Effect of sputtering pressure on the structure and properties of SiO2 films prepared

by magnetron sputtering
Leran Zhao1,2, Changjiang Zhao1,2, Juncheng Liu1,2 ✉, Zhigang Liu3, Yan Chen3
1
School of Materials Science and Engineering, Tiangong University, Tianjin 300387, People’s Republic of China
2
State Key Laboratory of Membrane Separation and Membrane Process, Tianjin 300387, People’s Republic of China
3
Institute of Spacecraft System Engineering, Beijing 100086, People’s Republic of China
✉ E-mail: jchliu@tjpu.edu.cn

Published in Micro & Nano Letters; Received on 12th April 2020; Revised on 25th May 2020; Accepted on 7th June 2020

The effects of sputtering pressure on the O/Si ratio, microstructure, surface morphology and optical properties within 300–1100 nm of SiO2
film via radio frequency magnetron sputtering were investigated. The results showed that the molar ratio of O/Si in the film increased from 1.96
to 2.03, from silicon rich to oxygen rich, with the sputtering pressure increase from 0.3 to 1.3 Pa. The SiO2 films deposited at different pressure
were all amorphous. There were many ditches with a length of about 50 nm on the surface of the film deposited at lower pressure. The increase
of sputtering pressure could reduce the number of ditches, and make the surface denser and more uniform. The refractive index increased first,
then decreased and finally increased with the increase of sputtering pressure, and the maximum and minimum values were obtained at 0.7 and
1.1 Pa, respectively. The change of absorptivity was approximately the same as that of the refractive index, while the change of the average
transmittance of coated quartz glass was exactly the opposite of refractive index. The minimum value of the average transmittance 92.6% and
the maximum value 93.1% were obtained at 0.7 and 1.1 Pa, respectively.

