Surface Innovations http://dx.doi.org/10.1680/si.12.

00014
Research Article
Received 02/12/2012 Accepted 07/02/2013
Silica-based superhydrophobic coating by Published online 12/02/2013
a single-step process Keywords: adhesion/coating/contact angle/
superhydrophobicity
Kousaalya, Garg and Kumar

ice | science ICE Publishing: All rights reserve

Silica-based superhydrophobic
coating by a single-step process
1 Adhimoolam Bakthavachalam Kousaalya BTech 3 Ravi Kumar PhD*
Department of Metallurgical and Materials Engineering, Materials Associate professor, Department of Metallurgical and Materials
Processing Section, Indian Institute of Technology Madras Engineering, Materials Processing Section, Indian Institute of
(IIT-Madras), Chennai, India Technology Madras (IIT-Madras), Chennai, India

2 Nitish Garg MTech

Department of Metallurgical and Materials Engineering, Materials
Processing Section, Indian Institute of Technology Madras
(IIT-Madras), Chennai, India

1    2    3

Silica-based superhydrophobic coatings were produced on glass substrate by dip-coating process. Colloidal solu-
tions containing nanoparticles of silica synthesized via seed growth method (single- and dual-sized particles) and
dispersed in three different solvents, ethanol, silica sol and acidic silica sol, were used. Coatings with dual-sized
particles in ethanol showed superhydrophobicity with a water contact angle of 155°. The coating adhesion was
improved with the use of acidic silica sol as solvent. Coatings prepared from colloidal solution containing 30 wt.%
of dual-sized silica particles of 600 and 800 nm in acidic silica sol, showed hydrophilicity with water contact angle
of 45° before heat treatment due to the presence of –OH groups from acidic sol. After heat treatment at 250°C
for 2 h in atmospheric ambience, the –OH groups reacted to form cross-linked Si-O-Si resulting in superhydropho-
bicity of the coating with water contact angle of 147°. In this work, silica based superhydrophobic coating was
fabricated by adjusting the ratios of the dual-sized silica particles without carrying out any secondary step such as
chemical modification or fluorination process on the coating.

1. Introduction
Nature exhibits excellent superhydrophobic surfaces with a high
contact angle (CA) of greater than 150° in certain plant leaves such
as lotus leaves,1 rice leaves and butterfly wings,2 cicada wings,3
which are self-cleaning. This has attracted immense research inter-
est to biomimic and fabricate artificial superhydrophobic surfaces,
which are used for numerous applications such as window glasses,
solar cell panels, energy conversion and conservation and naviga-
tion of ships to prevent marine fouling.4
In the process of preparing superhydrophobic surfaces, a good
control over chemistry coupled with geometry similar to hierar-
chical geometrical surface structures found in nature are used.5,6
For instance, (i) producing geometrically controlled rough surfaces
of any material and reducing its surface energy by the addition of
low surface energy materials or (ii) tailoring the low surface energy
material, by creating roughness at micro/nano scales would achieve
the objective.
Extensive research has focused on producing superhydrophobic
coating by using the former (i) method. Table 1 provides details of
coated material systems, and the method used for coating along with
the achieved CA. In all the cases, superhydrophobicity was achieved
only due to chemical modification of the coatings using low surface
energy materials such as fluorine and silicone polymer. However, in
the case of producing superhydrophobic coating via the later (ii) fluo-
rine- and silicone-based polymers play an important role.5 The use of
fluorine- and silicone-based materials for superhydrophobic coating

*Corresponding author e-mail address: nvrk@iitm.ac.in

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Surface Innovations Silica-based superhydrophobic coating by a
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Kousaalya, Garg and Kumar

