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A simple method for the fabrication of silica-based

superhydrophobic surfaces
Qianqian Shang, Yonghong Zhou, Guomin Xiao
American Coatings Association 2014
Abstract The present article reports on a simple and
convenient method for the fabrication of superhydro-
phobic surfaces based on silica particles by spraying the
as-prepared silica suspension containing silica sol and
silica microspheres on the substrate. The morphologies
of the silica particulate coatings could be controlled by
varying the silica microsphere concentration. The silica
particulate coatings as prepared were exceptionally
rough and superhydrophilic, with water contact angles
less than 5. The surface silanol groups of the hydro-
philic coatings could be functionalized using
1H,1H,2H,2H-peruorodecyltriethoxysilane to form
hydrophobic groups. The resulting surface showed
excellent superhydrophobic property with water con-
tact angle up to 165.6 0.9 and sliding angle of
3.5 0.4. In addition, the superhydrophobicity of the
coating possessed a good stability after 3 months of
exposure in air for a wide range of pH values.
Keywords Superhydrophobic, Silica particles,
Spray coating, Water contact angle
Introduction
A surface with water contact angle larger than 150 and
sliding angle lower than 10 is generally classed as a
superhydrophobic surface.
1
The design and fabrication
of articial superhydrophobic surfaces have received
considerable attentions in recent years because of their
promising applications in different areas, such as self-
cleaning materials,
24
corrosion resistance of metals,
5,6
and microuidic systems.
7
The lotus leaf, as well as other
self-cleaning superhydrophobic leaves, reveals that a
combination of low surface energy materials and a
specic surface topography based on micro/nanoscale
rough structure is necessary for the accomplishment of
superhydrophobic surfaces.
813
Micro/nanoscale hierar-
chical structure has been proven to be the prerequisite
surface property in obtaining superhydrophobic-
ity.
1,1012
Up to now, a great number of elegant technologies
have been reported to fabricate articial superhydro-
phobic surfaces, including electrospinning,
13,14
electro-
deposition,
15,16
electrospray,
17
lithography,
18
layer-
by-layer assembly,
19,20
spray coating,
2125
solgel
process,
2628
and so on. Among these technologies,
spray coating is a good choice to acquire superhydro-
phobic surfaces because of its great simplicity, scalabil-
ity, speed, and compatibility with a variety of substrates.
Moreover, this simple process has been widely used for
the preparation of painting or industrial coating in large
surface areas. Thus, the further development of super-
hydrophobic surfaces fabricated by spray coating as well
as a simple means of adjusting the water repellence of
such surfaces is highly desirable.
On the other hand, silica has been chosen as a
coating material for the fabrication of superhydropho-
bic surfaces by many researchers due to its promising
characteristics such as high thermal and mechanical
stability, low toxicity, low cost, and easy structural
regulation. In these reports, silica solgel or monodisperse
Q. Shang, Y. Zhou (&)
Institute of Chemical Industry of Forestry Products, CAF;
National Engineering Lab. for Biomass Chemical
Utilization; Key and Lab. on Forest Chemical Engineering,
SFA, Key Lab. of Biomass Energy and Material, Nanjing
210042 Jiangsu Province, Peoples Republic of China
e-mail: yhzhou777@sina.com
Q. Shang
e-mail: shang_qianqian@126.com
G. Xiao
School of Chemistry and Chemical Engineering, Southeast
University, Nanjing 211189 Jiangsu Province,
Peoples Republic of China
J. Coat. Technol. Res., 11 (4) 509515, 2014
DOI 10.1007/s11998-014-9573-z
509
silica particles were used to construct a hierarchical
structure together with layer-by-layer assembly
29
or
spin-coating.
30
These preparation processes for the
introduction of surface roughness were time-consum-
ing, which limited the practical applications of super-
hydrophobic surfaces in large areas.
In this study, we present a simple method for the
fabrication of superhydrophobic coating by spraying
silica suspension containing two kinds of particles from
silica sol and silica microspheres on the substrate.
Micro/nanoscale hierarchical structure with high sur-
face roughness and porosity could be obtained by a
one-step process, and the as-prepared coatings had
superhydrophilic properties with a contact angle below
5. After hydrophobic modication, the obtained
coating featured a superhydrophobic surface which
exhibited a static water contact angle up to
165.6 0.9 and a sliding angle of 3.5 0.4. The
superhydrophobic coating showed good stability after
being exposed in air for 3 months, and the contact
angle did not decrease obviously in the wide range of
pH values.
