Applied Surface Science 414 (2017) 224229

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Applied Surface Science

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

Effects of plasma treatment time on surface characteristics of

indium-tin-oxide lm for resistive switching storage applications
Po-Hsun Chen a , Ting-Chang Chang a,b, , Kuan-Chang Chang c,d, , Tsung-Ming Tsai c ,
Chih-Hung Pan c , Chih-Cheng Shih c , Cheng-Hsien Wu c , Chih-Cheng Yang c ,
Wen-Chung Chen c, Jiun-Chiu Lin c, Ming-Hui Wang c, Hao-Xuan Zheng a, Min-Chen Chen a,
Simon M. Sze e
a
Department of Physics, National Sun Yat-Sen University, Kaohsiung 804, Taiwan, ROC
b
Advanced Optoelectronics Technology Center, National Cheng Kung University, Tainan 701, Taiwan, ROC
c
Department of Materials and Optoelectronic Science, National Sun Yat-Sen University, Kaohsiung 804, Taiwan, ROC
d
School of Electronic and Computer Engineering, Peking University, Shenzhen 518055, China
e
Department of Electronics Engineering and Institute of Electronics, National Chiao Tung University, Hsinchu 300, Taiwan, ROC

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 implement a post-oxidation method to modify surface characteristics of indium tin
Received 13 December 2016 oxide (ITO) lms by using an O2 inductively coupled plasma (ICP) treatment. Based on eld emission-
Received in revised form 20 February 2017 scanning electron microscope (FE-SEM) and atomic force microscope (AFM) analysis, we found that the
Accepted 7 April 2017
surface morphologies of the ITO lms become slightly atter after the O2 plasma treatment. The optical
Available online 23 April 2017
characteristics and X-ray diffraction (XRD) experiments of either pure ITO or O2 plasma treated ITO lms
were also veried. Even though the XRD results showed no difference from bulk crystallizations, the
Keywords:
oxygen concentrations increased at the lm surface after O2 plasma treatment, according to the XPS
Inductively coupling plasma (ICP)
Resistive random access memory (RRAM)
inspection results. Moreover, this study investigated the effects of two different plasma treatment times
Indium-tin-oxide (ITO) on oxygen concentration in the ITO lms. The surface sheet resistance of the plasma treated ITO lms
Oxygen gas (O2 ) became nearly non-conductive when measured with a 4-point probe. Finally, we applied the O2 plasma
treated ITO lms as the insulator in resistive random access memory (RRAM) to examine their potential for
use in resistive switching storage applications. Stable resistance switching characteristics were obtained
by applying the O2 plasma treatment to the ITO-based RRAM. We also conrmed the relationship between
plasma treatment time and RRAM performance. These material analyses and electrical measurements
suggest possible advantages in using this plasma treatment technique in device fabrication processes for
RRAM applications.
2017 Elsevier B.V. All rights reserved.

1. Introduction sistive random access memory (MRAM) [1], ferroelectric random

Since ash memory has encountered its physical limitations
when facing scaling down issues, many candidates have been pro-
posed to try to overcome this dilemma. Over the past twenty years,
many kinds of next generation memory technologies have been
investigated for real memory applications, including magnetore-
Corresponding author at: Department of Physics, National Sun Yat-Sen Univer-
sity, Kaohsiung 804, Taiwan, ROC.
Corresponding author at: School of Electronic and Computer Engineering, Peking
University, Shenzhen 518055, China.
E-mail addresses: tcchang3708@gmail.com (T.-C. Chang),
kcchang@pkusz.edu.cn (K.-C. Chang).
access memory (FeRAM) [2], phase change memory (PCM) [3], and
resistive random-access memory (RRAM) [4]. Among these possi-
ble candidates, RRAM has received signicant attention in recent
years because of its non-volatile characteristics, extremely simple
structure with high compatibility to the CMOS fabrication process,
and high device density [57]. However, the resistive switching
(RS) mechanism of RRAM is still much disputed. Among those pos-
sible RS explanations, the conducting lament (CF) theory is the
most common, where the high resistance state (HRS) and low resis-
tance state (LRS) are repeatedly transformed by the formation and
breakage of a current conducting path [8,9].
Since RRAM has many excellent properties, numerous materials
have examined for use as either an electrode or insulator in possi-
ble data storage applications [1017]. The indium-tin-oxide (ITO)

