Cold Regions Science and Technology 138 (2017) 18–23

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Cold Regions Science and Technology

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

Robust anti-icing coatings via enhanced superhydrophobicity on

fiberglass cloth
Xiaolin Liu, Huawei Chen ⁎, Weipeng Kou, Deyuan Zhang
School of Mechanical Engineering and Automation, Beihang University, Beijing 100191, China

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

Article history: Robust superhydrophobic coatings with anti-icing properties were obtained by a simple approach, i.e., immers-
Received 26 March 2016 ing and spraying of adhesive/hydrophobic silica dispersion on fiberglass cloth. Scanning electron microscopy,
Received in revised form 15 November 2016 water contact angles, abrasion tests and dynamic icing tests were performed to characterize the morphology, hy-
Accepted 5 March 2017
drophobicity, mechanical durability and icephobicity of the coatings. The experimental results demonstrated that
Available online 6 March 2017
the coatings have good abrasion resistance. The water contact angle and the water sliding angle remain greater
Keywords:
than 150° and lower than 10°, respectively, after 60 cycles of abrasion. Furthermore, the anti-icing properties of
Anti-icing superhydrophobic surfaces were investigated under dynamic flow conditions. It was found that the coatings had
Fiberglass cloth the ability to delay ice nucleation without electrical heating, and avoid ice adhesion partly or even completely,
Superhydrophobic under a given mass of heat, which was much less than that of uncoated surfaces. The fiberglass cloth based coat-
Abrasion resistance ings could reduce by up to 51% of the heating power required to avoid ice accumulation, compared to uncoated
surfaces.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction occurs. Cao et al. (2009) prepared superhydrophobic surfaces using

Ice formation on surfaces may cause increasing severe problems that
will deteriorate performance of aircrafts, antennas, wind turbines,
power lines and cause unpredictable losses of life and property. Over
last decades, researchers have been dedicated in designing anti-icing
coatings to delay ice nucleation and reduce ice accretion. Until now, a
great amount of potential approaches such as superhydrophobic sur-
faces (Antonini et al., 2011; Mishchenko et al., 2010; Sarkar and
Farzaneh, 2009; Shen et al., 2015), slippery liquid infused porous sur-
faces (SLIPS) (Kim et al., 2012; Liu et al., 2015; Zhang et al., 2015),
anti-icing coating with an aqueous lubricating layer (Chen et al., 2014;
Dou et al., 2014) and antifreeze protein grafted surfaces (Gwak et al.,
2015) have been widely exploited to serve as anti-icing coatings. All of
these anti-icing strategies have been demonstrated to have the abilities
of reducing ice adhesion, delaying ice nucleation or repelling metastable
water droplets before freezing occurs. Due to convenience and simplic-
ity, superhydrophobic surfaces are still regarded as the most feasible
methods and are frequently applied.
In recent years, the feasibility of superhydrophobic surfaces working
as anti-icing coatings have been deeply researched. A large number of
reports have demonstrated that superhydrophobic surfaces can delay
ice nucleation and repel metastable water droplets before freezing
⁎ Corresponding author.
E-mail address: chenhw75@buaa.edu.cn (H. Chen).
nanoparticle-polymer composites for anti-icing, and demonstrated
that the anti-icing capability of the surfaces depended not only on
their superhydrophobicity but also on the surface morphology. He et
al. (2011) studied the effects of ZnO nanorod arrays superhydrophobic
surfaces towards ice/frost formation, and demonstrated that
superhydrophobicity to condensed micro-droplets at temperatures
below the freezing point is desirable for effectively retarding ice/frost
formation. Liao et al. (2015) studied the anti-icing performance in
glaze ice of nanostructured superhydrophobic film prepared by RF mag-
netron sputtering and hexadecyltrimethoxysilane modification, and
found that the nanostructured film could effectively reduce the freezing
area. Although these reports demonstrate that superhydrophobic sur-
faces are promising candidates for anti-icing applications, most of
these research just investigated the anti-icing properties of
superhydrophobic surface under static conditions or at low droplets ve-
locity. Without doubt, dynamic anti-icing performance, especially under
high droplets velocity conditions, is a practical challenge to the anti-
icing coatings.
In practical applications, anti-icing coatings often encounter ex-
treme environment like high wind, sand storm, freezing rain, etc. A
superhydrophobic surface must enhance its mechanical durability be-
fore working as a practical anti-icing coating. Recent research proposed
several approaches to improve the mechanical durability of the
superhydrophobic coatings such as adhesives (Lu et al., 2015) and tex-
tured surfaces (Jiang et al., 2014; Yokoi et al., 2015). However, dynamic
anti-icing tests have hardly been conducted for those coatings.

