Journal of Alloys and Compounds 892 (2021) 162228

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Journal of Alloys and Compounds

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

Antireflective and anti-dust modified silica based thin film on solar cell
cover glass ]]
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⁎
Hosein Salehi, Akbar Eshaghi 1, , Mohammad Rezazadeh, Hosein Zabolian
Department of Materials Engineering, Malek Ashtar University of Technology, Iran

a r t i cl e i nfo a bstr ac t

Article history: In this research, a thin film of silica modified with HMDS and PDMS was deposited on the glass substrates
Received 15 July 2021 by a spraying method. The thin film characterization was performed using X-ray diffraction, UV–VIS–NIR
Received in revised form 12 September 2021 spectrophotometer, field emission scanning electron microscopy and infrared fourier transform spectro­
Accepted 30 September 2021
scopy methods. Self-cleaning, thermal shock, anti-dust and pencil hardness tests were performed on the
Available online 6 October 2021
samples. The results showed that the average transmittance of the glass coated sample in the wavelength
range of 400–1000 nm was 96%, which increased as 5.4% in comparison to the uncoated glass. The modified
Keywords:
Anti-dust silica thin film has a uniform distribution of the silica nanoparticles with different sizes between 10 and
Hydrophobic 70 nm on the surface, which has a water contact angle and a slip angle of 96° and 5°, respectively. In the
Modified silica self-cleaning test, it was observed that water droplets slipped on the surface and carried contaminants
Self-cleaning while for the uncoated sample, this property is not observed. In the simulated anti-dust test, it was ob­
Thin film served that for coated glass, less dust particles are deposited on the surface than in the uncoated sample.
Also, in thermal shock test, temperature cycles of −10 and 60 °C were performed at 10 times and it was
observed that after eighth cycle, the coated sample lost its hydrophobic properties.
© 2021 Elsevier B.V. All rights reserved.

1. Introduction been used as self-cleaning coatings. However, most self-cleaning

Solar cells have received a lot of attention for generating elec­
tricity using natural sunlight [1–6]. Solar cell technology has led to
extensive research to increase the solar cell efficiency over the
decades. It is well known that glass shields are used as glass covers
to protect solar modules [7–9]. However, the accumulation of dust
particles on the glass cover due to the absorption and scattering of
light will reduce the efficiency and electrical power output of solar
cells [10–14]. The use of new technologies for easy and cheaper
cleaning of solar cell cover glass is developing and progressing. One
of these cases is the use of transparent self-cleaning, hydrophobic
and anti-dust thin films [15–18]. Transparent hydrophobic thin films
will increase the efficiency of solar cells through their anti-reflective
and self-cleaning properties. Anti-reflective properties will reduce
the unwanted reflections from solar cell surface and self-cleaning
effect will prevent the dust particles accumulation on solar cell
surface and light losses due to scattering and absorption will be
minimized [19–21]. Currently, several hydrophobic thin films have
⁎
Corresponding author.
E-mail addresses: Eshaghi.akbar@gmail.com, Eshaghi@mut-es.ac.ir (A. Eshaghi).
1
ORCID: 0000–0001-8145–8387
hydrophobic thin films lose their function under environmental
conditions [22,23]. Sand particles can damage self-cleaning coating.
Destructive UV radiation lead to the destruction of these coatings,
while in most areas there is no possibility of rain and the self-
cleaning effect of the coating alone is not enough to prevent the dust
particles accumulation [24–27]. According to the research that has
been done in the field of hydrophobic and self-cleaning coatings, it
can be seen that a little research has been done in the field of hy­
drophobic coatings resistant to environmental conditions. Eshaghi
et al. [28] prepared a thin film based on trimethoxymethylsilane on a
glass substrate by a sol-gel method. The prepared thin film showed
super-hydrophobicity (CA = 153 and SA = 6.5), high transparency
(95% transmission at 550 nm), and effective dust removing by water
droplets. Therefore, this film can be used as a self-cleaning and anti-
reflective coating for applications in solar cells cover glass. Zhang
et al. [2] showed that the efficiency of solar cells with self-cleaning
protective glass was higher than that of uncoated glass in the dust
test. Lu et al. [29] applied an antistatic coating on solar cells using
HMDS-modified silica nanoparticles. The result showed that
moisture and surface energy of dust particles had the greatest effect
on the dust particle accumulation. Yuan et al. [30] showed that
coatings with a surface roughness of less than 1.5 nm indicated
excellent dust removal performance. Also, hydrophobic methyl

