Solar Energy Materials & Solar Cells 111 (2013) 160–164

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Solar Energy Materials & Solar Cells

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

Sol–gel preparation of SiO2/TiO2/SiO2–TiO2 broadband antireflective coating

for solar cell cover glass
Longqiang Ye a, Yulu Zhang a, Xinxiang Zhang a, Teng Hu a, Rui Ji a, Bin Ding b, Bo Jiang a,n
a
Key Laboratory of Green Chemistry & Technology, College of Chemistry, Sichuan University, Chengdu 610064, China
b
Research Institute of Petroleum Exploration and Development of PetroChina, Beijing 100083, China

a r t i c l e i n f o a b s t r a c t

Article history: Triple-layer broadband abrasion-resistant antireflective (AR) coatings with excellent transmittance at
TM
Received 31 May 2012 400–800 nm were designed with the aid of thin film design software (TFCalc ). SiO2, TiO2 and SiO2–
Received in revised form TiO2 hybrid thin films with refractive indices of 1.44, 2.20 and 1.71 for the up, middle and bottom
21 December 2012
layers, were dip-coated from SiO2, TiO2 and SiO2–TiO2 hybrid sols by sol–gel process, respectively. SiO2
Accepted 21 December 2012
and TiO2 sols were prepared using tetraethyl orthosilicate (TEOS) and tetrabutyl orthotitanate (TBOT)
Available online 4 February 2013
as precursors and hydrochloric acid as catalyst. These designed triple-layer broadband AR coatings with
Keywords: an average transmittance as high as 98.4% at visible region were successfully obtained. Hexamethyldi-
Broadband antireflective coating silazane (HMDS) was further used to modify the surface of the AR coatings, which greatly improved the
Sol–gel process
hydrophobicity of the coatings, and thus gave the AR coatings some self-cleaning property. These triple-
Hydrophobicity
layer abrasion-resistant broadband AR coatings with excellent transmittance in the visible region have
Thin film design
Abrasion-resistance potential value in the field of solar cells.
& 2013 Elsevier B.V. All rights reserved.

1. Introduction cells [7–10]. For a quarter-wave (l/4) AR coating having a

Photovoltaic power has been getting more and more impor-
tant due to the growing depletion of oil resources and increasing
environmental consciousness. In the industries of solar cells,
photovoltaic devices are located outdoors; therefore glass covers
are essential for preventing damage from physical shock and
corrosion. There are, however, approximately 8% reflection on two
surfaces of the cover glass since the refractive index of cover glass
is around 1.52 while that of air is 1.0. The introduction of
antireflective (AR) coatings can effectively reduce these losses
and thereby improve the efficiency of the solar cells. AR coatings
derived from sol–gel process have attracted much interest due to
their advantages of low cost, simple operation process and
controllable microstructure, and been widely applied in energy-
related applications [1–6].
AR coatings used in solar cells must be high abrasion-
resistance to endure the outdoor conditions and cleaning pro-
cesses. The acid catalyzed silica sol derived coating is an ideal
material due to its low refractive index, excellent abrasion-
resistance and good durability. Titania coating is transparent to
visible light with high refractive index and low absorption
properties. Consequently, the acid catalyzed silica and titania
coatings are very convenient materials for AR coatings in solar
n
Corresponding author. Tel.: þ86 28 85418112; fax: þ86 20 85412907.
E-mail address: jiangbo@scu.edu.cn (B. Jiang).
refractive index equal to the square root of refractive index of
substrates, the transmittance can be reached as high as 100% at
the given wavelength. However, the average transmittance is low
in the entire visible region; this short back restricts their real
applications in the field of solar cells. Double-layer or multi-layer
broadband AR coatings have been also designed and prepared
[11,12] to reach a relatively high average transmittance in the
visible region.
In solar cells, the glass cover is an essential component as
important as silicon wafer. The preparation of AR coatings with
both excellent optical performance and abrasion-resistance on
silicon wafer has been widely reported [13–17,12] while these
coatings on cover glass receive relatively less attention. The glass
cover has a relatively low refractive index of about 1.52, and
based on optical theory and by considering available film mate-
rials, the preparation of AR coatings on substrates with low
refractive index is much harder than on substrates with relatively
high refractive index due to the absence of robust film materials
with low refractive index [18]. l/4–l/4 and l/4–l/2 double-layer
AR coatings have been reported for low refractive index substrate
[19,20], but these coatings cannot balance the abrasion-resistance
and broadband transmittance at visible region very well. Multi-
layer AR coatings become then a good choice. In 1940s, Lockhart
and King described a l/4–l/2–l/4 triple-layer broadband AR
coating which possessed satisfied transmittance at visible region
[21]. However, due to the limit of available film materials at that
time, they did not succeed to optimize the refractive indices