http://dx.doi.org/10.1016/j.coldregions.2017.03.004
0165-232X/© 2017 Elsevier B.V. All rights reserved.
 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23
In this work, the fiberglass cloth-based anti-icing coatings with su-
perior durability are firstly introduced. In our work, fiberglass cloth
and pressure-sensitive adhesive are combined and applied to improve
the durability of the coatings. Comparative experiments are carried
out to confirm their superior mechanical durability and anti-icing per-
formance especially under the high droplets velocity conditions. These
results will be helpful to provide insights into the role of
superhydrophobicity and mechanical durability towards dynamic
anti-icing performance, and therefore, helpful for practical applications
of anti-icing coatings.
2. Material and methods
2.1. Materials
Aluminum (A1060) plates, 34 mm × 34 mm in size, were used as
substrates. Plain weave fiberglass cloth was commercially available,
and the diameter of the original filament is about 5 ± 0.5 μm, 50 ± 5 fil-
aments in one tow, and the center distance between the tows is about
400 μm. (George et al., 2016) Pressure-sensitive adhesive was obtained
from 3 M Company. The hydrophobic SiO2 nanoparticles were obtained
from Wacker Chemie AG. 1H,1H,2H,2H-Perfluorodecyltriethoxysilane
(FAS-17) was obtained from SICONG chemical. Ethanol (Analytical re-
agent) and acetone (Analytical reagent) was purchased from Beijing
Chemical Works.
2.2. Fabrication of robust superhydrophobic coatings FC and AA
Two kinds of superhydrophobic coatings, i.e., with fiberglass cloth
(named FC, the acronym of fiberglass cloth) and without fiberglass
cloth (named AA, the acronym of aluminum/adhesive), were prepared
to investigate the durability. The procedure of fabricating
superhydrophobic surfaces are illustrated as shown in Fig.1.
2.2.1. Preparation of silica dispersion for spraying
A certain amount of hydrophobic fumed silica was added into ace-
tone and the dispersion was dispersed for 30 min in an ultrasonic
cleaner.
2.2.2. Preparation of adhesive-silica dispersion for immersing
Pressure-sensitive adhesive and hydrophobic fumed silica were
added into acetone. The weight ratios of adhesive and silica to acetone
were 0.03 and 0.012, respectively. And then the dispersion was dis-
persed for 10 min in an ultrasonic cleaner.
Fig. 1. Schematic of the fabrication of superhydrophobic coatings (a) FC and (b) AA.
19
2.2.3. Preparation of the fiberglass cloth based superhydrophobic coatings
FC
Fiberglass cloth was immersed into adhesive-silica dispersion for
2 min, spread out and entirely dried at room temperature. Subsequent-
ly, a thin layer of about 100 μm of pressure-sensitive adhesive was
sprayed on the aluminum substrates, and then the treated fiberglass
cloth was spread out and adhered to the substrates. Finally, the
superhydrophobic coating FC was obtained by spraying a thin layer of
silica dispersion onto the fiberglass cloth and FAS-17 was used to mod-
ify the possibly exposed part of the fiberglass and adhesives (Ganesh et
al., 2013; Yokoi et al., 2015).
2.2.4. Preparation of the aluminum/adhesive based superhydrophobic coat-
ings AA
To recognize the effect of fiberglass cloth, aluminum/adhesive based
superhydrophobic coatings AA were fabricated with adhesive and silica
dispersion, but without fiberglass cloth. After the pressure-sensitive ad-
hesive spraying step, the aluminum substrates were immersed into ad-
hesive-silica dispersion for 2 min. Then the aluminum/adhesive based
superhydrophobic coating AA was obtained by spraying a thin layer of
silica dispersion onto the substrates, and FAS-17 was used to modify
the possibly exposed part of the fiberglass and adhesives.
The main difference between these two coatings is the fiberglass
cloth which provided the regular micron-sized texture.
2.3. Characterization of robust superhydrophobic coatings FC and AA
The water contact angles (WCA) and water sliding angles (WSA)
were measured using 5 μL deionized water droplet on a SL200B Static
and Dynamic Optical Contact Angle Goniometer (Shanghai SOLON In-
formation Technology Co., Ltd.). The morphology of the coatings was
examined using a scanning electron microscopy (SEM, JCM 6010).
Sandpaper abrasion tests were carried out to measure the mechanical
durability of the coatings. The anti-icing properties of the coating FC
were investigated under dynamic flow conditions using a custom-
made low-temperature testing device.
3. Results and discussion
3.1. Morphology of the coatings
Superhydrophobic performance is dependent upon enough surface
roughness and low surface energy (Cassie and Baxter, 1944; Wenzel,
1936). Apart from low surface energy of hydrophobic SiO2 nanoparti-
cles, controlling morphology of coating surface is also necessary for
superhydrophobic performance.
The SEM images of the sample surfaces are presented in Fig.2. Fig.2a
shows the morphology of fiberglass cloth after immersed in adhesive-
20 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23
Fig. 2. SEM images and WCAs of FC and AA: (a) FC sample after immersed in adhesive-silica dispersion, before silica dispersion sprayed; (b) as-prepared FC sample; (c) as-prepared AA
sample.
silica dispersion, on which a thin layer of adhesive as well as silica nano-