Experimental
Materials
1H,1H,2H,2H-Peruorodecyltriethoxysilane (PFDTS)
was supplied by Quanzhou Sicong New Materials
Development Co., Ltd. Tetraethyl orthosilicate
(TEOS), ammonia solution (25 wt%), absolute ethanol
(EtOH), and acetone were purchased from Shanghai
Lingfeng Chemical Reagent Co., Ltd. All chemicals
were used as received without further purication.
Deionized water was used in all the experiments.
Fabrication of the silica particulate coatings
Silica microspheres with a size of about 400 nm were
rst prepared by the hydrolysis and condensation of
TEOS in ethanol solvent in the presence of ammonia
solution as described by Sto ber et al.
31
The reaction
was carried out at the mole ratio of TEOS:EtOH:NH
3
:
H
2
O = 1:63:1.07:35. The obtained silica microspheres
were washed with absolute ethanol three times, and
then dried in an oven at 80C for 5 h.
Silica suspensions comprising silica microspheres
and silica sol were prepared by modifying a previous
reported method.
32
The preparation details were as
follows. A certain amount of as-prepared silica micro-
spheres and 2 ml of ammonia solution were dispersed
into 15 ml ethanol and the mixture was stirred for 1 h
at 45C in a water bath. Then 1.4 g of TEOS was added
into 12 ml of ethanol and the solution was stirred for
15 min. Afterward, the solution with TEOS was added
into the silica microspheres and ammonia mixture
solution and the resulting solution was allowed to be
stirred for another 1 h at 45C to form a silica
suspension.
The silica suspensions were spray coated onto glass
substrates through a manual airbrush (HP-C Plus,
Anest-Iwata Co., Japan) with a 0.3 mm diameter tip
using compressed air (0.2 MPa). Before spraying, the
silica suspension was stirred for 15 min to prevent
setting, and only freshly prepared batches of silica
suspension were utilized. Following spray coating,
samples were placed horizontally and dried at room
temperature overnight. The glass substrates (up to a
dimension of 75 9 25 mm
2
in size; thickness 1 mm)
were cleaned with a piranha solution (H
2
SO
4
/
H
2
O
2
= 70/30, v/v) for 3 h and ultrasonicated in
ethanol and acetone for 30 min, and then rinsed
thoroughly with deionized water before coating.
Hydrophobic modication of the coating surface
was carried out by a simple chemical vapor deposition
(CVD) of PFDTS solution. This solution was prepared
by mixing 0.5 g PFDTS and 1.0 g distilled water into
50 g methanol and stirring over 1 h. The coated glass
substrate was put into a sealed vessel containing 2.0 g
PFDTS solution. The distance between the glass
substrate and the PFDTS solution was 2.5 mm. The
vessel was heated at 150C for 3 h to form a self-
assembled PFDTS monomolecular layer on the surface
of the silica coating. After being removed from the
vessel, the coated substrate was placed in an oven of
120C for 1 h to volatilize unreacted PFDTS molecules
on the coating.
Characterizations
The morphological and elemental analyses of the silica
coatings on substrates were examined using a scanning
electron microscope (SEM, Hitachi S-4800N, Japan)
with an accelerating voltage of 20 kV and equipped
with an energy dispersive X-ray spectroscopy (EDX)
detector. Samples were sputter-coated with gold before
imaging. Water contact angle measurements were
carried out using an OCA20 contact angle meter at
room temperature by dropping 5 lL of water onto the
coating surface. Five different positions across the
substrates were measured over the coatings. The
photograph of the water droplet was obtained by a
digital camera (Canon, IXUS115 HS).
Results and discussion
Multi-scale surface feature, especially micro/nanoscale
hierarchical surface structure, is advantageous for the
obtaining of superhydrophobicity. In this study, a
mixed silica suspension consisting of two types of silica
particles were synthesized from TEOS via base-cata-
lyzed hydrolysis and condensation. The diameter of
silica microspheres was about 400 nm and the SEM
image is shown in Fig. 1a. Figure 1b shows the SEM
J. Coat. Technol. Res., 11 (4) 509515, 2014
510
image of the agglomerated silica sol. It can be seen that
the diameter of the silica nanoparticles was less than
100 nm.
The surface morphologies of the silica coatings with
silica microsphere concentrations of 0.015, 0.03, 0.05,
and 0.07 wt% were investigated by SEM, as shown in
Fig. 2. The surface morphologies and structures of the
silica coatings changed with the silica microsphere
concentrations. When the silica microsphere concen-
tration was lower than 0.03 wt%, two types of silica
particles mixed uniformly. Silica particles aggregated
and formed particle clusters with micro/nanoscale
surface features (Figs. 2a and 2b). At the high concen-
tration of silica microsphere, the silica microspheres
tended to assemble on the substrate during the solvent
evaporation process. The silica sol linked and stacked
together and lled in the cavities and grooves between
the assembled silica microspheres (Figs. 2c and 2d). All
the silica particulate coatings as-formed maintained an
essential hierarchical surface structure, which was
benecial to trap enough air among textures for the
obtaining of superhydrophobicity.