0927-0248/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.solmat.2012.12.037
 L. Ye et al. / Solar Energy Materials & Solar Cells 111 (2013) 160–164
Fig. 1. The procedure of preparation of SiO2, TiO2 and SiO2–TiO2 hybrid sols.
of three layers. Precedent studies have shown that silica/titania
hybrid film with refractive index varying from 1.44 to 2.20 can be
obtained by mixing silica and titania sols together [22,23].
In this work, we tried to optimize Lockhart’s triple-layer AR
coating by investigating effect of refractive index of three layers
on the average transmittance and broadband property with the
TM
aid of thin film design software (TFCalc ), and an optimum triple-
layer broadband AR coating on solar cell cover glass was designed
having an average transmittance of 99.1% in the visible region of
400–800 nm. Then this SiO2/TiO2/SiO2–TiO2 triple-layer coating
with an average transmittance of more than 98.4% was success-
fully prepared by the sol–gel process.
2. Experimental details
2.1. Preparation of sol
Fig. 1 shows the procedure of the preparation of SiO2, TiO2 and
SiO2–TiO2 hybrid sols.
2.1.1. Preparation of SiO2 sol
A solution of TEOS, C2H5OH, H2O and HCl was first prepared
and stirred for 2 h at 30 1C. The molar ratio of TEOS: H2O:
C2H5OH: HCl was 1: 4.01: 36.83: 4.16  10  3 [24] and the final
concentration of SiO2 was 3% by weight. The resultant sol was
aged in a sealed glass container at 30 1C for 7 days and then
filtered through a 0.22 mm PVDF filter prior to use.
2.1.2. Preparation of TiO2 sol
A solution of TBOT, C2H5OH, H2O and HCl was first prepared
and stirred for 2 h at 30 1C. The molar ratio of TBOT:H2O:-
C2H5OH:HCl was 1:3.55:49.75:0.22 and the final concentration
of TiO2 was 3% by weight. The resultant sol was aged in a sealed
glass container at 30 1C for 7 days and then filtered through a
0.22 mm PVDF filter prior to use.
2.1.3. Preparation of SiO2–TiO2 Hybrid sols
SiO2 sol and TiO2 sol were mixed with various weight ratios
and stirred for 2 h at 30 1C. The mixed sols were aged in sealed
glass containers at 30 1C for 7 days. The hybrid sols were finally
filtered through a 0.22 mm PVDF filter prior to use.
161
2.2. Preparation of AR coatings
Borosilicate glasses were cleaned by ultrasonication in acetone
for 10 min, then wiped carefully with cleanroom wipers and dried
under a stream of compressed air prior to the deposition of the
triple-layer AR coatings. SiO2–TiO2 sol, TiO2 sol and SiO2 sol were
deposited on both sides of the well-cleaned substrates sequen-
tially at a relative humidity less than 20% by dip coating at
withdrawal rate 175 mm/min, 500 mm/min and 160 mm/min,
respectively. The triple-layer coatings were heated at 200 1C for
8 h. The surfaces treatment of the coatings were carried out by
immersing the coated samples into HMDS/C2H5OH solutions with
different concentrations for 48 h and then dried at 160 1C.
2.3. Characterization
Theoretical transmittance spectrum of triple-layer AR coating
TM
was simulated with TFCalc program (Software Spectra Inc), and
the experimental transmittance spectrum was measured with an
UV–vis spectrophotometer (Mapada, UV-3100PC). Surface morphol-
ogies and cross-sections of the AR coating were investigated
separately by atomic force microscopy (AFM) (SEIKO SPA-400) and
JSM-5900LV scanning electrons microscope (SEM). The refractive
indices of the coatings were determined by ellipsometry (SENTECH
SE850 UV). The mechanical durability of the resultant coatings was
assessed in the abrasion test, in which the standard normal stress
25 kPa was applied with rotational shear (100 rpm for 0.5 h) on an
abrasion-resistance machine (DZ-8103, Dongguan City Dazhong
Instrument CO, LTD.). The mechanical damages were determined
by the change of the average transmittance over the visible
spectrum before and after the abrasion test. Water contact angles
were measured with a Krüss DSA100 (Germany) instrument at room
temperature.
3. Results and discussion
3.1. Computer-aid design of triple-layer broadband AR coatings
Optical properties of antireflective coatings can be monitored
by many methods, such as vector method, admittance loci, and so
on. The computer-aid design is preferred because it is fast and
straightforward. In this work, the triple-layer AR coating was
TM
optimized using the TFCalc program. As the commonly used
sol–gel films are silica, titania and silica/titania hybrid films with
refractive index varying from 1.44 to 2.20, we have tried to
optimize the triple-layer AR coating with refractive index of
individual layer ranging from 1.44 to 2.20. The following princi-
TM
ples were followed during TFCalc program calculation: (1) The
optical thickness for up, middle and bottom layers are set to l/4,
l/2 and l/4; (2) Because of its low refractive index and excellent
abrasion-resistance, acid-catalyzed silica is chosen as the up
layer; (3) As the refractive index of up layer is given, the
optimization steps are to determine the optimum refractive
indices of the middle and bottom layer by computer program.
As examples, several triple-layer coatings design and the
corresponding theoretical transmittances are shown in Table 1.
C2 design gives an optimum result.
3.2. Experimental preparation of the triple-layer broadband AR
coatings
Table 2 shows the refractive indices and film thickness of the
computer designed optimum triple-layer broadband AR coatings,
and the corresponding theoretical transmittance spectrum is
162 L. Ye et al. / Solar Energy Materials & Solar Cells 111 (2013) 160–164