http://dx.doi.org/10.1016/j.apsusc.2017.04.060
0169-4332/ 2017 Elsevier B.V. All rights reserved.
 P.-H. Chen et al. / Applied Surface Science 414 (2017) 224229
lm is quite popular in semiconductor industry for its characteris-
tics of good conductivity and high transparency. Previous research
has applied ITO lm in RRAM to fulll all transparent memory
(ATM) applications [18,19]. In addition, experimental results have
shown that the RRAM with an ITO top electrode can produce self-
compliance current [20,21]. This has been attributed to a serious
internal resistance in the ITO lm, as compared to a traditional
metal electrode [22]. Other studies also revealed that the ITO elec-
trode has the benecial characteristics of lower operation current
and voltage, which are suitable for use in low power consumption
devices [23,24]. Therefore, we conclude that ITO is very suitable
material for potential applications in resistance switching storage.
In this study, we adopt O2 inductively coupled plasma (ICP) as an
oxidation technique to modify the surface characteristics of an ITO
lm, unlike ICPs standard application in the semiconductor indus-
try as an etching process. After O2 plasma treatment, we found
that the previous conductive ITO lm was modied and became
nearly non-conductive. A series of material analyses have also been
conducted to investigate the ITO characteristics either with or with-
out plasma treatment. In addition, two different plasma treatment
times were also considered. We concluded that the ITO lm was
post-oxidized after O2 plasma treatment based on material analy-
ses. Finally, we applied these O2 plasma treated ITO lms for use
as an insulator in RRAM. A stable resistance switching mechanism
was thus achieved in the ITO/ITO(O2 plasma)/TiN device. Accord-
ing to electrical measurements, we can conclude that the plasma
treatment time will affect forming voltage in this ITO-based RRAM.
However, the self-compliance current and high resistance state
(HRS) and low resistance state (LRS) distributions show almost no
difference in the devices regardless of plasma treatment time. These
experimental results also suggest possible future device fabrica-
tion processes to fulll ATM with an identical material as either
electrode or insulator, which is benecial to material selection in
RRAM applications.
2. Experimental details
2.1. O2 plasma treated lms
Three identical ITO lms were deposited by RF sputtering an ITO
target using 30-sccm Ar gas at a 4-mtorr working pressure. Then
the O2 plasma treatment was carried out to post-oxidize the ITO
lm. Different plasma treatment times of 180 s and 300 s were also
conducted on the ITO lms, respectively, denoted as ITO(O2 180 s)
and ITO(O2 300 s). The other non-treated ITO lm is denoted as pure
ITO lm. All three test lms were prepared in order to investigate
the effects of plasma treatment by material analyses.
2.2. RRAM devices
Two identical Ti/SiO2 /Si bottom substrates were deposited by
atomic layer deposition (ALD). Then identical patterned bottom
electrodes of TiN were made by a mask aligner and the ALD process
on these two test samples as TiN/Ti/SiO2 /Si. The thickness of the TiN
electrode was 180 nm. Next, two identical 10-nm thick ITO layers
were deposited for use as insulators by RF sputtering an ITO tar-
get using 30-sccm Ar gas at 4-mtorr working pressure. Afterward,
the O2 ICP treatment was applied to post-oxidize the ITO lm. The
plasma process is shown in Fig. 1(a). The plasma treatment param-
eters are also shown in Fig. 1(b). The O2 plasma treatment was
performed for 180 s and 300 s on the two samples, respectively, to
compare the effects different plasma treatment times. Finally, an
identical ITO lm top electrode was created by the same RF sput-
tering process to form devices of ITO/ITO(O2 180 s)/TiN (denoted as
O2 -180 s-RRAM) and ITO/ITO(O2 300 s)/TiN (denoted as O2 -300 s-
225
RRAM), respectively. The memory devices were pattered with a cell