https://doi.org/10.1016/j.jallcom.2021.162228
0925-8388/© 2021 Elsevier B.V. All rights reserved.
H. Salehi, A. Eshaghi, M. Rezazadeh et al.
Fig. 1. Water droplet images on the coated glass (a) and bare glass (b) surfaces.
Fig. 2. Transmittance spectra of the coated and bare glass samples.
groups can increase the dust removal performance of coatings.
However, coatings lose their dust removal function in humid air.
Therefore, the aim of this study was to fabricate a hydrophobic silica
base thin film with simultaneous of transparency, self-cleaning and
anti-dust properties, using TEOS, HMDS and PDMS precursors.
Fig. 3. Reflectance spectra of the coated and bare glass samples.
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Journal of Alloys and Compounds 892 (2021) 162228
Simultaneous modification of the film with HMDS and PDMS in­
creased the hydrophobicity of the glass coated substrate and in­
creased the contact angle of the glass substrate from 30° to 96°. The
resulting thin film with self-cleaning and anti-dust performance has
a high potential in optical devices such as solar cells for use in
outdoor environments.
2. Experimental method
2.1. Materials
High purity materials, including tetraethylorthosilicate (TEOS,
98%, Sigma Aldrich), Hexamethyldisilazane (HMDS, 98%, Sigma
Aldrich), polydimethylsiloxane (PDMS, 98%, Merck) and ethanol
(99%, Merck), (hexane, 95%, Sigma Aldrich) were used to fabrication
of the hydrophobic thin films.
2.2. Preparation of the glass substrates
Before the film deposition, the soda lime glass substrates were
cleaned. The primary contaminants were also washed with soap and
water. Then, the prepared substrates were rinsed with ethanol and
deionized water for 5 min and dried at 100 °C for 30 min
2.3. Preparation of the modified silica sol
To prepare hydrophobic silica sol, TEOS (2 ml) was added to
ethanol (30 ml), and after stirring the solution, HMDS (1 ml) was
slowly added to the solution and stirred again for half an hour. Then,
distilled water was added to the solution and finally the solution was
stirred for 2 h to form a clear sol (Sol A). In the next step, PDMS
(3 ml) and curing agent (1 ml) was slowly added to the hexane and
(10 ml) stirred for half an hour (Sol B). Finally, Sol B was added to the
sol A under stirring and the solution stirred for 2 h.
2.4. Hydrophobic film deposition
Film deposition on the glass substrate was performed by a spray
method (air pressure 5 psi, solution speed: 15 ml/sec, dis­
tance:10 cm, spray angle: 45°). The resulting films were dried at
room temperature for 5 h.
2.5. Film characterization
The surface morphology of the thin film was observed using field
emission scanning electron microscopy (FE-SEM, Hitachi S4160, cold
field emission, voltage 15 kV). Infrared Fourier Transform
Spectroscopy (FTIR, Perkin Elmer Model Specuum400) was used to
evaluate the surface functional groups on the film surface. The
H. Salehi, A. Eshaghi, M. Rezazadeh et al.
Fig. 4. ATR-FTIR spectra of the unmodified and modified silica thin films.
transmittance and reflectance of the thin films in the wavelength of
300–800 nm were measured by using a UV–VIS–NIR spectro­
photometer (Shimadzu UV-3100). Water contact angles (WCA) were
measured using a video and photo-based contact angle measure­
ment system (Dino-lite, AM-4515T8-Edge). Water contact angle was
measured at least 3 times across the surface of the sample using a
distilled water drop of 3 microliters. Water contact angle ( ± 1
standard deviation) was measured at ambient temperature of 30 ℃
and relative humidity of 50%. Iron oxide powder was also used for
self-cleaning test. The iron oxide powder was evenly sprayed on the
film surface. Then, water drop was applied on the surface by an in­
jector needle tube at a distance of 1 cm and the surface was inclined
gently (30°) to drop downwards. Photographs were taken before and
after dropping on the surface. Comparison of the photos taken by the
droplet motion and the effect of the iron oxide powder in different
samples were qualitatively compared. The hardness of the thin films
was measured by a pencil hardness method according to the ASTM D
3363 standard. To simulate the thermal shock test, the samples were
heated from ambient temperature (27 °C) to 60 °C (rate of 20 °C /
Fig. 5. FE-SEM images of the thin film surface at magnifications of (a) 50,000 and (b) 150,000.
3
Journal of Alloys and Compounds 892 (2021) 162228
min) in an oven (Memmert, Germany) and put at this temperature
for 10 min. The samples were then taken out of the oven and cooled
to ambient temperature and the contact angle was measured. Then,
the samples were cooled in a dry ice mixture to −10 °C. The samples
were kept at this temperature for 10 min and then removed from
this state to reach ambient temperature, after which the contact
angle was measured. This cycle was repeated for 8 times [20]. To
investigate the anti-dust properties, the dust simulation test was
used [19]. For this purpose, first, dust particles with a mesh size of
140, 90, 45 and 180 µm and a total weight of 4 g were poured into
the chamber test. The two coated and coated glass specimens were
placed inside the chamber at 45º angles. After that, the lid of the
chamber was closed and the fan was turned on so that the dust
particles inside the chamber were constantly moving in a suspended
manner. The test was performed for 3 min. The anti-dust process
was recorded using a camera.
3. Results and discussion
Fig. 1 shows water droplet images on the coated and bare glass
substrates. The water contact angles on the coated and uncoated
samples are about 96° and 30°, respectively. It means that by ap­
plying the thin film, the glass surface has changed from hydrophilic
to hydrophobic state. The change from hydrophilic to hydrophobic
state is due to the formation of methyl groups that reduce the sur­
face energy. It will be discussed in the following.
The reaction mechanism of the HMDS precursor films is as fol­
lows: C2H6O solvent does not react with the TEOS and C2H6O is used
only for the reaction of TEOS with HMDS monomer. TEOS monomer
with chemical composition of C8H20O4Si, consists of two alkane
groups and two methyl groups attached to four carbon atoms and a
central silicon ion. The TEOS hydrolysis reaction is as follows [31]:
nSi(OC2H5 )4 + 2nH2 O nSiO2 + 4nC2H5OH (1)
HMDS monomer is an organic-silicon compound with the che­
mical formula of C6H19NSi2, consisting of four methyl groups and
two alkane groups attached to a central silicon ion. It is formed
during the reaction of ammonia with trimethyl chloride. Therefore,
four methyl groups play an important role in network formation and
wettability. The four methyl monomer groups of the HMDS are ex­
pected to be hydrolyzed by the following three-step reac­
tions [31,32]:
H. Salehi, A. Eshaghi, M. Rezazadeh et al. Journal of Alloys and Compounds 892 (2021) 162228