1. Introduction: Solar cells and batteries are the main power
sources for satellites, spaceships, space stations, landing probes
and so on. It is always the goal of space solar cells to improve
the efficiency of photoelectric conversion to reduce the weight
sufficiently. There are two main ways to improve the photoelectric
conversion efficiency of the solar cells. One is to improve the
efficiency of the cell itself, the other is to reduce the loss of incident
light, that is, to reduce reflection. To reduce reflection, one method
is coating the surface of the cell glass cover with a film, the other is
processing the surface of the glass cover or the solar cell into a light
trapping structure which can increase the surface roughness and
scattering, double the optical path and enhance the absorption of
light [1]. For the space solar cell, in order to improve its service
life and resist the damage of space radiation or high-energy
particles, it is generally necessary to cover the top of cell with a
glass cover, so the main way to reduce the reflection is to use anti-
reflection film. In addition, the special application environment
requires the glass cover and its antireflection film to have enough
hardness and wear resistance, chemical stability, thermal shock
resistance and high radiation resistance [2], as well as strong
adhesion between them. Therefore, quartz glass is a nice candidate
material for space solar cell glass cover.
MgF2 and SiO2 are common coating materials. MgF2 is the
naturally occurring substance with the lowest refractive index. Its
refractive index at 550 nm is only 1.38 and transparent spectrum
is 0.21–10 μm [3]. However, there is a high tensile stress between
MgF2 film and quartz glass substrate, which makes the film,
especially the composite film easy to break [2]. Compared with
MgF2, SiO2 film has smaller decomposition pressure, better chem-
ical stability, higher hardness and higher wear resistance. Secondly,
the refractive index of SiO2 is also very low, about 1.46 at 550 nm,
and its transparent spectrum is 0.16–9 μm [3]. SiO2 film is often
used in combination with other oxide films with high refractive
index in the ultraviolet–near infrared spectrum to obtain better
anti-reflection effect [4].
Magnetron sputtering is a promising technique to prepare
inorganic films because of its some intrinsic advantages, such as
high density of the prepared film and its strong adhesion to the sub-
strate [5], easy control of the process, low cost [6], low preparation
temperature [7] and be conducive to multilayer film’s preparation
[8]. This method has been widely used in the field of solar cells.
For example, in order to improve the conversion efficiency of
cells, Cui et al. [9] prepared a homogeneous and uniform NiO
blocking interlayer fabricated with the reactive magnetron sputter-
ing method in CH3NH3PbI3 planar solar cell. Scholtz et al. [10]
prepared the barium titanate film, which reduced effectively the
reflectance loss for solar cells. Kang et al. [11] prepared the TiO2
antireflection layer on amorphous silicon/amorphous silicon
germanium tandem solar cells, which improved the efficiency of
the cell by 0.25%. The film’s structure and properties prepared
with magnetron sputtering can be significantly affected by the
sputtering pressure and other process parameters. Tang et al. [12]
prepared ZnO film with radio frequency (RF) magnetron sputtering
and observed that the increase of sputtering pressure led to the grain
size’s increase, while its quality would decrease when the pressure
was too high. Moon et al. [13] investigated the effect of sputtering
pressure on optical properties of aluminium-doped ZnO thin film,
and reported that the density and transmittance of the film increased
with the decrease of pressure. Chaiyakun et al. [14] found that
the crystallinity of TiO2 film deposited by reactive magnetron
sputtering decreased and the anatase phase appeared when the
sputtering pressure increased.
If the glass cover of space solar cell is made of quartz glass, it is
difficult to realise the effective antireflection of the glass cover with
SiO2 film alone. However, SiO2 film could be combined with other
materials, such as TiO2, to form a multilayer film, which is expected
to obtain a good antireflection effect. Wang et al. [15] found that
the maximum visible light transmittance of TiO2 coated glass
was 88.5%, while TiO2/SiO2 double-layer film could make the
transmittance reach 92.3%. Li et al. [16] prepared a TiO2–SiO2
stack coating which increased the solar transmittance of glass
slide substrate by 7.8%, thus increased the efficiency of Cu(In,
Ga)Se2 by 0.95%. Mazur et al. [8] prepared an antireflection multi-
layer film based on the combination of TiO2 and SiO2, and increas-
ing the visible light transmittance by 3%.
In order to prepare high-quality composite film, SiO2 film with
controllable chemical composition and optical parameters (refract-
ive index, absorptivity, transmittance etc.) should be prepared at

872 Micro & Nano Letters, 2020, Vol. 15, Iss. 12, pp. 872–876
& The Institution of Engineering and Technology 2020 doi: 10.1049/mnl.2020.0222
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Fig. 1 XPS spectra of SiO2 films
a Full spectrum of the film deposited at 0.3 Pa
b Si 2p spectrum of the film deposited at 0.3 Pa
c Si 2p spectra of the film deposited at 1.1 and 1.3 Pa