Maximum
S. No. Material used for coating Method contact angle Reference
achieved

1 Silica prepared from Stöber process coated and modified with Colloid assembly 160° 7
FAS method
2 Two different sizes of modified silica, coated and modified Drop coating 155° 8
with polydimethylsiloxane layer
3 Polyelectrolyte/silica nanoparticle multilayers, followed by Electrostatic layer- 157° 9
fluoroalkylsilane treatment by-layer assembly
4 Silica-polystyrene sol-gel coated and modified with FAS Dip coating 160° 10
5 Silane (METES and METES/DECYS) precursor with silica Spin coating 158·3° 11
particles
6 Colloidal silica particles and fluoroalkylsilane in TEOS Spin coating 150° 12
7 TEOS/MTMS in different ratios Dip coating 135° 13
8 Silica nanoparticles coated and modified with tridecafluoro- Dip coating 165° 14
1,1,2,2-tetrahydrooctyldimethylchlorosilane
9 Silica obtained from tetramethylsilane or tetramethoxysilane, Plasma-enhanced 160° 15
coated and modified with (heptadecafluoro-1,1,2,2- chemical vapor
tetrahydro-decyl)-1-trimethoxysilane deposition
Silica deposited and modified with trichloro(1H,1H,2H,2H- Layer-by-layer
10 160° 16
perfluorooctyl) silane processing
FAS, perfluoroalkysilane; TEOS, tetraethoxysilane; MTMS, methyltrimethoxysilane.

Table 1. Silica-based coatings with various types of surface modification to achieve superhydrophobicity.

is primarily due to the low surface-free energy exhibited by them. In 2. Experimental methods
general, the surface energy of polymers is typically lesser than water
(72·2 mJ/m2) due to the presence of organic groups, while the lowest
2.1 Synthesis of silica particles
Silica particles were synthesized by the hydrolysis of tetraethyl
is for fluorine-based polymers (12·4 mJ/m2 for polyhexafluoropro-
ester of orthosilicic acid (TEOS): Si(OC2H5)4 (Alfa Aesar, USA) in
pylene, 19·1 mJ/m2 for polytetrafluoroethylene) and silicone-based
ethanol, using ammonia as catalyst, by the following reaction, bet-
polymers (22 mJ/m2 for polydimethylsiloxane). Fluorination of sili-
ter known as seed growth method or “Stöber process.”19
cone polymer will further reduce the surface energy of the ­material.17
While nature exhibits superhydrophobicity due to the presence of
1. Si(OC 2 H 5 ) 4 + 4H 2O → Si(O) 2 ↓ + 4C 2 H 5OH
waxes containing predominantly –CH2– groups (whose surface
energy is lower than water), concomitant with surface roughness at
Silica seed sol was first synthesized by adding 1-g TEOS, 3-g water
nanoscale, it is reasonable to fabricate low surface energy material
and 3-g ammonia in 4-g ethanol, followed by continuous stirring at
with hierarchical nanostructure to achieve superhydrophobicity.1,5,18
room temperature (25 °C) for 1·5 h. Subsequently, a solution of 2-g
TEOS in 8-g ethanol was added to the reaction mixture and stirred for
Hence, to obtain superhydrophobic surfaces, materials with surface
3 h as explained by Xu et al.7 The precipitated silica particles (hence-
energy lesser than water are generally used, which contain toxic
forth referred to P-SiO2) were centrifuged using Eppendorf centrifuge
chemicals such as fluorine and involve multiple steps in producing
5810R, Germany, at three different speeds (1000, 2000 and 5000 rpm)
the coatings. Development of superhydrophobic surfaces with eco-
for 5 min at 5°C, to separate P-SiO2 of different sizes.
friendly chemicals is required6 and with a single-step process, that
can be made more economical. The current work focuses on develop-
ing such a silica-based superhydrophobic coating using simple dip- 2.2 Preparation of colloidal solutions
coating process with good adhesion, in a single-step process without The colloidal solutions were prepared using two differently sized
any additional processes like fluorination or any type of chemical P-SiO2 mixed in different proportions as solutes: P-SiO2 sepa-
modification, to reduce the surface energy of the coating. The ability rated after centrifugation at 2000 rpm designated as P-SiO2(A),
to alter the particle size distribution helps in introducing nanoscale and P-SiO2 separated after centrifugation at 1000 rpm designated
roughness on the coating resulting in superhydrophobicity. as P-SiO2(B). The following three solvents, ethanol, a silica sol