particles was deposited. After this immersing process, the coating have
already shown superhydrophobic performance. To further enhance its
superhydrophobicity, the silica dispersion spraying step was carried
out. Fig.2b, corresponding to the as-prepared coating FC, illustrates
that a thicker layer of silica nanoparticles was deposited on the fiber-
glass cloth and filled into the space between the fibers. By directly
using the fiberglass cloth as template, the micro-nano hierarchical
structure was easily achieved for desirable surface roughness.
The morphology of AA sample is shown in Fig.2c. Although no regu-
lar micro-textures, AA obtained microstructure during the adhesive
spraying process as well as nanostructure by self-assembly during the
silica dispersion spraying process.
3.2. Mechanical durability of the coatings
Abrasion tests were carried out to measure the mechanical durabil-
ity of the superhydrophobic coatings FC and AA. The substrates were
placed onto 2000 grit sandpaper upside down, while a weight of 100 g
was applied to the substrates. The substrates were moved for 15 cm
with a moving speed of 30 mm/s. WCAs and WSAs were measured
after every 10 abrasion cycles. The results are presented in Fig.3,
which illustrates that the WCAs of FC still maintained greater than
150° after 80 cycles of abrasion, and the WSAs of FC still maintained
lower than 10° after 60 cycles of abrasion. The WSAs of FC just increased
to 19.3° after 80 cycles of abrasion. However, for AA, the WCAs de-
creased to 147.8° only after 40 cycles of abrasion, and the WSAs in-
creased to over 90° after 80 abrasion cycles. The results demonstrate
that the fiberglass cloth coatings FC have strong abrasion resistance,
and much stronger than non-fiberglass cloth coatings AA.
Fig. 3. Abrasion tests of superhydrophobic coatings FC and AA. The inset is the schematic of
the abrasion test.
The SEM images of samples after abrasion tests are presented in
Fig.4. Fig.4a shows the SEM images of FC sample after 60 abrasion cycles.
Although some of the silica nanoparticles were taken away by abrasion
process (shown in the red circle), most of the silica nanoparticles were
locked in the gaps between the fibers (shown in the yellow circle),
which contributed to the abrasion resistance of the coatings. On the
contrary, Fig.4b and Fig.4c show the SEM images of AA sample after 60
abrasion cycles, demonstrating that the surface of AA sample was flat-
tened by abrasion action, and fragments of adhesive-silica mixture can
be seen on the sample surface (shown in the orange circle). Those frag-
ments can be taken away easily by airflow, water flow or by mechanical
abrasion, which cause a loss of silica nanoparticles, and then,
superhydrophobic properties.
There is no doubt that the adhesive plays a significant role in en-
hancing the mechanical durability. But we believe that the regular mi-
cron-sized texture of fiberglass cloth provided the coatings with
conspicuous ability of clamping silica nanoparticles. As is shown in
Fig.4d, in virtue of the regular micron-sized texture of fiberglass cloth,
only raised areas could be abraded, which was a negligible portion of
the coating surface. The adhesives deposited on the fibers prevented
most of the silica nanoparticles of the abraded area from being taken
away. And the space between fiber pieces of the abraded areas still
played an effective role of clamping silica nanoparticles and keeping
superhydrophobic performance.
3.3. Anti-icing properties of the coating surface
Dynamic icing tests were performed using a custom-made low-tem-
perature testing device (shown in Fig.5) to characterize the anti-icing
properties of the coating FC. The icing conditions are shown in Table 1.
The low-temperature container provided a cold environment in which
the temperature was maintained at −35 ± 5 °C. A square tube (width
110 mm, height 110 mm, length 360 mm) was used to confine flow of
cold wind. Airblast atomizer, whose nozzle diameter is 1 mm, was ad-
justed to spray cold wind with a speed of about 10 ± 0.5 m/s as well
as continuous water droplets with a mean volume diameter (MVD) of
about 30 ± 5 μm. Water was supplied to the airblast atomizer at a con-
stant rate (14.5 g/min), resulting in the Liquid Water Content (LWC) of
about 2.0 g/m3. The samples were placed side-by-side on the sample
holder at an inclination angle of 30°. Two identical ceramic heaters
were adhered to the bottom of the samples with thermally conductive
silicone rubber so as to heat the samples. One of the two samples was
coated with FC while the other was bare aluminum substrate (named
bare-Al) or coated with AA as a direct contrast. The process of ice forma-
tion was monitored by a digital camera and lasted for a constant interval
of 150 s. Different heating power was given to investigate the effect of
energy saving of the FC compared to bare-Al or AA.
The size of the samples is 34 mm × 34 mm, a little bit smaller than
the ceramic heaters, which is 40 mm × 40 mm, to eliminate the effect
of the edges and make sure the sample surface is uniformly heated.
Two identical ceramic heaters were parallel connected so that the
 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23 21

