2015 2nd International Conference on Material Engineering and Application (ICMEA 2015) ISBN: 978-1-60595-323-6

Effect of Sputtering Power on Microstucture and Electrochemical Characteristic of Nickel Films Deposited by Magnetron Sputtering 

Yongping Luo, Shunjian Xu, Zonghu Xiao, Wei Zhong, Hui Ou & Yuan Xiao 

Xinyu Institute of New Energy, Xinyu University, Xinyu, Jiangxi, China 

ABSTRACT: Nickel (Ni) film electrodes were deposited onto FTO by the magnetron sputtering 

method. The  influence of  sputtering power on  the morphology  and electrochemical perfor‐

mances of the as‐prepared films has been  investigated in this work. The surface crystal struc‐

ture and morphology of the prepared films were  investigated by using X‐ray diffraction (XRD) 

and scanning electron microscope (SEM). The results have shown that with the increase of the 

sputtering power from 80 W to 140 W, the increases of the film surface roughness and porosi‐

ty. The films deposited at sputtering power of 140 W possess the highest specific surface area 

and abundant pore structure, leading to better electrochemical performance of Ni film. 

1 INTRODUCTION

In recent years, Ni nanoparticles have become one of the interesting metallic nanomaterials in

many promising fields including chemical catalysis, electrocatalysis, conducting paints, magnet-

ic recording, rechargeable batteries, medical diagnosis, superconducting devices, and so on

(Gao et al., 2010; Chen et al., 2007). Ni particles were reported to be excellent catalysts for hy-

drogenation of nitrobenzene and nitrophenol, oxygen reduction, and oxidation of olefins (Zhu et

al., 2011). Besides this, cheaper nickel nanoparticles are also used as a component of the modi-

fied electrodes for alcohol sensing (Shibli et al., 2006) and fuel cell development (Suleimanov

et al., 2008) particularly in alkaline medium although electrocatalytic activity of bare Ni foil is

insignificant at low potential (Bagchi & Bhattacharya).

Up to now, several elegant methods have been established for the preparation of high-quality Ni

nanoparticles, such as polyol method (Couto et al., 2007), chemical reduction (Wu et al., 2010),

ball milling (Yue et al., 2011), electrodeposition (Li & Dai, 2005), decomposition of organome-

tallic precursors (de Caro & Bradley, 1997), chemical vapor deposition (Singjai et al., 2007),

thermal plasma (Choi et al., 2003), modified electroless plating (Wu et al., 2009), microwave-

assisted synthesis (Xu et al., 2008), and magnetron sputtering (Tkach et al., 2015). And so on.

Magnetron sputtering method shows remarkable advantages, such as method is simple, low

cost, easy to promote, and facilitate preparation of thin films.

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In the present study, the magnetron sputtering method was used to prepare Ni film under the

conditions of working pressure of 1.8 Pa, deposition time of 20 min, and different sputtering

power (80 W, 100 W, 120 W, and 140 W). XRD and SEM were used for the characterization of

the surface crystal structure and morphology of the prepared Ni films. The comprehensive study

of the electrochemical activity of Ni films under the different sputtering power was performed

by using cycle voltammetry (CV).

2 EXPERIMENTS

2.1 Film deposition Processing

The deposition of Ni films was carried out by using a magnetrons sputtering system come from

SKY technology development Co., Ltd (Shenyang, china), which was equipped with a rotary

vane pump as well as a turbo-molecular pump. Deposition was carried out by Ni targets used as

RF sources in an Ar atmosphere (gas flow: 30 sccm). Ni targets were obtained from Zhongnuo

Advanced Material Technology Co., Ltd. (Beijing, china), and had purity of 99.99%. FTO con-

ductive glass (25 × 20 mm) was obtained from CSG Holding Co. Ltd. (Shenzhen,china), and

used as substrate. Prior to Ni film deposition on FTO substrates, the target was sputter cleaned

for 20 min with shutter in a closed position. The films were deposited at a substrate temperature

of 300ºC. Working pressure of 1.8 Pa, deposition time of 20 min, sputtering power of 80 W, 100

W, 120 W and 140 W were applied.