Fig. 6. Particle size histogram in the range of 0–160 nm (internal image is the output of Anix Emica software).

Hydrolysis: particles are transformed into hydrophobic groups by forming of

Si O Si(CH3 )3bonds. Further bonding of the Si(CH3 )3can
(CH3)3SiNHSi(CH3 )3 + 2H2O 2HO Si(CH3)3 + NH3 (2)
bond on the silica surfaces by the condensation reaction between
Water condensation: hydroxyls in the sol aging process. In this process, Si-O-Si and H2O
bonds can be formed [32].
Si(OCH2 CH3)4 + 4H2O Si(OH)4 + 4CH3CH2OH (3)
The transmittance and reflectance spectra of the bare and coated
Hydrophobic bonds Formation: glass samples are shown in the Figs. 2 and 3. As can be seen, at a
wavelength of 700 nm, the transmittance of the coated sample is
Si OH + HO Si(CH3)3 Si O Si(CH3)3 + H2O (4)
about 96%, while for the uncoated sample is 90.5%. In addition, the
Therefore, it can be concluded that this sol is produced by con­ reflectance of the coated glass sample is lower than that of the un­
densation reactions between TEOS and HMDS hydrolysis. Only part coated sample. On the other hand, it can be concluded that the thin
of the hydrophilic silanol (Si-OH) groups on the surfaces of the silica film shows an anti-reflective effect.

Fig. 7. The self-cleaning process for the uncoated sample at different times; a) at the moment of the water droplet contact on the surface, b) 3, c) 5, d) 7, e) 11 and, f) 13s.

4
H. Salehi, A. Eshaghi, M. Rezazadeh et al. Journal of Alloys and Compounds 892 (2021) 162228

Fig. 8. The self-cleaning process for the coated sample at different times; a) at the moment of the water droplet contact on the surface, b) 0.27, c) 0.42, d) 0.66, e) 1.1 and, f) 1.47s.