The water repellence of the coating surface was
characterized by the sessile drop method using a 5 lL
water droplet at room temperature. The optical images
of a water droplet on different surfaces are shown in
Fig. 3. After being modied with PFDTS solution, all
the silica particulate coatings showed excellent super-
hydrophobicity, all achieving water contact angles that
were higher than 150. However, there was still obvious
variation of water contact angles exhibited by the
coatings fabricated with different silica microsphere
concentrations. When the concentrations of silica
microspheres were 0.015 and 0.03 wt%, the water
contact angle was 163.5 1.1 and 165.6 0.9, respec-
tively. Increasing the concentration of silica micro-
spheres to 0.05 and 0.07 wt%, the superhydrophobicity
Fig. 1: SEM images of the silica microspheres (a) and silica
nanoparticles (b)
Fig. 2: SEM images of the silica particulate coatings with different silica microsphere concentrations: (a) 0.015 wt%,
(b) 0.03 wt%, (c) 0.05 wt%, and (d) 0.07 wt%
J. Coat. Technol. Res., 11 (4) 509515, 2014
511
of the coatings started to decrease and the water contact
angle decreased to 157.9 1.8 and 154.5 0.5. In
addition, the sliding angle values of the as-prepared four
kinds of silica coatings are measured and listed in
Table 1. All the surfaces of silica coatings showed low
sliding angles (<9). It should be noted that the
superhydrophobic silica coating prepared at the silica
microsphere concentration of 0.03 wt% had the highest
contact angle of 165.6 0.9 and lowest sliding angle of
3.5 0.4. Figure 4 shows the photograph of water
droplets with different sizes on the superhydrophobic
surface obtained using silica microsphere concentration
of 0.03 wt%. It can be seen that the water droplet
looked like a ball even when its volume was up to 25 lL.
The coatings were extremely slippery relative to water.
Water droplets were very hard placed on the superhy-
drophobic coatings and would roll off the surface at a
small inclination.
Apart from surface roughness, surface chemical
composition also has a pronounced effect on the
surface hydrophobicity. Before hydrophobic treat-
ment, the contact angles of water were always below
5 for the coatings with different silica microsphere
concentrations. As soon as a droplet of water contacted
the highly rough silica particulate coatings, it spread
at instantaneously on the surfaces, indicating a great
superhydrophilic nature of the unmodied silica coat-
ings. The superhydrophilicity of the silica coatings
conrms Wenzels wetting theory,
33
where a water
droplet penetrates into the porous coating surface,
resulting in a strong attraction to the surface. It is
known that uorine is the most effective for lowering
the surface free energy. Thus, we treated the silica
particulate coatings using a peruorosilane through a
simple CVD technique to improve the water repel-
lence (Fig. 5). The superhydrophilic coatings were
treated with PFDTS solution for 3 h at 150C in a
sealed vessel, with the aim to form peruorooctylsilane
groups in place of surface silanol bonds. After surface
modication with PFDTS, the wettability of the silica
particulate coatings changed considerably. The contact
angle of all coating surfaces was higher than 150.
Particularly, for the sample prepared with a silica
microsphere concentration of 0.03 wt%, the contact
Fig. 3: The photograph of water droplets (5 lL) on the silica particulate coatings with different silica microsphere
concentrations: (a) 0.015 wt%, (b) 0.03 wt%, (c) 0.05 wt%, and (d) 0.07 wt%
Table 1: The contact angles and sliding angles of the
superhydrophobic coatings prepared at different con-
centrations of silica microsphere
Silica microsphere
concentration (wt%)
Static contact
angle ()
Sliding
angle ()
0.015 163.5 1.1 5.6 0.5
0.03 165.6 0.9 3.5 0.4
0.05 157.9 1.8 7.3 0.1
0.07 154.5 0.5 8.6 0.3
J. Coat. Technol. Res., 11 (4) 509515, 2014
512
angle reached 165.6 0.9. The surface chemical
composition of the silica particulate coating was
evaluated using EDX spectrometer. Figure 6 displays
the EDX spectrum of the silica particulate coating with
silica microspheres of 0.03 wt%, in which F and C
elements were detected except Si and O peaks. The
result was in good agreement with the chemical
composition of the coating.
It has been recognized that the superhydrophobicity
of a solid surface is mainly controlled both by its
chemical composition and micro/nanoscale hierarchi-
cal structure with high surface roughness and porosity.