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Surface Innovations Silica-based superhydrophobic coating by a
single-step process
Kousaalya, Garg and Kumar

– 20-nm silica in 50% H2O colloidal solution (Alfa Aesar, USA), 2.4 Characterization
and an acidic silica sol were used. The acidic silica sol was pre- The morphology and size of P-SiO2 were characterized using
pared by adding 2·4-g hydrochloric acid (36·5%) and 2-g TEOS in transmission electron microscope (TEM), Philips CM20, The
8-g ethanol followed by continuous stirring for 2 h at 60°C. Netherlands at an accelerating voltage of 200 kV. A small amount
of the precipitated silica particles, obtained before and after centrif-
The colloidal solutions that were prepared are described in Table ugation, were dispersed separately in ethanol and ultrasonicated for
2, in which the column on solute content gives the amount (wt.%) 30 min. A drop of both the solutions was deposited separately and
of P-SiO2(A) and P-SiO2(B) present in the solution. For example, dried over a carbon-coated copper grid and viewed through TEM.
the first solution given in Table 2 has 5 wt.% of P-SiO2(A), no The surface roughness of the etched glass before coating was char-
P-SiO2(B) and the solvent used is ethanol, while the fifth solution acterized using surface profilometer, Mitutoyo SJ-400, Japan. The
in the table has 5 wt.% of P-SiO2(A) and 10 wt.% of P-SiO2(B) as surface morphology of the coatings was studied using field emis-
solute and ethanol as the solvent. The solute, solvent mixtures men- sion gun scanning electron microscope (FEG-SEM), FEI Quanta
tioned in Table 2 were ultrasonicated for 30 min to obtain colloidal 400F, USA. The coatings were sputter coated with a gold layer of
solutions for producing coatings on glass substrates. thickness 5 nm before imaging them using SEM in secondary elec-
tron mode. Optical imaging was carried out in bright field mode
and differential interference contrast (Nomarski DIC) mode using
2.3 Coating procedure
Olympus IX71 inverted microscope, USA. The static CA measure-
The glass substrates were etched with H2SO4/H2O2 (50/50%) solu-
ments of the coated sample, before and after heat treatment, were
tion for 6 h, ultrasonicated for 30 min, rinsed with acetone and
carried out using CA goniometer, Digidrop GBX, France with 2·0–
distilled water. The glass substrates were then coated with the pre-
4·0 µl ­distilled water droplets at room temperature.
pared colloidal solutions through a dip-coating process using single
dip coater (SDC 2007C, Apex instruments Co., India) using the
following parameters: dipping and withdrawal rate of 50 mm/min 3. Results and discussion
each, holding time of 15 min and drying time of 5 min, and the
cycle was repeated for 10 times. The coated glass substrates were 3.1 Morphology of silica particles
heat treated at 250°C for 2 h in atmospheric ambience to ensure The TEM micrograph of P-SiO2 before centrifugation and P-SiO2
solidification and complete evaporation of the solvent. separated after centrifugation at 1000 rpm is shown in Figure 1(a,b)
and 1(c,d), respectively. Before centrifugation, the presence of debris
on the P-SiO2 is observed. However, after centrifugation, P-SiO2 was
Amount of solute present found to be completely spherical of uniform diameter, free of debris
(wt.%) Solvent and agglomerates. The silica particles with diameter of ~800 nm were
S. No.
used separated out after centrifugation at 1000 rpm for 5 min, while parti-
P-SiO2(A) P-SiO2(B) cles with diameter of ~600 nm were separated out after centrifugation
at 2000 rpm for 5 min. The selected area diffraction pattern shown as
1 5 0
insert in Figure 1d exemplifies that the silica particles are amorphous.
2 0 5 Since the particles separating out after centrifugation at 1000 rpm are
3 15 0 completely spherical, free of agglomeration and debris, only a rep-
Ethanol
4 0 15 resentative TEM image of P-SiO2 is provided here in Figure 1(c,d).
5 5 10 After centrifugation at 5000 rpm, the solution was clear with rather
6 10 5 minimal presence of silica particles for any further consideration.
7 0 5
8 5 0
Silica sol 3.2 Coating and adhesion
9 0 15
The prepared colloidal solutions were coated on glass substrates
10 15 0
with surface roughness (Ra) of ~0·05 µm. The coatings were
11 10 5
found to be transparent, with presence of few silica particles on
12 10 10
Acidic sol the glass substrate when coated with colloidal solution containing
13 15 10
5 wt.% (P-SiO2(A) or P-SiO2(B)) in ethanol/silica sol as solvents.
14 15 15 Hence, the silica content was increased to 15 wt.% (P-SiO2(A) or
Table 2. Composition of colloidal solutions for coating: P-SiO2 P-SiO2(B)) to ensure additional silica particles were available in the
­separated after centrifugation at 2000 rpm is designated as colloidal solution for coating.
P-SiO2(A), and P-SiO2 separated after centrifugation at 1000 rpm is
designated as P-SiO2(B). The coatings made using ethanol as solvent exhibited poor adhesion
with the glass substrate, in both cases, before and after heat treatment,