first. Therefore, we deposited SiO2 thin films on the quartz 3. Results and discussion
glass substrates and monocrystalline silicon wafers with RF 3.1. Effect of sputtering pressure on chemical composition of SiO2
magnetron sputtering, and investigated the effects of sputtering film: Fig. 1 presents the XPS spectra of SiO2 films. The black dash
pressure on chemical composition, phase component, surface dot line is the original data line; the red solid line and blue dotted
morphology and optical properties within 300–1100 nm wave- line are the fitting lines.
length of the film. The full spectrum of the film deposited at 0.3 Pa is shown in
Fig. 1a. The peaks’ positions of other full spectra are the same as
2. Experimental those in Fig. 1a, but the peaks’ intensity is different. It can be
2.1. Preparation of SiO2 film: SiO2 thin films were deposited known that the surface of all the films deposited at various sputter-
on pure quartz glass substrates (99%, 25 × 50 × 1 mm) with RF ing pressures contains only O, C and Si elements, among which,
magnetron sputtering and SiO2 target (99.99%, Ф101.6 × 3 mm, C is derived from organic pollutants on the surface. In order to
Nanchang Guocai Technology Co., Ltd., China). In order to analyse the change of valence state of Si element in the thin film,
measure the film’s refractive index, a single-sided polished silicon the narrow spectrum of Si 2p was fitted with peak separation.
wafer with the size of 10 × 10 mm was placed beside the quartz The charge-up shifts of Si 2p narrow spectrum were calibrated
glass substrate. High purity Ar2 (99.999%) and O2 (99.999%) via the binding energy of Si 2p in SiO2 being set to 103.3 eV
were used as the sputtering and the reactive gases, respectively. before the peak separation fitting [18]. From Fig. 1b, it can be
After the base vacuum was less than 6.6 × 10−4 Pa, these gases seen that the original Si 2p peak pattern is asymmetric, and it can
were introduced into the sputtering chamber to deposit SiO2 film. be divided into two peaks during fitting.
Cao et al. [17] found that with the change of O2/Ar gas flow, the The high peak with the binding energy EB1 of 103.3 eV can be
composition of SiO2 films varies from nearly pure Si to SiO2. attributed to Si4+. The weak peak with the binding energy EB2 of
The total gas flow was fixed at 80 SCCM, and O2 flow ratio at 101.3 eV is located between 101.8 eV corresponding to Si2+ and
60% because according to our previous work, the molar ratio 100.9 eV corresponding to Si1+ [19], and closer to 100.9 eV. The
of oxygen to silicon (hereinafter referred to as the O/Si ratio) narrow spectrum of the film prepared when the sputtering pressure
in SiO2 film was closest to 2 under these two parameters. The is lower than 1.1 Pa is similar to Fig. 1b. However, in Fig. 1c, there
sputtering pressure was set to 0.3, 0.5, 0.7, 0.9, 1.1 and 1.3 Pa, is only a symmetric peak at 103.3 eV in each Si 2p spectrum when
respectively, and the sputtering power was kept at 150 W. The the sputtering pressure is 1.1 and 1.3 Pa, respectively. Themo
transmittance of thin film is a function of the thickness. In Avantage 5.52 software was used to calculate the atomic mole
order to avoid the thickness effect on the transmittance, the percentages of O, Si and C in the films prepared under different
sputtering time and rotation speed of substrates were reasonably sputtering pressures. The results are listed in Table 1. From the
controlled during the experiment, so that the thickness of the above analysis and Table 1, it can be concluded that in the case
films was as consistent as possible under different sputtering of low pressure, the O/Si ratio in SiO2 film is <2.0, and the film con-
pressures. tains SiO and other silicon oxides in addition to SiO2. The O/Si
ratio of the film gradually increases with the increase of sputtering
2.2. Characterisation: X-ray photoelectron spectroscopy (XPS; pressure. When the sputtering pressure increases to 1.1 Pa, the O/Si
K-alpha, Thermofisher, USA) was used to analyse the surface ratio of the film reaches 2.02 and the film is no longer deficient
chemical composition of SiO2 film. X-ray diffractometer (XRD; in oxygen. This result can be understood from the following
D8 discover, Bruker AXS, Germany) was used to identify the
film’s phase component. Scanning electron microscopy (SEM;
GeminiSEM 500, Carl Zeiss Jena, Britain) was used to observe Table 1 Atomic mole percentages of O, Si and C in SiO2 films and O/Si
the film’s surface morphology. The film’s thickness and refractive ratios
index within 300–1100 nm spectrum were determined by spectrum
Sputtering pressure, Pa 0.3 0.5 0.7 0.9 1.1 1.3
ellipsometry (COSE-D-VN-D-C-AF-M-R-T, Syscos Instrument
Technology (Shanghai) Co. Ltd., China). The absorptivity and
O 1s (at %) 56.15 60.60 60.45 57.22 60.48 61.04
transmittance of coated quartz glass substrate (hereinafter referred
Si 2p (at %) 28.57 30.70 30.61 28.72 29.89 30.01
to as the transmittance of film) in the range of 300–1100 nm were
C 1s (at %) 15.28 8.70 8.66 14.06 9.63 8.94
measured with ultraviolet–visible–near infrared spectrophotometer O/Si 1.96 1.97 1.97 1.99 2.02 2.03
(Lambda 750, Perkin Elmer, USA).