In this study, all the surfaces were modied by a layer
of PFDTS with the same treatment, and the chemical
compositions are the same according to the results of
EDX. Thus, the contact angle of the prepared coating
surface was mainly determined by the micro/nano-
structure of the surface. The water contact angle h* of
the micro/nano-structured surfaces can be calculated
by the modied CassieBaxter equation
34
:
cos h

rf
1
cos h f
2
; 1
where r is the surface rough factor, h represents the
contact angle of a smooth surface, and h* is that of a
rough surface; f
1
and f
2
denote the fraction interfacial
areas occupied by the water/solid and water/air inter-
faces (f
1
+ f
2
= 1). It can be seen that an increment of
the value of f
2
increases the contact angle h* of the
rough surface, which indicates that the achievement of
superhydrophobicity is ascribed to the contribution of
the air trapped in the cavities of micro/nanoscale
hierarchical structures.
When the superhydrophobic surfaces were inclined
to a small angle, the air trapped in the cavities micro/
nanoscale hierarchical structures could be released and
gave rise to an expelling force on the water droplet.
32
Thus, water droplets could easily roll on the superhy-
drophobic surfaces, which gave these surfaces an ideal
lotus effect self-cleaning mechanism.
The stability of a superhydrophobic surface is an
important factor to determine its practical application.
In this article, medium stability and storage stability of
the superhydrophobic silica particulate coating with
silica microspheres of 0.03 wt% has been investigated,
as shown in Fig. 7. The contact angle of the prepared
superhydrophobic silica particulate coating in acidic
and basic solution with pH value from 1 to 13 was
measured (Fig. 7a). The contact angles of the surface
were all larger than 160 in a wide range of pHvalue for
24 h. Such observation indicated that the silica partic-
ulate coating had a good mediumstability, probably due
to the intrinsic chemical stability of PFDTS and silica
particles. In addition, the superhydrophobic surface was
exposed in air for 3 months and its superhydrophobicity
did not decrease obviously. The values of the water
contact angles varied little, indicating the long-term
storage stability of the as-prepared superhydrophobic
surface (Fig. 7b). Besides medium stability and storage
stability, wear resistance is also a big problem to limit
the applications of superhydrophobic surfaces. In our
method, the superhydrophobic coating could be easily
destroyed because there was no strong chemical bond-
ing between silica coating and glass substrate. Thus, the
as-prepared superhydrophobic coating was not suitable
for a harsh environment.
Fig. 4: Photograph shows 15 lL (left) and 25 lL (right)
water droplets on the modied silica particulate coating,
prepared by spraying a mixed silica suspension on the
substrate with a silica microsphere concentration of
0.03 wt%. The water droplets would roll on the surface,
even at very low tilt angle
OH OH OH
Si Si Si
O
O O
O
O
OEt
OEt
OEt
F
3
C(CF
2
)
7
(CH
2
)
2
150 C, 3 h
Si
Si
Si
Si
Si Si
Si O
O
O
O
O
O O
R R R
O
O O
Fig. 5: Scheme shows surface ctionalization of surface
hydroxyl groups, exchanging for low energy peruorodec-
ylsilane groups. R represents the hydrophobic group:
CH
2
CH
2
(CF
2
)
7
CF
3
0 2 4 6
8 10
keV
Si
O
C
F
Fig. 6: EDX spectrum of the silica particulate coating with
silica microsphere concentration of 0.03 wt%. Inset is the
EDX scanning area
J. Coat. Technol. Res., 11 (4) 509515, 2014
513
Conclusions
In conclusion, superhydrophobic silica particulate
coatings were prepared by spraying an ethanol sus-
pension consisting of silica sol and silica microspheres.
A micro/nanoscale hierarchical structure was formed
by a one-step process and the morphology of the silica
particulate coatings could be varied with the silica
microsphere concentration. The unmodied coatings
were superhydrophilic with a water contact angle of
less than 5. After hydrophobic treatment with PFDTS
solution, all the surfaces achieved excellent superhy-
drophobicity, with water contact angles higher than
150 and sliding angles lower than 9. The superhy-
drophobic surfaces possessed a good stability, with
their superhydrophobicity being maintained after
3 months of exposure in air for a wide range of pH
values. Such stable superhydrophobic coatings with a
high water contact angle as well as a low sliding angle
provide a potential application in lotus effect type self-
cleaning. However, the superhydrophobic coating was
not suitable for a harsh environment because of the
weak wear resistance.
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175
170
165
160
155
150
145
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0 2 4 6 8 10 12 14
pH value
0 20 40 60 80 100
Days
175
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)
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)
(a) (b)
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silica spheres of 0.03 wt%. (b) Effect of storage time on the superhydrophobicity of the silica particulate coating with silica
spheres of 0.03 wt%
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