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Optimization and electrochemical characterization of RF-sputtered iridium

oxide microelectrodes for electrical stimulation

Article in Journal of Micromechanics and Microengineering · January 2014

DOI: 10.1088/0960-1317/24/2/025015

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 Journal of Micromechanics and Microengineering
J. Micromech. Microeng. 24 (2014) 025015 (9pp) doi:10.1088/0960-1317/24/2/025015

Optimization and electrochemical

characterization of RF-sputtered
iridium oxide microelectrodes for
electrical stimulation
Xiaoyang Kang 1 , Jingquan Liu 1 , Hongchang Tian 1 , Bin Yang 1 ,
Yanna NuLi 2 and Chunsheng Yang 1
1
National Key Laboratory of Science and Technology on Micro/Nano Fabrication, Key Laboratory for
Thin Film and Microfabrication of the Ministry of Education, Institute of Micro-Nano Science and
Technology, Shanghai Jiao Tong University, Shanghai 200240, People’s Republic of China
2
Department of Chemical Engineering, Shanghai Jiao Tong University, Shanghai 200240,
People’s Republic of China
E-mail: [email protected]

Received 14 July 2013, revised 30 December 2013

Accepted for publication 3 January 2014
Published 15 January 2014

Abstract
A reactively sputtered iridium oxide (IrOx) thin film has been developed as electrochemical
modification material for microelectrodes to obtain high stability and charge storage capacity
(CSC) in functional electrical stimulation. The effect of the oxygen flow and oxygen to argon
ratio during sputtering process on the microstructure and electrochemical properties of the
IrOx film is characterized. After optimization, the activated IrOx microelectrode shows the
highest CSC of 36.15 mC cm−2 at oxygen flow of 25 sccm and oxygen to argon ratio of
(2.5:1). Because the deposition process of the reactively sputtered iridium oxide is an
exothermic reaction, it is difficult to form film patterning by the lift-off process. The lift-off
process was focused on the partially carbonized photoresist (PR) and normal PR. The higher
of the carbonization degree of PR reaches, the longer the immersion duration. However, the
patterning process of the iridium oxide film becomes feasible when the sputtering pressure is
increasing. The experimental results show that the iridium oxide films forms the pattern with
the lowest duration of ultrasonic agitation when the deposition pressure is 4.2 Pa and pressure
ratio between O2 and Ar pressure is 3:4.

Keywords: iridium oxide, microelectrode, sputtering, electrical stimulation, neural prosthesis

S Online supplementary data available from stacks.iop.org/JMM/24/025015/mmedia

(Some figures may appear in colour only in the online journal)

1. Introduction electrochemical characteristics [3–5]. The good chemical

stability and biocompatibility of the modification material
Neural recording and stimulating microelectrodes have been are also essential to maintain long-term stability in vivo.
extensively investigated as a major part of the neural prosthesis Furthermore, the low polarization could significantly reduce
[1, 2]. In order to obtain higher stability and charge storage the power consumption which is very important for functional
capacity (CSC) of the microelectrodes for the application of electrical stimulation. Benefitting from these advantages,
functional electrical stimulation, iridium oxide is an important iridium oxide is considered as a good candidate material for
modification material of the microelectrode due to its good electrical stimulation [6]. The thin film of iridium oxide can

0960-1317/14/025015+09$33.00 1 © 2014 IOP Publishing Ltd Printed in the UK

J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

Figure 1. Schematic diagram of the sputtering system.