2.2 Ni film Characterization

The morphology of as-prepared Ni films was characterized by using EVO MA 10 (Zeiss, Ger-

many) equipped with energy dispersive spectroscopy (EDS). X-ray diffraction (XRD) was car-

ried out by a Bruker D8 (German) X-ray diffractometer using Cu Kα radiation source and λ =

1.5406 Å at 30 kV and 30 mA. Electrochemical measurements were performed on an electro-

chemical analyzer (CHI660A, Shanghai, China) in deaerated aqueous solution containing 1 M

NaOH with a three-electrode configuration, in which Ni film as working electrode, a Pt wire as

the counter electrode and a Ag/AgCl electrode as reference electrode. All measurements were

carried out at ambient temperature.

3 RESULT AND DISCUSSION

3.1 XRD analysis of Ni films

The as-prepared Ni/FTO samples show almost the same XRD patterns as shown in Figure 1.

The peaks located at 44.4º, 51.7º and 76.4º attributed to the (111), (200), and (220) reflections of

the Ni phase (PDF 65-0380), respectively. The peaks of FTO and NiOOH can be seen in the

samples.

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20 30 40 50 60 70 80

FTO

111

200

220 * NiOOH

* 

2θ / deg.

Inte

nsity

/ α.

u.

a

b

c

d

Figure 1. XRD of Ti films under the conditions of working pressure of 1.8 Pa, deposition time of 20 min

and different sputtering power: (a) 80 W, (b) 100 W, (c) 120 W, (d) 140 W.

3.2 Effect of sputtering power on the morphology of Ni films

Figure 2 shows SEMs of Ni films obtained under the conditions of working pressure of 1.8 Pa,

deposition time of 20 min, and different sputtering power (80 W, 100 W, 120 W, and 140 W). It

can be seen from Figure 1(A) to (D), the increases of the film surface roughness and porosity

with the increase of the sputtering power. The film is thicker at relatively higher sputtering

power.

It is mainly attributed to the increase of the sputtering power increases the current between sub-

strate and target, ionized argon ion will be increasing. The bombardment of argon ion to the tar-

get surface becomes more intensified, the target atom will be more stripped from the target sur-

face. With the increase of the deposition rate, the particles sputter from the target will be

depositied on the particle cluster of NiO. The formation of island growth promotes a large of

pores were produced on the film surface.

Figure 2. SEMs of Ni film with different sputtering power: (A) 80 W, (B) 100 W, (C) 120 W, (D) 140 W.

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3.3 Effect of technology parameters on the electrochemical characteristic of Ni films

Figure 3 shows the CVs of Ti film with different sputtering power in 1 M NaOH solution at the

scan rate of 50 mV s-1. From the CVs, a pair of redox peaks was observed at 250 mV and 400

mV, which attributed to the Ni2+/Ni3+ redox couple. The redox peak current is biggest at the

sputtering power of 140 W, which probably due to the large specific surface area and abundant

porous microstructure of the Ni film prepared on the condition of the sputtering power of 140

W.

100 200 300 400 500 600-2.0

-1.5

-1.0

-0.5

0.0

0.5

1.0

1.5

2.0

2.5

E /V vs. Ag/AgCl

a

I / m

A

d

Figure 3. CVs of Ni film with different sputtering power: (a) 80 W, (b) 100 W, (c) 120 W, (d) 140 W.

4 SUMMARY

In this study, it was investigated that the effect of sputtering power on the morphology and elec-

trochemical properties of Ni films. The Ni films were prepared by using magnetron sputtering

on FTO substrates under sputtering power from 80 W to 140 W. The film deposited at a higher

sputtering power possessed a higher specific surface area and abundant pore structure, leading

to better electrochemical performance of Ni film.

ACKNOWLEDGEMENTS

This work was financially supported by Natural Science Foundation of China (51263021), Nat-

ural Science Foundation of Jiangxi (20141521050002).

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