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Procedia Engineering 168 (2016) 1086 1089

30th Eurosensors Conference, EUROSENSORS 2016

RF Sputtering of ZnO (002) Thin Films on top of 3C-SiC-on-Si

(100) Substrates for Low Cost Piezoelectric Devices
V. Valliyil Sasi+, A. Iqbal+, K. Chaik, P. Tanner, A. Iacopi and F. Mohd-Yasin*
Queensland Micro- and Nanotechnology Centre, Griffith University, Brisbane, QLD 4111, Australia

Abstract

In this paper, we deposited c-axis oriented ZnO thin films on top of epitaxial 3C-SiC/Si (100) substrates using RF magnetron
sputtering. We investigated the effect of O2/Ar ratio and the post-annealing temperature. The grazing angle incident x-ray
diffraction results show that ZnO thin-films are highly oriented along the (002) crystalline direction between the O2/Ar ratio of 30
% to 50 %, at the post-annealing temperature of 600 C in nitrogen environment. The recipe from this work can be used to
develop low cost piezoelectric devices such as an energy harvester.

2016
2016TheTheAuthors. Published
Authors. by Elsevier
Published Ltd. This
by Elsevier Ltd.is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of the 30th Eurosensors Conference.
Peer-review under responsibility of the organizing committee of the 30th Eurosensors Conference
Keywords: Physical vapor deposition processes; Polycrystalline deposition; X-ray diffraction; ZnO; Silicon carbide;

1. Introduction

Zinc oxide (ZnO) falls under II-VI semiconductor group, which has a wide band gap of 3.3 eV and an excitation
binding energy of 60 MeV at room temperature [1]. Due to its excellent electrical and optoelectronics properties,
ZnO can be used for many applications such as gas sensors, solar cells, and optical wave guides [2]. It is also used in
fabrication of surface acoustic wave (SAW) devices, film bulk acoustic resonators (FBARs) and piezoelectric
transducers [3].
ZnO has been deposited via different methods. Sputtering has the advantages of relatively simple apparatus, low
substrate temperature and high deposition rate with good surface flatness and transparency [4]. ZnO thin-films are

+
Both first and second authors contributed equally in the paper
* Corresponding author. E-mail address: f.mohd-yasin@griffith.edu.au

1877-7058 2016 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of the 30th Eurosensors Conference
doi:10.1016/j.proeng.2016.11.346
 V. Valliyil Sasi et al. / Procedia Engineering 168 (2016) 1086 1089 1087

normally deposited on silicon (Si) substrate because of its low cost per surface area and ease of fabrication.
However, the large difference of 39 % in lattice mismatch and 68 % in thermal expansion coefficients (CTE)
between ZnO and Si deteriorate the crystal quality because of dislocations and stresses that generates cracks in
deposited films. Therefore, ZnO films have been deposited on other substrates to mitigate both effects. One such
candidate material is a cubic silicon carbide (3C-SiC).
From the literature, there were two groups that sputtered c-axis ZnO on top of 3C-SiC buffer layer on Si
substrate. Sha et al. compared the Full Wave Half Maximum (FWHM) values of ZnO (002) diffraction peaks on top
of Si (111) and 3C-SiC-on-Si (111) substrates [5]. They measured the FWHM values of 0.65 to 0.55 on both
substrates, respectively. Phan et al. deposited c-axis oriented ZnO on top of polycrystalline 3C-SiC with (111)
orientation on Si (100) substrates using RF sputtering and sol-gel [6]. They reported the FWHM values of 0.2107
and 0.3498 of ZnO (002) diffraction peaks, respectively for both methods. In this paper, we would like to further the
investigation by studying the effect of oxygen concentration and post-annealing temperature on the crystal quality of
ZnO films being deposited on 3C-SiC (100)/Si(100) substrate. The targeted applications are for the low-cost
piezoelectric devices such as energy harvester.

2. Experimental procedures

We deposit c-axis oriented ZnO film on top of a 3C-SiC-on-Si substrate having the dimension of 15 mm by 15
mm using Denton RF sputterer operating at 450 W. Prior to this work, the 3C-SiC thin film of thickness 300 nm was
epitaxially grown on top of 150 mm Si(111) wafers using a custom-made hot-wall horizontal low pressure chemical
vapour deposition (LPCVD) system at Griffith University. The samples was piranha cleaned and the sputtering
system was pumped down to the base pressure of 510-5 Torr using turbo-pump for 15 minutes to reduce residual
gasses in the chamber. We used a Zn target of 100 mm in diameter with 99.995 % purity and set the distance from
the target to the substrate to 8 cm. All the sputtering was performed at 4 mTorr while the substrate temperature was
set to 200 C to follow industry practice. The chamber was pumped with Ar for 6 minutes with the substrates
shutter being closed in order to clean the Zn target from previous reactions. We increased the O2/Ar ratio from 30 %
to 60 % in a step of 10 % to evaluate the effect of O2 concentration on the crystal orientation, with a total gas flow of
34 sccm. All the sputtering was done for 30 minutes and the samples were kept for 90 minute in order to allow the
substrate temperature to cool down to 50 C, before the samples were taken out of the chamber. The second
experiment was designed to investigate and enhance the crystal quality of ZnO (002) using post-annealing treatment
as demonstrated by Fang et al.s systematic studies [7]. We annealed our samples prepared at 40 % O2/Ar ratio at
400 C, 600 C and 800 C in the annealing chamber (custom-made glass tube) for 60 min, while the nitrogen gas
was pumped into the chamber with a flow of 1700 cc/min. The samples were then cooled down at a rate of 6 C/min.
The deposited ZnO films were characterized by the following parameters (equipment): x-ray diffraction (Bruker D8
Advance X-Ray diffraction tool) and film thickness (Dektak profilometer).

