indicate that s-MoOx with two processes of ‘‘spin-coating/annealing”
Interface engineering shows mostly enhanced hole injection capacity and thus promoting device performance. Our experi-
ments provide an alternative approach for constructing efficient OLED with solution process.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction with all solution process. Moreover, solution-processed techniques

Organic light-emitting diodes (OLEDs) have been received
numerous attentions in both academic researches and industrial
applications because of their advantageous performance such as
amazing color gamut, high efficiency and manufacturing conve-
nience [1]. OLED is a typical carrier-injection dependent device
that carrier balance governing luminous efficiency. Inserting car-
rier injection material between electrode and carrier transport
layer is consequently proposed to fulfill such a function. Some
extra metal oxides of MoOx [2,3], V2O5 [4], NiO [5] and WO3 [6]
are widely-used hole injection layers (HILs) for their appropriate
work function and superior film morphology. It is well established
that MoOx stands out as the favorite candidate for its non-toxicity,
medium evaporation temperature, good transparence, tailored
work function and improved device durability [3,7–11]. However,
MoOx is usually deposited using cost-intensive vacuum thermal
evaporation. Recently, solution-processable techniques such as
printing, roll-to-roll and doctor blading advance electronic devices
⇑ Corresponding authors.
E-mail addresses: liulmxps@126.com (L. Liu), zhang-xiaowen@163.com
(X. Zhang).
possess low-cost and scalable manufacturing. Solution processed
HILs such as poly(3,4-ethylenedioxythiophene):poly(styrenesulfo
nate) (PEDOT:PSS) [7,11], graphene oxide (GO) [12–14] and copper
phthalocyanine-3,40 ,400 ,400 0 -tetra-sulfonated acid tetra sodium salt
(TS-CuPc) [15] are intensively investigated in OLEDs. PEDOT:PSS
possesses strong hole injection ability, but its acidic nature and
hygroscopicity are detrimental to device durability [7,11,16].
While GO behaves a work function of only 5.0 eV [14], which lim-
its hole injection promotion especially in violet/blue emitters with
deep highest occupied molecular orbital levels.
Solution-processed MoOx is predominantly derived from sol-gel/
precursor solution [17–23], ammonia-dissolved/dispersed solution
[20,24,25], alcohol-dissolved/dispersed solution [1,11,18,26,27],
nanoparticles suspension [8,28], or phosphomolybdic acid (PMA)
[29]. It is also reported that MoO3 powders show small amounts
of solubility in water [7,20,25,30–32], which provides an easy-
to-do and environment-friendly approach for preparing solution-
processed aqueous MoOx (s-MoOx). In this study, we focus on
s-MoOx with facile fabrication process by directly dissolving MoO3
powders into de-ionized water. Based on the MoOx aqueous solu-
tion, superior film morphology is obtained by using conventional
method of spin-coating/annealing process. Moreover, the MoOx

https://doi.org/10.1016/j.optlastec.2017.11.010
0030-3992/Ó 2017 Elsevier Ltd. All rights reserved.
86 Q. Zheng et al. / Optics and Laser Technology 101 (2018) 85–90