size of 0.36 m2 . All electrical measurements were performed with
an Agilent B1500A semiconductor parameter analyzer. The DC and
AC biases were applied to the bottom electrode with top electrode
grounded.
3. Results and discussion
Material analyses were rst carried out to investigate the char-
acteristics of the plasma treated ITO lm. Fig. 2(a)(c) shows the
observed surface roughness of the pure ITO, ITO(O2 180 s), and
ITO(O2 300 s), respectively, by use of eld-emission scanning elec-
tron microscopy (FE-SEM). Grains are clearly seen in Fig. 2(a), as
has been conrmed in experimental results reported in previous
ITO-related studies [25,26]. After the O2 plasma treatment shown
in Fig. 2(b), however, the grains of the ITO lm became less obvi-
ous. An apparently similar surface roughness was also observed in
Fig. 2(c), when plasma treatment time was increased to 300 s.
To further conrm these results, 3D atomic force microscopy
(AFM) was conducted. As shown in Fig. 3(a)(c), the surface of the
pure ITO lm similar to reference [27] is rougher and more granular
than that of plasma treated ITO lms, which conrms the results of
the FE-SEM examination. In addition, the root-mean square (RMS)
surface roughness of around 0.864 nm in the pure ITO lm is larger
than that of 0.821 nm in the ITO(O2 180 s) and 0.805 nm in the
ITO(O2 300 s) lms. As a result, we conclude that the surface rough-
ness of the ITO will become atter after O2 plasma treatment.
Fig. 4 shows a comparison of the optical properties of O2 plasma
treated ITO and pure ITO lms. The pure ITO lm has a good trans-
mittance rate (higher than 80%) within the range of visible light
wavelength (380780 nm). The O2 plasma treated lms, while also
having good transmittance rates at longer wavelengths, exhibited a
slight decrease in short wavelengths between 300 nm and 400 nm.
After conversion via Taucs plot to obtain their energy bandgap vari-
ations, we found the energy band gap to be about 3.5 eV for the
pure ITO lm. In contrast, we found the energy band gap of the
treated lms decreases to 3.28 eV and 3.32 eV for ITO(O2 180 s)
and ITO(O2 300 s), respectively. We conclude that the decrease in
both short wavelength and band gap after O2 plasma treatment is
because of the oxidation effects induced by O2 plasma on the ITO
lm. Previous studies have also reported the same slight decrease
in transmittance is primarily induced by the decrease in carrier
concentration [28]. In addition, the reduction of the tted band gap
after O2 plasma treatment is mainly a product of the BursteinMoss
effect [28]. In addition to optical properties, X-ray diffraction (XRD)
was applied to examine the bulk crystallization of these three lms.
As is clear in Fig. 5, four main peaks corresponding to (222), (400),
(440), and (622) were found in both pure ITO and O2 plasma treated
ITO lms [29,30]. Regardless of plasma treatment time, the same
XRD peaks were also obtained. This XRD examination results indi-
cate that the crystallizations of these three bulk lms are nearly
identical.
Next, X-ray photoelectron spectroscopy (XPS) was performed to
verify the surface elemental compositions in these ITO-based lms.
Fig. 6(a) shows the XPS experimental results of the ITO(O2 180 s)
and ITO(O2 300 s) lms, where In 3d5/2 , In 3d3/2 , Sn 3d5/2 , Sn 3d3/2 ,
and O 1s peaks were obtained. In addition, the atomic ratio of each
element was calculated, where O:Sn:In is 51.8%:4.5%:43.7% for the
ITO(O2 180 s) lm, and O:Sn:In is 50.4%:4.8%:44.8% for the ITO(O2
300 s) lm, respectively. The pure ITO was found to be O:Sn:In equal
to 45.1%:5.2%:49.7% (not shown here). Note that the concentration
of O is clearly higher after the O2 plasma treatment. Moreover, the
longer the plasma treatment time, the higher concentration of O
on the surface. To explore the reason for this increase in O on the
surface, we examine the spectroscopy of O 1s in these three lms. As
226 P.-H. Chen et al. / Applied Surface Science 414 (2017) 224229