Micro & Nano Letters, 2020, Vol. 15, Iss. 12, pp. 872–876 873
doi: 10.1049/mnl.2020.0222 & The Institution of Engineering and Technology 2020

discussion. At low sputtering pressure, the deposition rate is high
and the gas density in the chamber is small, which lead to fewer col-
lisions between Si or SiO sputtered from the target and ionised O2−
[2]. Eventually, the incident particles Si or SiO will be deposited on
the substrate without complete oxidation. Moreover, the O/Si ratio
of the film prepared at 1.1 and 1.3 Pa is slightly greater than the
ideal stoichiometric ratio, 2.0. The gas density increases with the in-
crease of sputtering pressure, and the number of collisions between
Ar+ from the plasma and other particles increases at the same time
in the process of flying towards the cathode target, which leads to
the lower kinetic energy of Ar+ before hitting the target. As a
result, both the Si, SiO, SiO2 and other particles sputtered out per
unit volume and sputtering yield decrease. As can be seen from
Table 2, the deposition rate of the film is slightly reduced with
the increase of sputtering pressure. However, in contrast, the
amount of ionised O2− in the atmosphere increases, and some of
the O2− may be deposited into the film as they impinge on the sub-
strate surface, causing the film to be oxygen-rich.
3.2. Effect of sputtering pressure on phase component of SiO2 film:
Fig. 2 presents the XRD patterns of SiO2 films. It is clear that every
pattern has a weak diffraction peak at 2θ = 69.1°. The substrate
temperature during deposition process should be much lower than
573°C. If the film crystallised to some extent, the crystal phase
should be α-quartz. Compared with PDF #81-0066 card, all the
XRD patterns display no obvious diffraction peak at 2θ = 27.3° or
2θ = 21.6°, corresponding to quartz (011) or (100) lattice plane,
respectively, which means the SiO2 films deposited at various
sputtering pressures are all in amorphous. This is because the
substrate was not heated [20]. The diffraction peak at 2θ = 69.1°
should be attributed to (400) lattice plane of the monocrystalline
silicon wafer substrate [21].
3.3. Effect of sputtering pressure on surface morphology of SiO2
film: Fig. 3 presents the SEM images of SiO2 films deposited at
different sputtering pressures. It is observed that many ditches
with a length of about 50 nm exist on the surface of the films
prepared at the lower sputtering pressures. When the sputtering
Table 2 Thickness and deposition rate of SiO2 films
sputtering pressure, Pa 0.3 0.5 0.7 0.9 1.1 1.3
average thicknessa, nm 75.13 76.23 78.40 78.56 73.44 73.06
sputtering time, s 1760 1900 1950 1950 2000 2050
deposition rate, Å/s 0.43 0.40 0.40 0.40 0.37 0.36
a
Measure the thickness at three different locations for each sample and
calculate its average.
Fig. 2 XRD patterns of SiO2 films prepared under different sputtering
pressures
874
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Fig. 3 Effect of sputtering pressure on the surface morphology of SiO2 film
a 0.3 Pa
b 0.7 Pa
c 1.1 Pa
d 1.3 Pa
pressure is 0.7 Pa, the ditches are the most and clearest. When the
sputtering pressure is 1.1 Pa, ditches have disappeared and the
film surface becomes denser. When the sputtering pressure is
1.3 Pa, the film surface is smooth and continuous without
obvious defects. The number of ditches on the film surface
increases first and then decreases, and finally the ditch disappears
to form a uniform film.
At lower pressure, the kinetic energy of particles deposited on the
substrate is larger, but not enough to help particles escape from the
substrate, resulting in a large residual stress on the film [22].
Moreover, the oxygen content in the film prepared at a sputtering
pressure lower than 1.1 Pa is insufficient. The internal stress in
SiO film is tensile due to the lack of oxygen, whereas the internal
stress in SiO2 film is compressive [23]. This may be the reason
for the appearance of ditches in the film. In addition, the growth
of vacuum-deposited film involves atoms diffusing over the
surface until they become trapped in low energy lattice sites [24].
As the sputtering pressure increases from 0.3 to 0.7 Pa, the impin-
ging particles gradually become less energetic, and their transverse
diffusion of particles on the film surface decreases, increasing the
number of ditches and surface defects significantly. The mobility
of particles on the surface can be enhanced by the substrate tem-
perature increase [25], although the substrate is not heated during
sputtering, the impact of incident particles will increase its tempera-
ture. Bhatt and Chandra [25] demonstrated that the substrate tem-
perature reached equilibrium about 20 min after the beginning of
sputtering, and the test results indicated that the substrate tempera-
ture increased slightly with the increase of sputtering pressure.
Therefore, as the sputtering pressure increases from 0.7 to 1.3 Pa,
