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

Contents lists available at ScienceDirect

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

nanoparticle-polymer composites for anti-icing, and demonstrated
Ice formation on surfaces may cause increasing severe problems that that the anti-icing capability of the surfaces depended not only on
will deteriorate performance of aircrafts, antennas, wind turbines, their superhydrophobicity but also on the surface morphology. He et
power lines and cause unpredictable losses of life and property. Over al. (2011) studied the effects of ZnO nanorod arrays superhydrophobic
last decades, researchers have been dedicated in designing anti-icing surfaces towards ice/frost formation, and demonstrated that
coatings to delay ice nucleation and reduce ice accretion. Until now, a superhydrophobicity to condensed micro-droplets at temperatures
great amount of potential approaches such as superhydrophobic sur- below the freezing point is desirable for effectively retarding ice/frost
faces (Antonini et al., 2011; Mishchenko et al., 2010; Sarkar and formation. Liao et al. (2015) studied the anti-icing performance in
Farzaneh, 2009; Shen et al., 2015), slippery liquid infused porous sur- glaze ice of nanostructured superhydrophobic film prepared by RF mag-
faces (SLIPS) (Kim et al., 2012; Liu et al., 2015; Zhang et al., 2015), netron sputtering and hexadecyltrimethoxysilane modification, and
anti-icing coating with an aqueous lubricating layer (Chen et al., 2014; found that the nanostructured film could effectively reduce the freezing
Dou et al., 2014) and antifreeze protein grafted surfaces (Gwak et al., area. Although these reports demonstrate that superhydrophobic sur-
2015) have been widely exploited to serve as anti-icing coatings. All of faces are promising candidates for anti-icing applications, most of
these anti-icing strategies have been demonstrated to have the abilities these research just investigated the anti-icing properties of
of reducing ice adhesion, delaying ice nucleation or repelling metastable superhydrophobic surface under static conditions or at low droplets ve-
water droplets before freezing occurs. Due to convenience and simplic- locity. Without doubt, dynamic anti-icing performance, especially under
ity, superhydrophobic surfaces are still regarded as the most feasible high droplets velocity conditions, is a practical challenge to the anti-
methods and are frequently applied. icing coatings.
In recent years, the feasibility of superhydrophobic surfaces working In practical applications, anti-icing coatings often encounter ex-
as anti-icing coatings have been deeply researched. A large number of treme environment like high wind, sand storm, freezing rain, etc. A
reports have demonstrated that superhydrophobic surfaces can delay superhydrophobic surface must enhance its mechanical durability be-
ice nucleation and repel metastable water droplets before freezing 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-
⁎ Corresponding author. tured surfaces (Jiang et al., 2014; Yokoi et al., 2015). However, dynamic
E-mail address: [email protected] (H. Chen). 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 19

In this work, the fiberglass cloth-based anti-icing coatings with su- 2.2.3. Preparation of the fiberglass cloth based superhydrophobic coatings
perior durability are firstly introduced. In our work, fiberglass cloth FC
and pressure-sensitive adhesive are combined and applied to improve Fiberglass cloth was immersed into adhesive-silica dispersion for
the durability of the coatings. Comparative experiments are carried 2 min, spread out and entirely dried at room temperature. Subsequent-
out to confirm their superior mechanical durability and anti-icing per- ly, a thin layer of about 100 μm of pressure-sensitive adhesive was
formance especially under the high droplets velocity conditions. These sprayed on the aluminum substrates, and then the treated fiberglass
results will be helpful to provide insights into the role of cloth was spread out and adhered to the substrates. Finally, the
superhydrophobicity and mechanical durability towards dynamic superhydrophobic coating FC was obtained by spraying a thin layer of
anti-icing performance, and therefore, helpful for practical applications silica dispersion onto the fiberglass cloth and FAS-17 was used to mod-
of anti-icing coatings. ify the possibly exposed part of the fiberglass and adhesives (Ganesh et
al., 2013; Yokoi et al., 2015).