Fig. 1. (a) O2 plasma treatment process in the RRAM devices. (b) Detailed O2 plasma treatment parameters in the proposed techniques in this study.

Fig. 2. FE-SEM images representing surface roughness of (a) pure ITO and ITO lms treated by O2 plasma for (b) 180 s and (c) 300 s.

shown in Fig. 6(b), both an oxygen lattice and an oxygen deciency
were observed in these three lms. However, the peak of the oxygen
deciency is clearly higher in the O2 plasma treated lms shown in
Fig. 6(b)(ii) and (iii), as compared to the peak of oxygen deciency in
the pure ITO lm shown in Fig. 6(b)(i). In addition, the surface sheet
resistance measurements for all three lms are shown in Fig. 6(c),
with sheet resistance of pure ITO lm about 90 /, while those of
ITO (O2 180 s), and ITO (O2 300 s) lms were both larger than 1 M
/.
Based on these XPS and 4-point probe measurements, we con-
cluded that the surface characteristics of the pure ITO lm were
modied after the O2 plasma treatment. This is mainly because
the oxygen concentration is increased by O2 plasma treatment,
making the previously conductive ITO lm become nearly non-
conductive [31,32]. Moreover, when the plasma treatment time is
increased, the oxygen mole concentration also increases. In order
to understand the benets of such modications, it is best to
explore the use of such O2 treated ITO lms in potential RRAM
applications. To conrm how these modications affect electrical
performance when treated ITO lms are integrated as the insulator
of the RRAM devices, two devices were constructed: ITO/ITO(O2
 P.-H. Chen et al. / Applied Surface Science 414 (2017) 224229 227

Fig. 3. 3D-AFM image (scan size 0.8 m 0.8 m) of (a) pure ITO lm, (b) ITO(O2 180 s), and (c) ITO(O2 300 s) lms. The RMS surface roughness is about 0.864 nm in the pure
ITO lm, which is larger than that of 0.821 nm in (O2 180 s), and 0.805 nm in (O2 300 s) lms.

Fig. 4. Optical properties of pure ITO, ITO(O2 180 s), and ITO(O2 300 s) lms. Inset
shows the tted energy band gaps of these three lms converted by Taucs plot.

Fig. 6. (a) X-ray photoelectron spectroscopy (XPS) results for ITO (O2 180 s) and
ITO (O2 300 s) lms. The inset table shows the mole concentration of O, Sn and In
elements of the treated ITO lms. (b) O 1s spectroscopy of (i) pure ITO, (ii) ITO (O2
180 s) and (iii) ITO (O2 300 s) lms indicates the oxygen deciency and oxygen lattice
variations. (c) The 4-point probe measurement results reveal the sheet resistance of
these three lms.

Fig. 5. X-ray diffraction (XRD) was applied to examine bulk characteristics of crys-
tallizations in these three ITO lms.
228 P.-H. Chen et al. / Applied Surface Science 414 (2017) 224229

Fig. 7. (a) Negative and (b) positive forming processes of the ITO/ITO(O2 180 s)/TiN and ITO/ITO(O2 300 s)/TiN devices. Statistical results of (c) negative and (d) positive
forming voltages for both devices. (e) Extracted HRS and LRS variations with a small read voltage of 0.1 V over 100 continuous DC sweep cycles. (f) Box plot showing HRS and
LRS distributions in both devices.