the deposited particles could fully diffuse on the surface and
coalesce in ditches or join with the ditch edges, making the film
gradually dense and uniform under the combined effect of internal
stress transition and the substrate temperature increasing.
3.4. Effect of sputtering pressure on optical properties of SiO2 film:
The thickness and deposition rate of SiO2 films prepared at different
sputtering pressures are listed in Table 2. According to Table 2, the
average thickness for all samples is 75.8 nm, and the maximum dif-
ference of the film thickness is 5.5 nm (78.56–73.06 nm). With the
increase of sputtering pressure, the deposition rate of the sample
decreases slightly, from the highest 0.43 Å/s to the lowest 0.36 Å/s.
Fig. 4 shows the effect of sputtering pressure on the refractive
index of SiO2 film. As can be seen from Fig. 4, firstly, the refractive
index of all samples decreases gradually with the increase of wave-
length, and all the refractive index curves have no intersection
Micro & Nano Letters, 2020, Vol. 15, Iss. 12, pp. 872–876
doi: 10.1049/mnl.2020.0222
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of the film surface; then, the surface defects gradually decrease,
and the absorptivity decreases accordingly; finally, the film no
longer lacks oxygen, and the surface becomes more uniform, and
the stoichiometric ratio and surface microscopic morphology do
not change much further, making the absorptivity curve change
little.
Fig. 6 shows the transmittance spectra of SiO2 films. From Fig. 6,
it can be found that the transmittance of all samples in the 300–
1100 nm spectrum is above 90% and the longer the wavelength,
the higher the transmittance. Furthermore, the transmittance of
films prepared at low sputtering pressures in the ultraviolet region
decreases sharply due to the influence of absorptivity, which has
a great influence on the average transmittance.
In order to visually analyse the influence of sputtering pressure
on the film’s optical properties and considering the blue shift of
Fig. 4 Effect of sputtering pressure on the refractive index of SiO2 film the solar spectrum in space, the average transmittance in the
range of 300–1100 nm was calculated according to the transmit-
tance spectrum from each film, and listed in Table 3 together
points. Secondly, the refractive index of the thin film increases first, with the refractive index and the absorptivity at 550 nm. 550 nm
then decreases and finally increases with the increase of sputtering is often used as the reference wavelength when designing multilayer
pressure, and the maximum and minimum values are obtained at 0.7 antireflective films or coatings [27]. Fig. 7 is based on the data in
and 1.1 Pa, respectively. In general, the refractive index of the film Table 3. As can be seen from Fig. 7, although the change trend
is influenced by its stoichiometric ratio and density. When the film
density is approximately the same, the refractive index of the
silicon-rich film will be higher [5]. Therefore, when the pressure
is lower than 1.1 Pa, that is, when O/Si ratio is < 2.0, the refractive
index of the film is generally higher than that of the film when O/Si
ratio is > 2.0. Defects will affect the propagation of light in the film.
According to Sections 3.2 and 3.3, it is known that the film quality
is the worst at 0.7 Pa. As the sputtering pressure increases from 1.1
to 1.3 Pa, the refractive index of the film increases slightly, resulted
from the lower porosity of the film due to the decrease of deposition
rate [26]. The larger the film’s density, the higher the film’s refract-
ive index.
Fig. 5 shows the effect of sputtering pressure on the absorptivity
of SiO2 film. It can be seen clearly that the absorptivity of the
film decreases with the increase of wavelength, and it changes
rapidly in the ultraviolet region due to the short-wave cut-off
characteristic of SiO2 film [13]. In addition, when the sputtering
pressure increases from 0.3 to 0.9 Pa, the absorptivity changes sig-
nificantly, that is, it first increases and then decreases as the Fig. 6 Effect of sputtering pressure on the transmittance of SiO2 film
pressure increases, and the maximum value of absorptivity is
obtained at 0.7 Pa. However, when the sputtering pressure increases
further from 0.9 Pa, the absorptivity curve of the film does not Table 3 Refractive index, absorptivity (550 nm), average transmittance
change much. (300–1100 nm) of SiO2 films
Both the non-uniform structure and the deviation of stoichiomet-
ric ratio will also affect the absorptivity besides the intrinsic absorp- sputtering pressure, Pa 0.3 0.5 0.7 0.9 1.1 1.3
tion [2, 3]. With the increase of sputtering pressure, first, the refractive index, % 1.43 1.46 1.53 1.39 1.37 1.39
absorptivity increases with the increase of ditches in the unit area absorptivity 0.033 0.033 0.034 0.032 0.032 0.032
average 92.9 92.8 92.6 93 93.1 93
transmittance, %