Table 1
The parameters of the l/4  l/2  l/4 triple-layer AR coatings on glass (l0 ¼ 550 nm).

Bottom layer Middle layer Up layer The average transmittance

(400–800 nm)/%
Refractive index Film thickness Refractive index (n2) Film thickness Refractive index Film thickness
(n1) (d1)/nm (d2)/nm (n3) (d3)/nm

C1 1.61 85 2.20 125 1.44 95 98.6

C2 1.71 80 2.20 125 1.44 95 99.1
C3 1.81 76 2.20 125 1.44 95 98.4
C4 1.71 80 2.10 131 1.44 95 99.0
C4 1.61 85 2.10 131 1.44 95 98.9
C5 1.81 76 2.30 120 1.44 95 98.7

Table 2
The parameters of the theoretical and experimental triple-layer AR coatings
on glass.

Theoretical parameter Experimental parameter Dip-coating

(C2) speed (mm/min)

Refractive Film Refractive Film

index thickness/ index thickness/
nm nm

Cover 1.52 – 1.52 – –

glass
Bottom 1.71 80 1.71 84 175
layer
Middle 2.20 125 2.20 128 500
layer
Up 1.44 95 1.44 86 160
layer

Fig. 3. The refractive indices of SiO2–TiO2 hybrid film as a function of weight ratio
of silica.