be obtained through different fabricating processes, including could reduce the energy of the sputtered atoms to avoid
the electrodeposited iridium oxide film [7], thermal iridium the carbonization of the photoresist [22, 23]. The pattern
oxide film [8], sputtering iridium oxide film (SIROF) [9] and process of the iridium oxide film is then realized under a
activated iridium oxide film [10]. However, the SIROF is paid relatively high sputtering pressure. Under a relatively low
more attention due to its good mechanical and electrochemical pressure, the carbonization phenomenon could be observed.
properties, and compatibility with the integrated circuit and If the carbonized area is close to the microelectrode site, it is
microelectro mechanical systems process [13–15]. difficult to guarantee the size and shape of microelectrode site.
Many researchers have focused on the study of the The energy of the sputtered atoms and the surface
deposition mechanism of reactively sputtered iridium oxide morphology of the film are obviously affected by the sputtering
thin film. Based on the generic curves, Wessling et al pressure. Meanwhile, the different flow ratios of Ar and
have investigated the influence of the oxygen supply to O2 change the chamber pressure. Previous investigations of
the chamber and pumping speeds on the electrochemical IrOx sputtering under various chamber pressures maintained
properties of the iridium oxide thin film [16]. However the a consistent ratio between the Ar and O2 gas flows, and the
study was mainly about the application of the macro sized reported highest CSC was 28.3 mC cm−2 [24]. Because the Ar
electrodes; the pattern process of the sputtered iridium oxide and O2 gas flows were set to provide equal partial pressures,
thin film was not demonstrated. In addition, the consistency there were a limited total number of testable chamber pressure
in microelectrode site size and patterning is critical to values. However, the effect of Ar to O2 flow ratio was
ensure precision and reproducibility of stimulation events for not taken into consideration which can greatly impact on
stimulating microelectrodes [17]. Thus, the dimension of the electrochemical properties in sputtered films.
electrode has a serious effect on the results of the electrical This study investigates the effect of the oxygen flow
stimulation. While many processes for patterning sputtered under various sputtering pressure on microstructure and
films exist, the lift-off process is ideal for iridium oxide electrochemical properties of the iridium oxide thin film,
due to the following two reasons: the limited selectivity and aiming to achieve a stable and high CSC electrochemical
reaction rate of metal etchants, and limited throughput of laser material for microelectrodes in electrical stimulation
micromachining. applications.
To realize the pattern of the iridium oxide film by
the lift-off process, the sputtering temperature should be
2. Experimental details
controlled to avoid the carbonization of the photoresist
[18, 19]. The sputtering temperature, or chamber temperature, 2.1. Working principle of reactively sputtered iridium oxide
during the sputtering process can be partially controlled by thin film
an artificial heat source, which remained off during the heat-
sensitive process to maintain a lower chamber temperature. Nichiden Anelva, SPF-210H sputtering equipment was
Normally, during sputtering process, the higher sputtering rate deployed to deposit iridium oxide thin films, as shown in
is generated under condition of lower pressure and higher figure 1. All films were deposited on the silicon wafer with
temperature, which contributes to more uniform deposited Ti adhesion layer by the reactively sputtered process in
film [20, 21]. Because the process of the reactively sputtered Ar/O2 plasmas. The Ti adhesion layer with 50 nm thickness
iridium oxide is an exothermic reaction and the heat of was sputtered with 10 sccm (standard cubic centimeters per
the exothermic reaction is constant, high sputtering pressure minute) Ar flow under the chamber pressure of 2.4 Pa. Before

2
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

the deposition process of the iridium oxide, an Ar sputter

(a)
process was performed to remove the potential oxide layer on
the Ti adhesion layer. The RF-power worked at 13.56 MHz,
150 W and was coupled with the target electrode via the (b)
manual impedance matching network. The manual impedance
matching network could adjust the reflected power from 0.05
to 1 of the RF-power, and the plate current was related to the (c)
reflected power. When the reflected power was kept at 10 W,
the plate current was in the range of 110 to 120 mA. The
system was continually cooled with circulating water. (d )
Prior to deposition process, the sputtering chamber
was evacuated to 2 × 10−4 Pa by an oil-sealed mechanical
(e)
pump and a vertical turbo molecular pump. The wafer
was not artificially heated to prevent the occurrence of the
carbonization of the photoresist. The flows of Ar and oxygen
were controlled by the gas mass flow control meters. A (f )
10 sccm Ar flow was introduced, and the chamber pressure
was adjusted to 2.4 Pa by the main valve. At the same RF-
power, the amount of the sputtered iridium atoms is controlled
by the Ar flow. The constant argon flow creates the constant ( g)
amount of the sputtered iridium atoms. The oxidization of the
sputtered iridium atoms is controlled by the flow of the oxygen,
and the oxygen flow was selected from 5 to 40 sccm using a (h)
mixture of Ar and O2 (from 1:0.5 to 1:4). While the oxygen
flow was turned on, the main valve was kept at the position of
2.4 Pa, and the sputtering pressure was from 2.5 to 5.4 Pa.