aqueous solution and subsequent annealing don’t involve ammo-
nium molybdate ((NH4)6Mo7O244H2O) precursor [33,34] and
plasma treatment [9], which considerably simplifies device fabrica-
tion. In addition, in comparison with conventional one process of ‘
‘spin-coating/annealing” [30], the hole injection capacity of s-
MoOx can be further enhanced by employing two processes of ‘‘spi
n-coating/annealing”, which contributes to extremely enhance-
ment in device efficiency and decrease in driving voltage. Our
results pave an alternative way for advancing OLEDs with solution
process.
2. Experiment details
MoOx solution (0.25% in weight ratio) was obtained by
dissolving MoO3 powders (>99.5%) into de-ionized water with
continuously-prolonged stirring and heating at about 75 °C. The
hydrolysis reaction of MoO3 was occurred as Eq. (1).
þ
MoO3 þ H2 O ¼ MoO2
4 þ 2H
It is obvious that accumulation of H+ ions significantly retards
hydrolysis and weakens solubility of MoO3 powders in de-
ionized water. The maximum concentration of MoOx aqueous
solution was 0.25% in our experiments. ITO coated glass was chem-
ically cleaned and served as substrate/anode for studied OLEDs.
The HIL was formed by spin-coating MoOx solution (filtered
through a 0.22 lm filter) at 4000 rpm for 60 s and subsequently
heat treated at 120 °C for 20 min in air conditions. The hole trans-
port layer (55 nm) of N,N0 -bis(naphthalen-1-yl)-N,N0 -bis(phenyl)-
benzidine (NPB), emitting layer (25 nm) of tris(8-hydroxy-quinoli
nato)aluminium (Alq3), electron transport layer (15 nm) of 4,7-
diphenyl-1,10-phenanthroline (BPhen) and bilayer cathode of LiF
(0.8 nm)/Al (100 nm) were sequentially piled by thermal deposi-
tion under a vacuum of 4  104 Pa. The MoOx HIL with one pro-
cess of ‘‘spin-coating/annealing” refers as s-MoOx1 (Device A1).
While the MoOx HIL with two or three processes of ‘‘spin-coat
ing/annealing” refers as s-MoOx2 (Device A2) or s-MoOx3 (Device
A3). The OLED without HIL (Device B) or using vacuum thermal
evaporation MoOx (e-MoOx, 2 nm) as HIL (Device C) was also con-
structed for comparison. The active area of these devices was 5  5
mm2. The layer thickness and deposition rate were monitored and
controlled in situ with an oscillating quartz thickness monitor.
Typical deposition rate for organics was 2 Å/s. Fig. 1 shows the
schematic structure of s-MoOx based OLEDs. The molecular struc-
tures of organic materials used are shown in Fig. S1 in Supporting
Information.
The current-voltage-luminance (I-V-L) characteristics were
simultaneously measured with a computer controlled pro-
grammable Keithley 2636B Source Meter and Konica Minolta LS-
150 Luminance Meter. The electroluminescent (EL) spectrum and
1931 Commission Internationale d’Eclairage (CIE) color coordi-
nates were measured with an Ocean Optics Maya-2000-Pro Spec-
ð1Þ trum Scan. All measurements were carried out at room
temperature under ambient conditions. An atomic force micro-
scopy (AFM, Bruker Dimension Edge) was used for characterizing
surface morphology. The X-ray photoelectron spectroscopy (XPS)
was characterized with Thermo Scientific Escalab 250Xi System.
A monochromatic Al Ka (1486.6 eV) was used in the XPS measure-
ment. An Agilent 4294A Precision Impedance Analyzer was used
for impedance spectroscopy analysis.
3. Results and discussions
Fig. 2 shows the AFM images of bare ITO and s-MoOx2 film coat-
ing onto ITO substrate. One sees that bare ITO shows distinct grains
and grain boundaries embedded with a small amount of pin-holes
on film surface. With MoOx coating onto ITO, smooth surface with

Fig. 1. Schematic structure of OLEDs with HIL of s-MoOx formed by spin-coating MoOx aqueous solution. The image of 0.25% MoOx aqueous solution (faint yellow) is also
incorporated in the figure. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 2. The AFM images of (a) ITO and (b) ITO/s-MoOx2 with scanning area of 2 lm  2 lm.
 Q. Zheng et al. / Optics and Laser Technology 101 (2018) 85–90 87

improved flatness is observed. The average roughness (Ra) of ITO/
MoOx is reduced to 1.11 nm in comparison with that (1.35 nm) of
bare ITO. It indicates that the incorporation of MoOx fills some
existing pin-holes and/or removes some spikes of ITO, suggesting
homogeneous MoOx film formation on ITO substrate.
Atomic composition analysis of s-MoOx film is conducted by
XPS measurements, as shown in Fig. 3(a) and (b). The Mo 3d core
level spectrum exhibits two bands of Mo 3d3/2 and Mo 3d5/2,
resulting predominantly from the existence of Mo6+. Small
amounts of Mo5+, observed at 1.1 eV lower binding energies,
accounts for the existence of oxide vacancy [1,7,21,35]. Moreover,
detailed calculation shows that x = 2.95 for s-MoOx film in this
study. It is quite similar to e-MoOx film (x = 2.98) [1], behaving
non-stoichiometric and thus semi-conducting properties. Such
special characteristics of MoOx play a key role in tailoring hole
injection characteristics in OLEDs [1,7–9].
The electro-optic properties of Devices A1, A2, A3 and compar-
ing with Devices B and C are shown in Fig. 4. Some of critical

Fig. 3. The XPS spectra of s-MoOx film: (a) full spectrum and (b) corresponding Mo 3d core level spectrum.