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Surface Innovations Silica-based superhydrophobic coating by a
single-step process
Kousaalya, Garg and Kumar

(a) (c)

5 µm 100 nm

(b) (d)

Presence of debris
on the silica particle
1 µm 1 µm

Figure 1. TEM images of silica particles synthesized via Stöber

­process. (a,b) Before centrifugation and (c,d) after centrifugation at
1000 rpm P-SiO2(B) (size ~800 nm); diffraction pattern (shown as
insert) exemplifying the amorphous nature of silica particles. TEM,
­transmission electron microscopy.

(a) (b) +10 sec (c) +30 sec

500 µm 500 µm
500 µm

(d) (e)

100 µm 100 µm

Figure 2. Crack patterns observed in the coating obtained from 15

wt.% P-SiO2(A) silica particles in silica sol (a) bright field optical micro-
graph: 50×; (b) image taken after 10 s; (c) image taken after 30 s; (d)
bright field image: 20× and (e) differential interface contrast image.

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Surface Innovations Silica-based superhydrophobic coating by a
single-step process
Kousaalya, Garg and Kumar

which was clearly evident from the fact that the coating was easy to
remove from the glass substrate while handling. In the case of silica
sol as solvent, the obtained coatings were not stable even during the
coating process. The coatings were found to crack during the drying
time between the coating cycles. Hence, the development of crack
patterns in the coating during drying was viewed through optical
microscope in bright field mode and differential interface contrast
mode. Figure 2 shows the development of cracks with time on glass
substrate coated with colloidal solution of 15 wt.% P-SiO2(A) in
silica sol in bright field mode. Figure 2a shows the optical image
obtained immediately after removal of the glass substrate from the
colloidal solution after dipping the substrate for 15 min. Figure 2b
and figure 2c were obtained after 10 and 30 s, respectively. From
Figure 2a–2c, formation of cracks on the coating with increase in
time is clearly evident. Figure 2d obtained after 90 s shows that the
coating had completely cracked. Figure 2e shows the corresponding
differential interference contrast image. The formation of cracks at a
4/20/2012 HV mag WD det vac mode 3 µm faster rate in the coating with silica sol as solvent could be due to the
5:35:04 PM 30·00 kV 14 000 x 10·5 mm ETD High vacuum Quanta FEG evaporation of water present in the silica sol resulting in spallation
Figure 3. FEG-SEM images of the coating with (10 wt.% of P-SiO2(A) during 5 min of drying time between the cycles.
and 5 wt.% of P-SiO2(B)) in acidic silica sol binder, also showing the
cross-linked adhesive layer. FEG-SEM, field emission gun scanning Hence, subsequently coatings were carried out with acidic silica sol as
electron microscope. solvent using colloidal solutions containing varying amount of solutes
as mentioned in Table 2. Sakka et al.20 has shown that the use of acidic