2.2. Fabrication process of the microelectrode

Figure 2. Fabrication process of the iridium oxide microelectrodes.
Figure 2 shows the fabrication process of the iridium oxide (a) Photoresist spin coating, (b) UV exposure and developing,
microelectrodes. A 5 μm thick positive photoresist (PR) layer (c) Ti/IrOx layer sputtering, (d) Lift-off, (e) CVD Parylene C,
was spun on the silicon wafer (3 inches in diameter, 100 crystal ( f ) Photoresist spin coating, (g) UV exposure and developing,
orientation), as shown in figure 2(a). The PR (AZ4330) was (h) RIE open microelectrode site.
spun at 1500 r min−1 (30 s) and baked at 50 and 90 ◦ C for 1 h,
separately. Next, the PR was patterned by the ultraviolet (UV) standard three electrodes system with an Ag/AgCl reference
light exposure and developed (figure 2(b)). Then a Ti adhesive and a Pt-sheet counter electrode.
layer and iridium oxide (IrOx) thin film were sputtered and The applied potential for activation was swept from −1.0
patterned by a lift-off process (figures 2(c) and (d)). 5 μm to 1.0 V at 0.05 Hz for 100 cycles [24]. After activation, six
thick Parylene-C film was deposited on the silicon wafer by cycles were collected for each CV curve, with a potential
the chemical vapor deposition process (figure 2(e)). A 10 μm range of −0.6 to 0.8 V to keep the voltage in the ‘water
thick PR was spun (figure 2( f )), patterned (figure 2(g)) and window’. The ‘water window’ is a voltage range that neither
stored at 65 ◦ C for 1 h in a vacuum baking oven. At last, the hydrogen nor oxygen is produced from the water in the
microelectrode site and bonding pad were formed by a reactive measurement. The CSC of the iridium oxide microelectrodes
ion etching system (Nextral 100, Reactive Ion Etcher, Alcatel, was measured under the scan rate of 100 mV s−1 [16].
France) (figure 2(h)). The fabricated iridium oxide electrode Electrochemical impedance spectroscopy (EIS) was measured
was shown in figure 3. at the same electrochemical cell at the same time. The
amplitude of sinusoidal signal is 10 mV and its frequency
2.3. SEM, AFM and electrochemical measurement range varies from 0.1 to 100 kHz. The image of the
The morphologies of the samples were observed by a fabricated iridium oxide electrode is shown in figure 3.
field-emission scanning electron microscope (SEM, Carl To improve the validity of comparing electrical impedance
Zeiss Ultra55), as shown in figure 3. The diameter of the based on changes in the sputtering process, we have utilized
microelectrode site is 100 ± 0.5 μm (mean ± sd n = 8). Its a custom developed tool (figure S1, Supplementary data
corresponding surface area is calculated as 7850 ± 79 μm2. are available from stacks.iop.org/JMM/24/025015/mmedia)
Atomic force microscopy (AFM, Nanoscope III, Digital Instr.) to ensure consistent contact area for each of the tested
was also performed to obtain the surface roughness of the microelectrodes. Voltage transient measurements were used
samples. The CSC of the iridium oxide microelectrodes was to evaluate the voltage following property and stability by a
calculated by the cyclic voltammetry (CV). The CV was current-controlled stimulation pulse. The voltage transient was
measured in a physiological saline solution (0.9% NaCl) by the recorded by the configuration with three electrodes, including

3
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

Figure 3. Optical photograph and SEM of the fabricated iridium oxide electrode.

sputtering chamber contributes to the increasing of the pressure

rapidly. While the oxygen flow is larger than 20 sccm, there is a
good linear relationship between the oxygen pressure and flow.
It shows that the oxidation reaction proceeds and all sputtered
iridium is transformed into the oxidation state.