Fig. 5 Effect of sputtering pressure on the absorptivity of SiO2 film Fig. 7 Effect of sputtering pressure on optical properties of SiO2 films

Micro & Nano Letters, 2020, Vol. 15, Iss. 12, pp. 872–876 875
doi: 10.1049/mnl.2020.0222 & The Institution of Engineering and Technology 2020

of absorptivity is only slightly different from that of the refractive
index, they are basically the same on the whole, while the change
trend of average transmittance is exactly the opposite of that of
the refractive index. As the sputtering pressure increases, the
average transmittance decreases first, then increases, and finally
decreases. The minimum value of 92.6% and the maximum one
of 93.1% are obtained at 0.7 and 1.1 Pa, respectively. Although
the change from 92.6 to 93.1% seems very small, it means that
the increase in the uniformity of transmittance over the entire
region.
4. Conclusion: In summary, the SiO2 films with controllable
refractive index were obtained, which was very important for us
to prepare the composite film containing SiO2 layer. The main
conclusions are as follows:
(1) The defect of low O2 content in the film could be improved and
the O/Si ratio increased from 1.96 with less oxygen to 2.03 with rich
oxygen with the sputtering pressure’s increasing.
(2) The SiO2 films prepared at different sputtering pressures were all
amorphous. The sputtering pressure increase could reduce the
number of ditches on the film surface and make the surface more
dense and uniform. This was mainly affected by both the stress in
the film and the diffusion of the deposited particles on the surface.
(3) The refractive index of the thin film increased first, then
decreased and finally increased with the increase of sputtering pres-
sure. The absorptivity change of the film was basically the same as
that of the refractive index, while the average transmittance change
was completely the opposite.
5. Acknowledgments: This work was supported by Major Science
and Technology Projects of Military Civilian Integration of Tianjin
(grant no. 19ZXJRGX00040), and partly supported by the National
Natural Science Foundation of China (grant no. 51352002).
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Micro & Nano Letters, 2020, Vol. 15, Iss. 12, pp. 872–876
doi: 10.1049/mnl.2020.0222