varying from 1.44 to 2.20 have been obtained by mixing the

Fig. 2. Theoretical and experimental transmission spectra of the triple-layer AR
coating.
given in Fig. 2. The theoretical average transmittance in the
visible region can reach up to 99.1%.
Accurate control of the refractive index (n) and film thickness
(d) of the individual layers is the key factor to achieve the right
multi-layer AR coating. As shown in Table 2, the refractive indices
required for up, middle and bottom layers are 1.44, 2.20 and 1.71,
respectively. The silica layer with n ¼1.44 and titania layer with
n ¼2.20 were used as the up and middle layers, then it remains to
find a film material with a refractive index of 1.71 to use as the
bottom layer. sol–gel process provides a convenient route for
preparation of hybrid materials with accurate stoichimetric ratio.
In this work, silica/titania hybrid films with refractive index
starting silica and titania sols together in different proportions.
Fig. 3 shows the effect of weight ratio of silica on the refractive
index of silica/tatania hybrid film. The refractive index of the
hybrid film is proportional to the weight ratio of silica in the
hybrid sols. The bottom layer with refractive index of 1.71 can be
obtained when the silica weight ratio is about 50%.
The film thickness is another important factor influencing the
optical properties of the AR coating, which can be easily con-
trolled by varying the sol concentration and/or the dip-coating
speed in the sol–gel process. For a sol with given concentration, it
is convenient to control the film thickness by changing dip-
coating speed. As a result of a series of experiments, Table 2 gives
the optimized dip-coating speed for individual layers, which are
175 mm/min, 500 mm/min and 160 mm/min for bottom, middle
and up layers, corresponding to the film thickness of 84 nm,
128 nm and 86 nm, respectively, which showed that the film
thickness can be controlled with reasonable accuracy.
3.3. Optical property of the triple-layer AR coating
The silica/titania hybrid, titania and silica films were then
deposited successively on the glass substrate by dip-coating
method to form the triple-layer broadband AR coatings. Fig. 2
shows the experimental and theoretical transmittance spectra of
triple-layer broadband AR coating as well as the experimental
transmittance of glass substrate. The average transmittance of the
experimental triple-layer AR coating in the region of 400–800 nm
is 98.4%. Compared to the transmittance of the glass substrate of
92.0%, an enhancement of 6.4% in transmittance is achieved with
 L. Ye et al. / Solar Energy Materials & Solar Cells 111 (2013) 160–164
the triple-layer AR coating. Fig. 2 also indicates that the experi-
mental transmittance spectrum is in good agreement with our
TM
previous theoretical design by the TFCalc program. The trans-
mission difference in the short-wavelength regions is probably
due to the dispersion of the refractive index in the wavelength
region [12,25]. In the theoretical design it has been assumed that
the refractive index of films and substrate did not change with
wavelength and the refractive index at 550 nm was adopted as
the refractive index for the entire visible region. Actually, the
refractive index of titania and silica increases with the decrease of
the wavelength, which leads to the differences between the
experimental and designed transmittance spectra.
3.4. Morphology of the coatings
The microscopic structure of the triple-layer coatings, obtained by
SEM, is shown in Fig. 4. From the cross-sectional image of the triple-
layer coatings, we can find that the borders between any two of the
three layers are apparent, indicating no interpenetration among the
interfaces of the layers. Fig. 5 shows the surface morphologies of
single-layer acid catalyzed SiO2 coating and the triple-layer coatings,
the root-mean-square (RMS) roughness (Rq) for the single-layer silica
coating is 0.81 nm and reaches to 1.87 nm for triple-layer broadband
AR coating, which is probably due to the accumulation of the
roughness for the three layers. Even with a considerable increase in
roughness, this roughness value for the triple layers coating is still
small to cause any intense surface light scattering [26].
Fig. 4. The cross-sectional SEM photograph of the triple-layer coating.
Fig. 5. AFM patterns of the single-layer acid catalyzed SiO2 coating (a) and the triple-layer coating (b).
163
3.5. Mechanical performance
For outdoors use, the abrasion-resistance is very important for AR
coatings because they have to endure abrasion process due to
atmospheric conditions and cleaning processes. The decrease of the
average transmittance in the visible region was adopted to evaluate
the abrasion-resistance of the AR coatings after being rubbed with
abrasion-resistance test equipment. As shown in Fig. 6, the AR
performance of the coating remains almost intact, with only a 0.2%
reduction in the region of 400–800 nm, indicating an excellent
abrasion-resistant property of this triple-layer AR coating. The excel-
lent abrasion-resistance achieved is an anticipated result of the
upfront film design. The film materials used in this work are the
sol–gel silica and titania which are robust and condense. In particu-
larly, the growth of silica sol with an acid catalyst results in a
structure of linear chains which leads to a high abrasion-resistance
with high adhesive force on substrates [24,27]. Furthermore, the
adhesion of the coatings was examined by a tape test [20]. The tape
(Brand Panda) was laid across the coated surface, and then was
slowly pulled away. The AR properties showed no change after
peeling of the tape, which indicates good adhesion among individual
layers and the glass substrate.
3.6. Hydrophobic treatment of triple-layer AR coatings with HMDS
The hydrophobicity of AR coatings used in solar cells is also
important in preventing contaminants. A very hydrophobic surface
can afford the AR coating some self-cleaning property, because the
water can easily roll and take away the contaminants from the
hydrophobic surface [28]. Hydrophobicity is generally characterized
by water contact angle measurement, and an increase in the value
of water contact angle indicates a more hydrophobic surface.
The acid-catalyzed silica film is hydrophilic due to the many
hydroxyl groups on silica film surface. The hydrophobicity of the
surface can be significantly improved by replacing the polar
hydroxyl groups with nonpolar groups by surface modification.
Fig. 7 shows the variation in water contact angle of the AR
coatings as a function of HMDS concentration in C2H5OH solution.
It is clearly that the HMDS treatment improves dramatically the
water contact angle of the AR coatings. The increase in hydro-
phobicity is caused by the introduction of –OSi(CH3)3 groups into
the surfaces of the AR coatings [29].
4. Conclusions
Triple-layer broadband antireflective (AR) coating with average
transmittance of 99.1% was designed by computer-aid calculation.
164 L. Ye et al. / Solar Energy Materials & Solar Cells 111 (2013) 160–164
Fig. 6. Change in transmittance of AR coatings before and after abrasion.
Fig. 7. Water contact angle versus concentration of HMDS.
Silica/titania hybrid film with refractive index varying from 1.44 to
2.20 was prepared by the sol–gel process and applied as film
materials for the triple-layer broadband AR coating. SiO2/TiO2/SiO2–
TiO2 triple-layer AR coating with an average transmittance of 98.4%
in the visible region was successfully achieved using sol–gel dip
coating method. The hydrophobicity of AR coating can be signifi-
cantly improved by surface modification with HMDS. This triple-
layer abrasion-resistant broadband AR coating with excellent
transmittance in the visible region and improved self-cleaning
property has potential value in the field of solar cells.
Acknowledgment
The authors gratefully acknowledge the support from China
National Petroleum and Gas Corporation science and technology
development project ‘‘Nano intelligent chemical agent’’ (2011A-
1001).
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