3.2. Morphology and surface microstructure

Figures 5 and 6 show SEM and AFM images of iridium

oxide films under different oxygen flows, respectively. The
morphology and surface microstructural parameters of these
samples are summarized in table 1. Although the surface
of the film at 10 sccm is very rough, the cross section
SEM in figure S2 (Supplementary data are available from
stacks.iop.org/JMM/24/025015/mmedia) shows that the film
has a continuous layer structure. The iridium at 15 sccm
oxygen flow cannot be oxidized further, which results in the
Figure 4. Oxygen partial pressure as a function of the oxygen surface roughness of 17.1 nm. Although a dendritic surface
supply to the sputter chamber (mean ± sd n = 3).
microstructure is developed at 25 sccm, the film obtains good
adhesion property to the substrate. Finally, a dendritic surface
large-area Pt-sheet return electrode and a noncurrent-carrying with increasing aggregation is produced at 40 sccm oxygen
Ag/AgCl reference electrode. flow. The aggregation is also validated by the AFM data shown
in figure 6(d).
3. Result and discussion
3.3. CV characteristics
3.1. Sputtering process with different oxygen flow
Figure 7 shows CV curves of sputtered iridium oxide thin
Oxygen flow and its partial pressure are two key parameters film microelectrodes under oxygen flows varied from 5 to
in the process of the reactively sputtered iridium oxide. The 40 sccm. It can be seen that the electrochemical behavior of
oxygen pressure under different oxygen flow could imply the microelectrode highly depends on the oxygen flow and its
target and film characteristics of the sputtering process, as pressure.
shown in figure 4. It can be seen that the initial oxygen pressure For the case of low oxygen flow, only part of the iridium in
is about 0.1 Pa only, which shows that almost all oxygen the reactively sputtered thin film is under oxidation state. Since
participates in the oxidation reaction of iridium. The oxygen there is metallographic phase iridium existing in the film, the
pressure increases obviously when the oxygen flow arrives at CV shapes are narrow and the redox peaks are broad. When
15 sccm. Based on the insert figure in the figure 4, the nonlinear the oxygen flow arrives at 25 sccm, all iridium is changed to
relationship between oxygen flow and pressure implies that the oxidation state and shows a wide CV shape. Meanwhile,
little oxygen takes part in the oxidation reaction, which is also the sharp peaks disappear due to the high electrochemical
called the ‘target poisoning process’. During this deposition activity of the redox reactions, which results in large pseudo
process, the initially produced iridium oxide is absorbed on capacitance and a large CSC [1, 11–13, 25–30]. It is also
the surface of the iridium target which prevents oxidation observed from figure 5(c) (25 sccm) that this film can be easily
reactions. As a result, the accumulating oxygen exists in the permeated by water and ionic species, which contributes to

4
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

(a) (b)

(c) (d )

Figure 5. SEM images of the samples sputtered at different oxygen flows to the chamber. (a) 10 sccm, (b) 15 sccm, (c) 25 sccm, (d) 40 sccm.

(a) (b)

(c) (d)

Figure 6. AFM images of the samples sputtered at different oxygen flows. (a) 10 sccm, (b) 15 sccm, (c) 25 sccm, (d) 40 sccm.

5
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

Table 1. Summarized morphology and surface microstructure parameters of the samples shown in figures 5 and 6.

Oxygen flow (sccm) O2 pressure (Pa) Surface texture Roughness (nm)

10 0.5 Fractal surface with some tiny feather-shaped grains 20.9

15 1.2 Dendritic surface with not clear and well defined grain boundary 17.1
25 1.8 Dendritic surface 14.0
40 3 Dendritic surface with increasing aggregation 20.5

pressure. In this case, the film is electrochemically unstable.