180 s)/TiN (denoted as O2 -180-RRAM) and ITO/ITO(O2 300 s)/TiN
(denoted as (O2 -300-RRAM).
Fig. 7(a) shows the negative forming processes without any
external current compliance in both O2 -180-RRAM and O2 -300-
RRAM devices. The forming voltage was observed to increase
slightly (from 4.8 V to 5 V) when the O2 plasma treatment time
is increased from 180 s to 300 s. However, both devices show the
same self-current compliance (3 A) when applying a 10 V bias. In
addition to negative bias forming, positive forming process is also
investigated, and shown in Fig. 7(b). Here, the forming voltage also
increases from +2.7 V in the O2 -180-RRAM to +2.85 V in the O2 -300-
RRAM device. Again, self-compliance currents (2 A) appear in both
devices. To further conrm their variations in forming voltages, the
statistics of 10 random points of both negative and positive forming
voltages were investigated. Fig. 7(c) and (d) shows that the aver-
age negative forming voltage of the O2 -180-RRAM device is 4.9 V,
slightly lower than the 4.95 V for the O2 -300-RRAM device. As for
positive forming process, the average positive forming voltage is
+2.7 V for O2 -180-RRAM, slightly lower than +2.75 V for O2 -300-
RRAM.
In addition to this investigation of forming voltage statistics,
DC measurements of these two devices were also conducted. Both
devices show very stable resistance switching characteristics with
negative SET and positive RESET operations (not shown here). To
extract the high resistance state (HRS) and low resistance state
(LRS) variations, a small read voltage of 0.1 V was applied without
altering the resistance states, as shown in Fig. 7(e). The ratios of HRS
and LRS in both devices were around 100, which is very suitable
for resistance data storage applications. Fig. 7(f) shows box plots
of these HRS and LRS distributions in both O2 -180-RRAM and O2 -
300-RRAM devices. Note that the ratios of HRS and LRS are almost
identical in both devices regardless of plasma treatment time.
Since both devices have identical top and bottom electrode
combinations, the characteristics of the insulator will most clearly
affect the electrical performance in these RRAM devices. Electri-
cal measurements of forming and DC operations indicate that the
insulator properties do indeed affect forming voltage, depending
on the degree of oxidation of the insulators that is produced by dif-
ferent plasma treatment times. Once the insulator lms undergo
soft-break down by external electrical elds during the forming
 P.-H. Chen et al. / Applied Surface Science 414 (2017) 224229
process, self-compliance currents are mainly limited by the inter-
nal resistance from the top ITO electrode. As a result, we obtained
different forming voltages with identical self-compliance currents
in both devices. Further, the distributions of the HRS and LRS are
almost the same in both devices.
4. Conclusion
In conclusion, we implemented a plasma treatment technique
to post-oxide ITO lm. We examined the lm surface characteristic
after the O2 plasma treatment with material analyses and electri-
cal measurements. From material analyses results, we found ITO
lm be oxidized after the O2 plasma treatment. In addition, the
conductivity of the ITO lm was dramatically modied to become
nearly non-conductive. Moreover, the effects of different plasma
treatment times on lm characteristics were also considered. These
experimental results were applied in an investigation of treated
ITO used as insulators in RRAM devices. We found that stable resis-
tance switching characteristics can be achieved in this ITO-based
RRAM, according to electrical measurements. These material anal-
yses and electrical measurements suggest possible advantages in
using this plasma treatment technique in device fabrication pro-
cesses for RRAM applications.
Acknowledgement
This work was performed at National Science Council Core
Facilities Laboratory for Nano-Science and Nano-Technology in
Kaohsiung-Pingtung area and was supported by the Ministry of
Science and Technology, Taiwan (MOST) under Contract Nos.
MOST-103-2112-M-110-011-MY3.
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