Fig. 4. (a) Luminous and (b) power efficiencies as a function of current density, and (c) current density and (d) luminance as a function of voltage characteristics of OLEDs
with different HILs.
88 Q. Zheng et al. / Optics and Laser Technology 101 (2018) 85–90

parameters are displayed in Table 1. It is observed that Device A2
(s-MoOx2 as HIL) shows maximum luminous efficiency of 7.9 cd/A
and power efficiency of 5.9 lm/W, which have been enhanced by
83.7% and 1.8 times, respectively, as compared with those (4.3
cd/A and 2.1 lm/W) of Device B (without HIL). This is explicitly
resulted from the fact that s-MoOx promotes hole injection. More-
over, the performances of Device A2 are superior to Device C
(e-MoOx as HIL). For instance, in comparison with Device C, the
maximum luminous efficiency and power efficiency of Device A2
have been enhanced by 43.6% and 73.5%, respectively. The driving
voltage at luminance of 1000 cd/m2 has been decreased from 4.9 V
(Device C) to 4.0 V (Device A2). It suggests that s-MoOx to an
extremely extent enhances hole injection in comparison with
e-MoOx. This can also be verified by the current density versus
voltage curves as shown in Fig. 4(c), i.e., Devices A1, A2 and A3
(s-MoOx as HIL) show higher current density than Device C
(e-MoOx as HIL) at the same voltage. The promoted hole injection
better favors carrier balance in the emitting layer and thereby pro-
moting luminance. The s-MoOx based OLED reaches a luminance
of 22344 cd/m2 at 8 V, which almost doubles that (11281 cd/m2)
of e-MoOx based device (see Table 1). Typical s-MoOx based OLED
gives Alq3 emission with EL peak of 535 nm and CIE color coordi-
nates of (0.338, 0.556), as shown in Fig. S2 in Supporting
Information.
It should be noted that Device A2 shows the best performance
in comparison with Devices A1 and A3. As is known that MoO3
powders behave lower concentration in water, the two processes
of ‘‘spin-coating/annealing” (s-MoOx2) may better favors filling sur-
face pinholes and/or removing corrugations than one process of ‘‘
spin-coating/annealing” (s-MoOx1), which improves film morphol-
ogy. Consequently, we propose that s-MoOx2 forms continuous film
during fabrication process, as schematically depicted in Fig. S3(a)
in Supporting Information. While 2-nm-thick e-MoOx tends to pro-
duce film discontinuity, as schematically depicted in Fig. S3(b) in
Supporting Information. In such a case, some holes still injecting
from ITO directly to NPB without the MoOx HIL, which deteriorates
hole injection capacity as a result of larger barrier height at ITO/
NPB interface. This obviously accounts for the fact that e-MoOx
behaves slightly inferior hole injection capacity to s-MoOx.
To further investigate the hole injection capability of s-MoOx,
the following series of hole-only devices (HODs) are fabricated
for I-V measurements and impedance spectroscopy analysis.

Table 1
Performance summary of OLEDs with different HILs.

Devices HIL Maximum luminous Maximum power Luminance at Voltage at luminance

efficiency (cd/A) efficiency (lm/W) 8 V (cd/m2) of 1000 cd/m2 (V)
Device A1 s-MoOx1 6.7 5.6 17928 4.2
Device A2a s-MoOx2 7.9 5.9 22344 4.0
Device A3 s-MoOx3 6.5 5.4 14508 4.4
Device B w/o 4.3 2.1 7134 6.5
Device C e-MoOx 5.5 3.4 11281 4.9
a
The champion device in this study.