3. Results and discussion

Table I shows the summary of the data that can be divided into two parts. The first part details the characteristics
of the samples that were prepared at 30 %, 40 %, 50 % and 60 % O2/Ar ratio and post-annealed at 600 C. The
second part summarizes the characteristics of the samples that were prepared at 40 % O2/Ar ratio and subsequently
post-annealed at 400 C, 600 C and 800 C. The following parameters, namely peak position for (002) orientation,
area under the curve for (002) orientation, FWHM of diffraction peak of (002) and peak intensity (002) are extracted
from the XRD plots of the samples. We extract the values of the FWHM of the diffraction peaks using Gaussian
fitting. The grazing incident X-ray diffraction (GIXRD) measurement at 1 incidence was employed due to smaller
thickness of ZnO films compared to the substrates. The grain size was calculated from the FWHM of (002)
diffraction peak using the Sherrer equation [8].
1088 V. Valliyil Sasi et al. / Procedia Engineering 168 (2016) 1086 1089

Table 1. Summary of data for ZnO (002) film on top of 3C-SiC(100)-on-Si(100) substrate

Sample ID O2/Ar Annealing Peaks position Area for (002) Thickness FWHM of Peak Grain
On ratio temperature (002) (%) (nm) Diffraction Intensity size
peak
SiC(111) (%) (C) (cps) (nm)
(O)
VA2 30 600 34.56 60 810 0.29 1987 29.98
VA4 40 600 34.59 75.5 960 0.295 1996 29.47
V1 50 600 34.58 96 720 0.29 12451 29.98
V3 60 600 - - - - - -
C4 40 400 34.49 44 960 0.34 285.6 25.56
VA4 40 600 34.59 75.7 960 0.295 1996 29.47
C5 40 800 34.51 75 960 0.4 740 21.73

2500
2000 (002) 30 % O2
1500
1000 (101)
500
(100) (102)
(a.u.)

0
2500
2000 40 % O2
(002)
1500
1000
Intensity

500 (101)
(101)
140000
12000
(002) 50 % O2
10000
8000
D

6000
4000
2000
0
(101)
15 60 % O2
10
5
0
27 30 33 36 39 42 45 48 51 54 57 60

2(Deg)
FIG. 1 Grazing angle XRD of ZnO deposited on 3C- FIG 2: Grazing angle XRD of AlN deposited at 40 % on 3C-SiC
SiC(100)/Si(100) film at different O2/Ar ratio (100)/Si (100) film at different annealing temperature

Several important observations can be deduced from Table I. Fig 1 shows the diffraction peaks of all the samples
at 30 %, 40 %, 50 % and 60 % O2/Ar ratio at the post-annealing temperature of 600 C. The diffraction peak at 2
i.e. 34 represents the ZnO (002) orientation is maximum for 30 %, 40 % and 50 % O2/Ar ratio. The FWHM of the
(002) diffraction peak is measured as 0.29, 0.28 and 0.29 for these concentrations, respectively. The best
deposition is perhaps at 50 % O2/Ar ratio, before the crystal quality degraded afterwards. This trend can be
explained as follows. As the amount of O2 increases from 30 % upwards, the deposition rate decreases, which
provides more time for the adatoms to accommodate themselves into the low-energy configured close packed lattice
sites before the arrival of the next layer of reactive species [9]. Once it reached 60 % O2 concentration, the
frequency of collision between the Ar and O2 increases which decreases the kinetic energy of the adatoms, which is
required for making the B1 and B2 bonds to create the (002) orientation [9]. It is also evident from Table 1 that the
area under the curve increases with increase in O2 concentration. Furthermore, the grain size doesnt change with
increasing O2 concentrations.
Figure 2 shows the XRD spectra of the samples prepared on SiC(100)/Si substrate at 40 % O2 concentration,
annealed at three different temperatures. The FWHM of the (002) diffraction peak is measured as 0.34, 0.295, 0.4
at 400 C, 600 C and 800 C, respectively. The annealing temperature of 600 C assists in enhancing the c-axis
 V. Valliyil Sasi et al. / Procedia Engineering 168 (2016) 1086 1089 1089

oriented crystalline quality. The quality seems to deteriorate after 800 C as demonstrated by the FWHM values, as
well as the reducing value of the peak intensity and the reducing percentage of (002) oriented area under the curve,
which can be credited to the presence of porosity [7].

4. Conclusion

We have demonstrated the RF sputtering of a c-axis oriented ZnO thin film on top of an epitaxial 3C-SiC-on-Si
(100) substrate. The FWHM values of ZnO (002) diffraction peaks for the samples from 30 to 50 % O2/Ar ratio
show minimal changes, with the mean of 0.29 and standard deviation of 0.03. The post-annealing temperature of
600 C has been found to be the most optimized condition for the ZnO (002) deposition, which is in agreement with
Fang et al. [7]. The targeted application for the ZnO thin film is for low-cost piezoelectric devices.

Acknowledgements

This work is supported by Queensland Micro- and Nanotechnology Centre (QMNC) and Griffith School of
Engineering. This work was performed in part at the Queensland node of the Australian National Fabrication
Facility, a company established under the National Collaborative Research Infrastructure Strategy to provide nano
and microfabrication facilities for Australias researchers. The authors would like to express our gratitude to Zailan
Mohd Yusof of The National University of Malaysia for the XRD measurements.

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