Amount of solute present (wt.%)

Contact
S. No. Solvent used
angle
P-SiO2(A) P-SiO2(B)

1 5 0
—
2 0 5
3 15 0 ~36°
Ethanol (after heat treatment)
4 0 15 ~36°
5 5 10 ~155°
6 10 5 ~155°
7 0 5
—
8 5 0
Silica sol (before heat treatment)
9 0 15 ~110°
10 15 0 ~110°
11 Before heat treatment 10 5 ~47°
12 10 5 ~102°
13 Acidic sol 10 10 —
After heat treatment
14 15 10 ~114°
15 15 15 ~147°

Table 3. Wettability of various compositions of colloidal solutions for coating: P-SiO2 separated after centrifugation at 2000 rpm designated as
P-SiO2(A) and P-SiO2 separated after centrifugation at 1000 rpm designated as P-SiO2(B).

5
Surface Innovations Silica-based superhydrophobic coating by a
single-step process
Kousaalya, Garg and Kumar

(a) (b)

CA - 36° CA - 110°

Figure 4. Contact angle on coatings: (a) 15 wt.% of P-SiO2(A) in

ethanol and (b) 15 wt.% of P-SiO2(A) in silica colloidal sol.

catalyst will result in the formation of a linear silica-based polymer as

opposed to formation of silica particles with the use of base catalyst.
Hence, the use of hydrochloric acid as catalyst with absence of suf-
ficient amount of water was used in the preparation of acidic silica sol.
This acidic silica sol contains abundant active hydroxyl groups (-OH)
in silica-based linear oligomer/polymer formed from TEOS.7 During
the coating process, P-SiO2 and linear silica-based polymer present in
acidic sol get assembled onto the surface, which on subsequent dry-
ing at 250°C for 2 h, results in gradual volatilization of hydrochloric
acid and ethanol present in the solvent. The surface morphology of
the coated surface characterized by FEG-SEM reveals the presence of
cross-linked adhesive type layer (Figure 3) in the coating. Xu et al.7
has shown that active hydroxyl (-OH) groups present in the linear
silica-based polymer react with silica present in the solute and the
hydroxyl groups present on the surface of glass substrate during heat CA - 155°
treatment resulting in cross-linked Si-O-Si bonds, thereby ensuring
better adhesion of the coated particles. The obtained coating exhibited Figure 5. Contact angle on coatings with dual-sized particle
substantial improvement in adhesion to the glass substrates. distribution (10 wt.% of P-SiO2(A) and 5 wt.% of P-SiO2(B)) in
ethanol.
3.3 Surface wettability
Table 3 lists the CAs achieved on all the coatings provided on the P-SiO2 in ethanol. Figure 5 shows the CA measurement carried out
glass substrates as explained in Table 2. Figure 4 shows the CA on the fabricated coatings with 10 wt.% of P-SiO2(A) and 5 wt.%
measurement carried out on the coating with 15 wt.% of P-SiO2(A) of P-SiO2(B) in ethanol. In case of coating uni-particle size, uni-
in ethanol and silica sol as solvents. Silica coatings with 15 wt.% formity of the silica particle spheres as seen from the SEM images
of (P-SiO2(A) or P-SiO2(B)) in ethanol exhibits a CA of ~36°. The (Figure 6a), makes the surface smooth enough and thus making it
coatings made using 15 wt.% of (P-SiO2(A) or P-SiO2(B)) in silica hydrophilic. On the contrary, coating with dual-sized distribution of
sol as solvent are hydrophobic with maximum CA of ~110°, inspite P-SiO2, the microstructure provides nanoscale roughness as is seen
of its poor adhesion as shown in Figure 2 and explained in Section from the SEM image (Figure 6b). Due to this roughness, nano-air
3.2. In case of coatings with silica sol as solvent, it is important pockets that are created on the surface of the coating could decrease
to note that silica particles of two different sizes, 600-nm silica the wettability of the surfaces and therefore could be responsible
particles from solute and 20-nm silica particles from solvent are for the superhydrophobic nature of the coating.4
present. The enhanced CA achieved on the coating is attributed to
the nanoscale roughness created by the presence of two differently The CA measurements were carried out before and after heat treat-
sized particles, which is in agreement with earlier literature.18 ment on the samples coated with acidic sol as solvent as shown
in Table 3. It was found that the coating has a hydrophilic nature
Hence, coatings on glass substrates were made using dual-sized with CA of ~45° (image not shown) before heat treatment and was
particle distribution (10 wt.% of P-SiO2(A)/P-SiO2(B) and 5 wt.% found to increase significantly after heat treatment. Saman et al.21
of P-SiO2(B)/P-SiO2(A)) in ethanol. These coatings exhibit a CA has shown that acidic silica sol has a monolithic morphology.
as high as 155° in contrast to uni-sized particle distribution of However, this monolithic morphology results in smoothening of the