The iridium at the high valence oxidation state is transformed
into the stoichiometric state during the activation process.
Thus, the distinguished peaks in the CV curves are obtained.
The aggregation of iridium oxide on the substrate shown in
figure 5(d) leads to the decline of the CSC. CSC after 100
cycles of activation is measured and shown in figure 8. The
measurements in figure 8 are taken from five samples (each
oxygen flow) under the same process run. The maximum CSC
occurs at the oxygen flow of 25 sccm. At that point the oxygen
pressure is 1.8 Pa while the chamber pressure is 4.2 Pa (the ratio
of O2:Ar pressure is 3:4). It should be noted that the point is also
the second point after the so-called target poisoning process.
The 15 sccm point is the target poisoning point, and the
20 sccm point is the transition point. This means the maximum
CSC occurs just at the start of the compound mode [16]. At this
Figure 7. CV data of iridium oxide thin film microelectrodes
fabricated at different oxygen flows (mean ± sd n = 5). The films
state, the reactively sputtered iridium oxide process consumes
were activated with 100 cycles. the least oxygen and the appropriate oxygen pressure to turn
all the metallic iridium into the iridium oxide.
The minimum consumption of oxygen generates the
minimum released heat during the exothermic reaction. At
an oxygen partial pressure of 1.8 Pa (oxygen flow is 25 sccm);
the amount of heat absorbed by the PR is acceptable to avoid
the carbonization. Thus, the reactively sputtered iridium oxide
thin film can be patterned by the lift-off process. There was no
evidence that a baking temperature less than 65 ◦ C and a baking
time less than 1 h could prevent the carbonization of PR. In the
standard lift-off process, the wafer was dipped into acetone and
immersed into an ultrasonic bath until the PR was completely
removed. After the sputtering process, the fully carbonized PR,
partially carbonized PR and normal PR existed on the wafer
at the same time. It should be noticed that the fully carbonized
PR could not be removed by the lift-off process. Thus, the lift-
off process was focused on the partially carbonized PR and
normal PR. The higher the carbonization degree reaches, the
longer the immersion duration. The measurements in figure 9
Figure 8. Charge storage capacity CSC after 100 cycles of activation are taken from six samples (each oxygen flow) from the same
with respect to the oxygen flow to the deposition chamber process run. The immersion duration required to complete this
(mean ± sd n = 5). process was impacted by the sputtering process parameters
used for metal deposition (figure 9).
For the O2 flow less than 20 sccm, the film pattern can
higher charge delivery [16]. The maximum CSC of 36.147 ± be well realized. However, the metallographic phase iridium
1.015 mC cm−2 occurs at the oxygen flow of 25 sccm, as exists in the film during the process, which results in the
shown in figure 8. relatively poor electrochemical property. When the O2 flow
Along with the further increase of oxygen flow and is larger than 20 sccm, all iridium is transformed into the
pressure, the aggregation phenomenon of the film surface oxidation state. But as the further increasing O2 flow, the
microstructure is obvious. The oxidation state iridium with immersion duration gets longer. As a result, the defects of
high valence results from the superfluous oxygen flow and patterns will increase. Compared with the other sputtering

6
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

Figure 9. Duration of ultrasonic bath process with respect to the Figure 11. Double layer capacitance calculated from impedance
oxygen flow to the deposition chamber (mean ± s.d. n = 6). magnitude spectra versus oxygen flow to the deposition chamber
(mean ± sd n = 5).