Fig. 4. SEM images of FC and AA after abrasion tests. (a) FC sample after abrasion; (b) and (c) AA sample after abrasion, at low and high magnification, respectively; (d) Schematic of the
abrasion effects upon the fiberglass cloth based superhydrophobic coating. Most of the silica nanoparticles were boned to the fibers and clamped by the space between the fiber pieces.

Fig. 5. Schematic of the custom-made low-temperature testing device.

same heating power would applied to two samples in each test. Change
the applied voltages and compare the icing performance of two sam-
ples. We take heating power density (Pd, heating power per unit area,
W/cm2) as the criterion to judge the energy consumption.
3.3.1. Anti-icing performance of FC compared to bare-Al
The icing performance of FC and bare-Al sample without electrical
heating and the icing area fraction of the sample surfaces are shown in
Fig.6. Time-lapse images of the ice formation illustrate that mixed ice
on bare-Al sample kept developing rapidly during this test, and almost
completely covered the sample surface in 30 s; Rime ice on FC sample
kept developing much slower than bare-Al sample, from the lower left
corner to the whole sample surface. When bare-Al sample was
completely covered with mixed ice, only 24% of FC sample was covered
with rime ice, forming a sharp contrast. These results demonstrated that
fiberglass cloth based superhydrophobic coatings had the ability of re-
markably delaying ice nucleation without electrical heating.
The icing performance of FC and bare-Al sample with electrical
heating is shown in Fig.7. A group of tests with different heating
power were carried out here and four typical tests were selected to re-
flect the key results. When the applied voltage was 5 V (Pd =
0.239 W/cm2, Fig.7a), bare-Al sample was fully covered with rime ice,
while only nearly half of FC sample was covered. When the voltage
was increased to 7 V (Pd = 0.473 W/cm2, Fig.7b), bare-Al sample was
half covered with mixed ice (mixture of rime ice, clear ice and even
Table 1.
Icing conditions of dynamic icing tests.
Icing conditions Air speed [m/s] Temperature [°C] LWC [g/m3]
10 ± 0.5 −35 ± 5 2.0
liquid water), and the mixed ice kept developing into a 24 mm long
tip at the leading edge of the sample. By contrast, only a tiny piece of
ice gathered at the leading edge of FC sample, and it was noticed that
the ice piece was partly peeling off from the surface. Then the voltage
was finely increased to 7.4 V (Pd = 0. 525 W/cm2, Fig.7c) and no ice ac-
cumulated on the surface of FC sample while a large amount of mixed
ice could still be found on bare-Al sample. During this test, in fact,
there were tiny pieces of ice gathering at the leading edge of FC sample,
but periodically blown away by the wind, as is shown in Fig.8. Till the
voltage was increased to 10.8 V (Pd = 1.080 W/cm2, Fig.7d), little
mixed ice could accumulate on bare-Al sample. Repeated tests were
conducted to eliminate the influence of accidental factors.
With the help of electrical heating, FC showed outstanding perfor-
mance on anti-icing: the adhesive force between FC and ice was much
smaller than bare-Al substrate, and the accumulated ice was easy to
be blown away by wind. However, the mixed ice kept developing on
bare-Al sample throughout the test. Only when the applied voltage
was high enough (10.8 V in this test, for example), would the bare-Al
sample be able to avoid ice accumulating. In comparison with bare-Al
sample, FC sample was able to avoid icing under a smaller heating
power, saving 51% of the energy.
3.3.2. Anti-icing performance of FC compared to AA
The results of the abrasion tests have demonstrated that the fiber-
glass cloth coatings FC have better mechanical durability than non-fi-
berglass cloth coatings AA. To investigate the role of mechanical
durability on anti-icing performance, another group of dynamic icing
tests were performed and four typical tests were selected to reflect
MVD [μm] the key results.
The icing performance of FC and AA with electrical heating is shown
30 ± 5
in Fig.9. Fig.9a shows icing cycles of FC (right) and AA (left) without
22 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23
Fig. 6. Time-lapse images of the ice formation on bare-Al and FC without electrical heating (a), and the icing area fraction of the sample surfaces (b): Mixed ice on bare-Al (left) kept