Fig. 5. (a) The I-V curves of HODs with different HILs. Inset: Schematic structure of HODs. (b) the Z-V, (c) u-V and (d) C-V transition characteristics of HODs with different HILs.
 Q. Zheng et al. / Optics and Laser Technology 101 (2018) 85–90
Cell 1: ITO/s-MoOx1/NPB/Al.
Cell 2: ITO/s-MoOx2/NPB/Al.
Cell 3: ITO/s-MoOx3/NPB/Al.
Cell E: ITO/e-MoOx/NPB/Al.
Cell 0: ITO/NPB/Al.
The I-V curves of these studied HODs are comparatively
depicted in Fig. 5(a). It is obvious that Cell 2 shows the highest cur-
rent as compared with other cells at the same voltage, suggesting
s-MoOx2 behaving robust hole injection capacity.
The impedance and phase versus voltage (Z-V, u-V) transition
characteristics are delineated in Fig. 5(b) and (c). One sees that
all these cells show high impedance of about 105 X and phase of
about 90° at low voltage of <1.5 V, indicating an insulating state.
With increasing voltage of more than 2 V, the impedance drops
quickly and the corresponding phase shifts from 90° to 0°, indi-
cating that holes injecting and a transition from insulating state
to semi-conducting state is occurred [3,7,36–38]. On the other
hand, s-MoOx shows lower starting voltage of Z-V and u-V transi-
tions than e-MoOx. The s-MoOx2 (Cell 2) behaves the lowest voltage
of phase approaching 0° in comparison with other HILs (Cells 1, 3
and E) or without HIL (Cell 0), since u = 0° means a purely conduc-
tive process [1,36–38]. These phenomena mean that s-MoOx pro-
motes hole injection ability. The two processes of ‘‘spin-coating/
annealing” (s-MoOx2) give extremely enhancement in hole injec-
tion capacity and thus improving OLED performance.
Fig. 5(d) shows the capacitance versus voltage (C-V) character-
istics of cell 1, cell 2, cell 3, cell E and cell 0. When the voltage is
less than 2 V, there is no significant difference in capacitance,
which corresponding to static dielectric properties of HODs. When
the voltage larger than 2 V, the capacitance getting higher with
increasing voltage. It suggests that holes injecting from ITO and
accumulated at somewhere of NPB, i.e., promoting carrier storage
ability and thus contributing to capacitance promotion [1,38,39].
With further increasing voltage, the C-V curves show a capacitance
peak (Cp), as marked with arrows in Fig. 5(d). It is observed that
the voltage of Cp increases in the sequence of cell 2 (5.4 V) < cell
1 (5.6 V) < cell 3 (5.7 V) < cell E (6.5 V) < cell 0 (8.5 V). The voltage
of Cp means the starting of electron-hole recombination which
deteriorates carrier storage capacity and contributes to capacitance
dropping [1,39,40]. It is reasonably deduced that the lower voltage
of Cp, the stronger hole injection ability, since all these HODs share
the same cathode structure. The C-V transition curves provide
another fact that s-MoOx2 behaves powerful hole injection ability
which considerably boosts holes moving towards adjacent hole
transport layer.
4. Conclusions
Favorite HIL of s-MoOx is facilely and environment-friendly fab-
ricated. The AFM and XPS measurements show that s-MoOx
behaves superior film morphology and non-stoichiometry with
slight oxygen deficiency. With Alq3 as emitter, s-MoOx based OLED
shows maximum luminous efficiency of 7.9 cd/A and power effi-
ciency of 5.9 lm/W, which have been enhanced by 43.6% and
73.5%, respectively, in comparison with e-MoOx based device. I-V,
Z-V, u-V and C-V transition curves of HODs indicate that s-MoOx2
possesses mostly promoted hole injection capacity and thereby
contributing to excellent device performance. Our experiments
provide an alternative approach for constructing efficient OLED
with solution process.
Acknowledgements
Q. Zheng and D. Qu equally contribute to this work. Authors
would like to acknowledge the financial support given by the
89
National Natural Science Foundation of China (61565003,
51362031), Guangxi Natural Science Foundation
(2016GXNSFAA380131), Science and Technology Project of Zhong-
shan (2014A2FC305, 2014A2FC306), Guangxi Experiment Center of
Information Science (YB1417), Innovation Project of GUET Gradu-
ate Education (2016YJCX02), Program for Postgraduate Joint Train-
ing Base of GUET-CJYRE (20160513-15-Z), and the open project
fund of Zhongshan Branch of State Key Laboratory of Electronic
Thin Films and Integrated Devices (412S0601, 412S0613).
Appendix A. Supplementary material
Supplementary data associated with this article can be found, in
the online version, at https://doi.org/10.1016/j.optlastec.2017.11.
010.
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