It is well known that the transmittance increases with decreasing
the surface roughness and refractive index. The films with nan­
ometer scale roughness may effectively reduce the light scattering at
the surface, resulting in an enhanced transmittance. In addition, the
transmittance may also be influenced by the refractive index. Many
researchers indicated that silica sol-gel derived thin films indicated
porous structure. Therefore, the porosity of the coated glass gives
rise to low refractive index. Thus, the reflection on the glass sub­
strate decreased and transmittance increased [33,34].
The surface groups formed on the glass substrates were in­
vestigated using ATR-FTIR method. Fig. 4 shows the ATR-FTIR spectra
of the silica and modified silica thin films. The absorption bands
observed around the wavenumber of 2900 cm−1 and 1400 cm−1 are
due to the stretching vibration of the -CH3 groups. The absorption
peaks at the wavenumber of 780 cm−1 indicates the stretching
vibration of the Si-C and the kinetic vibration of the -CH3. The ab­
sorption bands observed around 1270 cm−1 and 1400 cm−1 are due to
the symmetric and asymmetric deformation of the Si-CH3 bonds
[28–30]. The C-H and Si-C peaks are perfectly visible for the silica
modified with HMDS and PDMS. This indicates that Si-CH3 groups on
the coating surface reduce surface free energy, which effectively
increases hydrophobicity. ATR-FTIR spectra of the silica and modified
silica thin films show a very strong absorption band near around
1050 cm−1 due to the stretching vibration of the Si-O-Si bonds [32].
The observed peaks at about 900 cm−1, 1650 cm−1 and broadband
absorption band at 3400 cm−1 are due to the -OH groups. OH groups
are completely visible for unmodified silica, which disappear after
surface modification by HMDS and PMDS [10]. Hydroxyl groups on
the unmodified silica surface form hydrogen bonds with water
molecules, increasing wettability and decreasing the contact angle of

Fig. 9. Pencil hardness abrasion test process for a the coated sample at different times; A) at the start, b) 3, c) 5, d) 7, e) 9 and, f) 11s.