developing rapidly during this test, and almost completely covered the sample surface in 30 s. Rime ice on FC sample (right) kept developing slowly during this test, from the lower
left corner to the whole sample surface, but much slower than bare-Al sample.
electric heating. For each cycle of icing tests, the icing area fraction of AA
was always larger than that of FC. The anti-icing property of AA deteri-
orated rapidly with the increase of icing cycles, and after 5 cycles of icing
tests, the surface of AA was completely covered by rime ice. However,
the anti-icing property of FC maintained steady, and only 42% of FC sur-
face was covered after 5 cycles of icing tests. The results demonstrated
that FC have better durability than AA.
Fig.9b shows the icing tests with different heating power: When the
applied voltage was 5 V (Pd = 0.239 W/cm2) or 6 V (Pd =
0.349 W/cm2), the icing area of AA was always larger than that of FC.
Then the voltage was increased to 7.4 V (Pd = 0.525 W/cm2) and no
ice accumulated on the surface of FC while some rime ice mixed with
liquid water could still be found on AA (circled with the white dotted
line). Till the voltage was increased to 7.9 V (Pd = 0.605 W/cm2), no
ice could accumulate on both samples. Repeated tests were conducted
to eliminate the influence of accidental factors.
This group of dynamic icing tests demonstrated that FC have better
anti-icing performance than AA, which indicated that better mechanical
durability may markedly enhance the coatings' anti-icing performance.
However, it should be noted that, although defeated by FC, AA still per-
formed much better than bare-Al sample, reducing by up to 44% of the
energy.
Fig. 7. Digital images (top view) of dynamic icing tests of FC and bare-Al with different
heating power. Heating power density of every single ceramic heater was (a)
0.239 W/cm2, (b) 0.473 W/cm2, (c) 0.525 W/cm2 and (d) 1.080 W/cm2.
4. Conclusion
A very simple immersing-spraying method was proposed to fabri-
cate abrasion resistant superhydrophobic coatings based on fiberglass
cloth, of which the WCA was 156.0° and the WSA was smaller than
1.0°. The prepared coatings showed good superhydrophobicity and me-
chanical durability. Little decrease of superhydrophobicity could be no-
ticed after 60 cycles of abrasion. And we believe that the regular micron-
sized texture of fiberglass cloth, with the cooperation of the adhesive,
provided the coatings with conspicuous ability of clamping silica nano-
particles. Dynamic icing tests were performed using a custom-made
low-temperature testing device to characterize the anti-icing properties
of the coatings. And the results demonstrated that fiberglass cloth based
superhydrophobic coatings had the ability of remarkably delaying ice
nucleation without electrical heating. And with the help of electrical
heating, the FC coating showed outstanding performance on anti-
icing: the adhesive force between the FC coating and ice was much
smaller than uncoated surface, and the accumulated ice was easy to be
blown away by wind. In comparison with uncoated surfaces, FC sample
Fig. 8. Digital images (top view) of the ice formation on FC and bare-Al when applied
voltage was 7.4 V: (a), test started; (b) and (c), tiny piece of ice gathered and blown
away from FC; (d), (e) and (f), tiny piece of ice slipping off the leading edge of FC.
Mixed ice on bare-Al sample kept developing during this test.
 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23
Fig. 9. Digital images (top view) of dynamic icing tests of FC and AA: (a) Icing cycles
without electric heating; (b) Icing tests with different heating power, and the heating
power density of every single ceramic heater was 0.239 W/cm2, 0.349 W/cm2, and
0.525 W/cm2, respectively.
could avoid icing under a smaller heating power, reducing by up to 51%
of the energy. These results will be helpful to provide insights into the
role of superhydrophobicity and mechanical durability towards dynam-
ic anti-icing performance, and therefore, helpful for practical applica-
tions of anti-icing coatings. This fabrication method is simple, low-
cost, and suitable for large-scale application.
Acknowledgement
This work was supported by the National Natural Science Founda-
tion of China (Grants 51175020) and NSFC Major Program (51290292).
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