iridium oxide is not only affected by the deposition condition

and electrochemical activation process, but also the working
voltage [31–35]. Because the working voltage during EIS
measurement is 10 mV, the electrochemical activity is in a
smaller voltage range than the ‘water window’ region for the
CSC measurement. Therefore, the changing tendency is not in
accordance with the CSC in the mid-range-frequency.
The microelectrode impedance is dominated by the double
layer capacitance (CDL) at the low-frequency. The capacitance
C can be calculated from |Z| = (ωC)−1 at the frequency
ω = 1 s−1 [16]. Based on the impedance magnitude spectra
in figure 10, the capacitances are calculated and shown in
figure 11. The measurements in figure 11 are taken from
five samples (each oxygen flow) from the same process run.
It is obtained that the maximal double layer capacitance
and CSC occur at the oxygen flow supply of 25 sccm and
Figure 10. Impedance magnitude spectra of the reactively sputtered
iridium oxide thin film at different oxygen flow (mean ± sd n = 5). pressure of 1.8 Pa. The changing tendencies of the double layer
capacitance and CSC are similar. It shows that the double layer
capacitance could be employed as an indirect measurement of
conditions, the pattern under 25 sccm O2 flow is realized at the
the electrochemical activity for the sputtered iridium oxide. In
lowest duration of ultrasonic agitation with 7.25 ± 0.49 min.
other words, lager CDL means lager CSC.

3.4. Electrochemical impedance spectroscopy

3.5. Voltage transients of the microelectrode under electrical
The obtained EIS under the oxygen flow from 5 to 40 sccm stimulation waveforms
is shown in figure 10. The impedance of each curve varies in
a smaller range and they are enclosed in a small envelope. An example of the voltage transient in response to a biphasic,
It shows that there are different electrochemical activities symmetric current pulse is shown in figure 12. The current
of the reactively sputtered iridium oxide thin film for all pulse amplitude is 100 μA, and the pulse width includes
curves. In particular, the impedance magnitude at the low- 100 μs, 200 μs and 400 μs. Figure 12(a) shows the voltage
frequency (below 10 Hz) and high-frequency (over 10 kHz) transient of the 1 k pure resistance. The response time is
range decreases when the oxygen flow varies from 5 to defined as the shift time from the negative phase to positive
20 sccm. After that, it shifts to increase around the 25 sccm phase of the voltage response. The current pulses were applied
oxygen supply. This result is in accordance with the changing by the Master-8 programmable pulse-generator (Master-8 8-
tendency of the CSC shown in figure 8. channel programmable pulse-generator, two channels with ten-
In the mid-range-frequency (10 Hz–10 kHz), the changing turn dial, Israel). The biphasic pulse was obtained by a negative
tendency of the CSC cannot match the impedance. This is pulse and a delayed positive pulse. The response time of the
attributes to that the conductivity of the iridium oxide depends pure resistance was zero when the delayed time was equal to
on the electrode potential. The electrochemical activity of the the width of the negative pulse.

7
J. Micromech. Microeng. 24 (2014) 025015 X Kang et al

4. Conclusion

Iridium oxide (IrOx) thin films have been deposited by

a reactively RF-sputtering process for the modification
material of the microelectrode in the application of functional
electrical stimulation. The optimal condition of IrOx thin films
deposition is that the oxygen flow is 25 sccm and the sputtering
pressure is 4.2 Pa. The highest charge storage capacity arrives
at 36.15 mC cm−2. At this condition this film has excellent
electrochemical properties, and the pattern of this film is
formed by the lift-off process. Moreover, the testing results
of electrical stimulation show that the optimally processed
iridium oxide film is a promising microelectrode material
with 35% of the energy consumption of the film sputtered at
40 sccm oxygen flow.
(a)

Acknowledgments

The authors thank to financial support from the National

Natural Science Foundation of China (nos 51035005 and
61176104), 973 Program (2013CB329401), Science and
Technology Commission of Shanghai Municipality grant
(nos 13511500200 and 11JC1405700), WUXI-SJTU project
(2011JDZX017), HF Key Lab (HF2012-k-01), NDPR
Foundation of China (no 9140A26060313JW3385), SJTU-
Funding (YG2012MS51). The authors are also grateful to the
colleagues for their essential contribution to this work.

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