6
Surface Innovations Silica-based superhydrophobic coating by a
single-step process
Kousaalya, Garg and Kumar

(a) (b)

4/20/2012 HV mag WD det vac mode 2 µm 4/20/2012 HV mag WD det vac mode 2 µm
5:11:03 PM 30·00 kV 20 000 x 10·5 mm ETD High vacuum Quanta FEG 5:59:50 PM 30·00 kV 20 000 x 10·5 mm ETD High vacuum Quanta FEG

Figure 6. SEM images of the coated samples (a) coating with single
particle size 15 wt.% of P-SiO2(A) in ethanol and (b) coating with
dual-sized particle distribution 10 wt.% of P-SiO2(A) and 5 wt.% of
P-SiO2(B) in ethanol. SEM, scanning electron microscope.

(a)
(b) (c)

CA - 102° CA - 114° CA - 147°

Figure 7. Contact angle on coatings with dual-sized particle distribu-

tion in acidic sol after heat treatment: (a) 15 wt.% (10 wt.% of
P-SiO2(A) and 5 wt.% of P-SiO2(B)), (b) 25 wt.% (15 wt.% P-SiO2(A)
and 10 wt.% of P-SiO2(B)) and (c) 30 wt.% (15 wt.% P-SiO2(A) and
15 wt.% of P-SiO2(B)).

surface of coating. This smoothening effect and presence of –OH 4. Conclusions

groups are responsible for hydrophilicity of the coating prior to
heat treatment. The CA experiments on coatings using acidic silica
sol as solvent with 10 wt.% of P-SiO2(A) and 5 wt.% of P-SiO2(B)
as solute was found to have CA of 102°, while use of ethanol as
solvent showed CA of 155°. This reduction in CA observed in the
former is attributed to the smoothening effect of the acidic sol as
a result of its monolithic nature. However, when the total P-SiO2
content in the colloidal solution was increased to 25 wt.%, and 30
wt.% increase in the CA was observed, with 30 wt.% of P-SiO2 (15
wt.% of P-SiO2(A) and 15 wt.% of P-SiO2(B)) in acidic sol show-
ing CA of ~147°. As a result of the increase in solute content, the
smoothening effect of acidic sol was reduced resulting in higher
CA, approaching superhydrophobicity.
Superhydrophobic coatings with CAs of ~150° with good adhesion
on the glass substrates were produced by a simple and inexpensive
layer-by-layer colloidal assembly method without any requirement
of secondary process such as fluorination. Nanosized, highly uniform
spherical silica particles were produced using seed growth “Stöber
Method.” The particles were separated to various sizes by centrifu-
gation and used in appropriate ratio to obtain superhydrophobicity.
The acidic silica binder helped increasing the adhesive strength by
­forming cross-links with the glass substrate and silica particles.
Acknowledgements
The authors would like to acknowledge Department of
Biotechnology, IIT-M for performing centrifugation experiments

7
Surface Innovations
and also Medical Materials Laboratory, Department of Metallurgical
and Materials Engineering, IIT-M and Polymer Engineering
Laboratory, Department of Chemical Engineering, IIT-M for car-
rying out contact angle measurement.
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