5
H. Salehi, A. Eshaghi, M. Rezazadeh et al.
Fig. 10. Thermal stability of the thin film at different temperatures within 1 h.
the water droplet. The thin film modified by HMDS and PDMS has
the ability to achieve hydrophobic and superhydrophobic properties
due to the presence of very low surface free energy due to the for­
mation of the Si-CH3 groups and nano-metric roughness due to the
presence of hybrid nanometer particles.
Fig. 5 shows FE-SEM images of the modified silica thin film. As
can be seen from the images, the coated sample has a relatively
uniform distribution of the nanoparticles. However, the particles in
some areas are agglomerated. The particle size was measured using
Anix Emica software. Fig. 6 shows a histogram of the particle size
with an internal image of the software output. As can be seen, the
smallest and largest particle sizes are 3 and 158 nm, respectively.
Also, the average particle size is 31 nm. The results show that the
relative percentage of the particle size in the range of 160–60 nm is a
13%. On the other hand, the highest percentage of the particle size is
about 20%, which is related to the range of 10–15 nm. These nano­
particles provide a rough surface with a nanometer scale that, ac­
cording to the Casey-Baxter model, can trap air and create
hydrophobic properties. As the results show, the reason for the
significant increase in the transmittance is the particle size of less
than 30 nm, which reduces the Mie and Rayleigh scattering [35].
Figs. 7 and 8 show the time interval during the self-cleaning
process for the uncoated and coated samples, respectively. As can be
seen from the Fig. 7, due to the lack of the water droplet movement
at the beginning of the test, 11 drops of water were finally dropped
by the needle tube so that the fluid had the necessary force to move
on the surface. The water droplets move down the slope at a slight
speed and finally stand at the bottom of the surface for 13 s by
wetting the surface sample. It can be seen that the iron oxide par­
ticles remain completely and stick on the sample surface due to
Fig. 11. FE-SEM images of the coated sample at 500 °C.
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Journal of Alloys and Compounds 892 (2021) 162228
Fig. 12. Thermal shock effect on the water contact angles.
surface wetting. Fig. 8 shows a completely different behavior on the
coated sample. As can be seen from the Fig. 8, the whole test process
was performed with two drops. A drop of water simply rolls on the
surface of the coated sample. The particles adhere to the surface of
the water droplet and roll downwards in the same way and are
completely removed from the surface. This indicates the self-
cleaning behavior of the coated surface. The water droplet on the
coated surface has enough acceleration and movement to leave
the surface, so that the water droplet reaches the bottom of
the surface in 1.47s Fig. 8-f shows the final result of the self-cleaning
test for the coated sample.
Fig. 9 shows a pencil abrasion test for the coated sample. The
hardness of the coated sample was measured as 6 H. Therefore, it can
be concluded that the coated sample has an excellent scratch and
abrasion resistance [26,36].
Fig. 10 shows the thermal stability of the coated sample. As
shown in Fig. 10, the coated sample had maintained its thermal
stability up to 450 °C. In addition, the water contact angle was in­
creased on the coated surface. The reason for increasing the contact
angle after annealing is due to the evaporation of the OH bonding
groups. However, the water contact angle was decreased after 500 °C
(4.6°) and the coated sample was altered from hydrophobic to su­
perhydrophilic state. The reason that the coated sample turns to the
superhydrophilic state can be related to the decomposition of the
methyl groups. Methyl groups, Si- (CH3)3, and other organic groups
are decomposed in the oxidation process and leading to the water
adsorption and the films become super-hydrophilic state [28]. In
H. Salehi, A. Eshaghi, M. Rezazadeh et al.
Fig. 13. Anti-dust test results for the uncoated and coated samples.
addition to the methyl groups decomposition, changing the mor­
phology of the film at 500 °C is also effective in creating a super­
hydrophilic state. Fig. 11 shows FE-SE images of the thin film at
500 °C. As can be seen, the protrusion is formed on the film surface,
which is caused by SiO2 particles smaller than 100 nm. The very
small size of the nanoparticles greatly increases the surface area.
Also, the large number of the hydroxyl groups on the film surface
form hydrogen bonds with water molecules, which greatly increases
wettability and decrease the water contact angle to 4.7º [37].
Fig. 12 shows the water contact angle relative to the number of
the thermal shock test cycles at temperatures of 60 and −10 °C.
Contact and slip angles were also measured during each cycle. As can
be seen from the figure, the coated sample retained its hydrophobic
properties in 7 cycles. In the first to fifth cycles, the slip angle did not
change. In the sixth cycle, after cooling the sample, it was observed
that a part of the surface is frozen and it was observed that the slip
angle increased. In the seventh cycle, the slip angle of the coated
sample decreased and the adhesion of water droplets decreased
again compared to the previous cycle. In the eighth cycle, after
cooling, the icy areas on the surface increased. The coated sample
has lost its hydrophobic properties and the droplet moves on the
surface at a slower speed than in the sixth cycle. On the other hand,
the path of the droplet on the sample surface is quite clear. Ac­
cording to the above explanations, it can be concluded that in the
first to fifth cycles, methyl groups have maintained their stability,
but in the sixth cycle onwards, thermal shock has caused the de­
struction of the hydrophobic groups.
Fig. 13 shows the time interval during the self-cleaning process
for the uncoated and coated samples. As can be seen from the Fig. 13,
dust particles are deposited on the uncoated surface, while for the
coated sample, it is observed that no particles are deposited on the
surface. Therefore, it is obvious that by applying a hydrophobic
coating, the adhesion force can be reduced and then the particle
deposition rate can be reduced [29]. This indicates the anti-dust
properties of the coating.
In this research, we have obtained a hydrophobic thin film with
simultaneous thermal shock resistance and anti-dust properties
which did not report in the literature. The resulting thin film with
self-cleaning and anti-dust performance has a high potential in op­
tical devices such as solar cells for use in outdoor environments.
4. Conclusion
In this research, a thin film of silica modified with HMDS and PDMS
was deposited on the glass substrates by a sol gel method. The modified
silica thin film has reduced the reflectivity of the glass substrate about 3%
and increased the transmittance from 90.5% to 96%. The water contact
7
Journal of Alloys and Compounds 892 (2021) 162228
angle on the coated glass substrate increased from 30º to 96º. The coated
glass samples maintained their hydrophobic and optical properties up to
450 °C. In addition, the coated glass samples retained their hydrophobic
properties up to 7 cycles in the thermal cycle test. The coated samples
showed self-cleaning and anti-dust properties. It is concluded that the
silica modified with HMDS and PDMS can be used as a self-cleaning and
anti-dust coating on solar cell cover glass and optical instruments.
Declaration of Competing Interest
The authors declare that they have no known competing fi­
nancial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
The authors would like to acknowledge the Iran National Science
Foundation (INSF, Grant Number: 98026126) for the financial sup­
port of this research.
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