2. Material and methods 2.2.4. Preparation of the aluminum/adhesive based superhydrophobic coat-
ings AA
2.1. Materials To recognize the effect of fiberglass cloth, aluminum/adhesive based
superhydrophobic coatings AA were fabricated with adhesive and silica
Aluminum (A1060) plates, 34 mm × 34 mm in size, were used as dispersion, but without fiberglass cloth. After the pressure-sensitive ad-
substrates. Plain weave fiberglass cloth was commercially available, hesive spraying step, the aluminum substrates were immersed into ad-
and the diameter of the original filament is about 5 ± 0.5 μm, 50 ± 5 fil- hesive-silica dispersion for 2 min. Then the aluminum/adhesive based
aments in one tow, and the center distance between the tows is about superhydrophobic coating AA was obtained by spraying a thin layer of
400 μm. (George et al., 2016) Pressure-sensitive adhesive was obtained silica dispersion onto the substrates, and FAS-17 was used to modify
from 3 M Company. The hydrophobic SiO2 nanoparticles were obtained the possibly exposed part of the fiberglass and adhesives.
from Wacker Chemie AG. 1H,1H,2H,2H-Perfluorodecyltriethoxysilane The main difference between these two coatings is the fiberglass
(FAS-17) was obtained from SICONG chemical. Ethanol (Analytical re- cloth which provided the regular micron-sized texture.
agent) and acetone (Analytical reagent) was purchased from Beijing
Chemical Works. 2.3. Characterization of robust superhydrophobic coatings FC and AA

The water contact angles (WCA) and water sliding angles (WSA)
2.2. Fabrication of robust superhydrophobic coatings FC and AA were measured using 5 μL deionized water droplet on a SL200B Static
and Dynamic Optical Contact Angle Goniometer (Shanghai SOLON In-
Two kinds of superhydrophobic coatings, i.e., with fiberglass cloth formation Technology Co., Ltd.). The morphology of the coatings was
(named FC, the acronym of fiberglass cloth) and without fiberglass examined using a scanning electron microscopy (SEM, JCM 6010).
cloth (named AA, the acronym of aluminum/adhesive), were prepared Sandpaper abrasion tests were carried out to measure the mechanical
to investigate the durability. The procedure of fabricating durability of the coatings. The anti-icing properties of the coating FC
superhydrophobic surfaces are illustrated as shown in Fig.1. were investigated under dynamic flow conditions using a custom-
made low-temperature testing device.

2.2.1. Preparation of silica dispersion for spraying 3. Results and discussion

A certain amount of hydrophobic fumed silica was added into ace-
tone and the dispersion was dispersed for 30 min in an ultrasonic 3.1. Morphology of the coatings
cleaner.
Superhydrophobic performance is dependent upon enough surface
roughness and low surface energy (Cassie and Baxter, 1944; Wenzel,
2.2.2. Preparation of adhesive-silica dispersion for immersing 1936). Apart from low surface energy of hydrophobic SiO2 nanoparti-
Pressure-sensitive adhesive and hydrophobic fumed silica were cles, controlling morphology of coating surface is also necessary for
added into acetone. The weight ratios of adhesive and silica to acetone superhydrophobic performance.
were 0.03 and 0.012, respectively. And then the dispersion was dis- The SEM images of the sample surfaces are presented in Fig.2. Fig.2a
persed for 10 min in an ultrasonic cleaner. shows the morphology of fiberglass cloth after immersed in adhesive-

Fig. 1. Schematic of the fabrication of superhydrophobic coatings (a) FC and (b) AA.
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- The SEM images of samples after abrasion tests are presented in
particles was deposited. After this immersing process, the coating have Fig.4. Fig.4a shows the SEM images of FC sample after 60 abrasion cycles.
already shown superhydrophobic performance. To further enhance its Although some of the silica nanoparticles were taken away by abrasion
superhydrophobicity, the silica dispersion spraying step was carried process (shown in the red circle), most of the silica nanoparticles were
out. Fig.2b, corresponding to the as-prepared coating FC, illustrates locked in the gaps between the fibers (shown in the yellow circle),
that a thicker layer of silica nanoparticles was deposited on the fiber- which contributed to the abrasion resistance of the coatings. On the
glass cloth and filled into the space between the fibers. By directly contrary, Fig.4b and Fig.4c show the SEM images of AA sample after 60
using the fiberglass cloth as template, the micro-nano hierarchical abrasion cycles, demonstrating that the surface of AA sample was flat-
structure was easily achieved for desirable surface roughness. tened by abrasion action, and fragments of adhesive-silica mixture can
The morphology of AA sample is shown in Fig.2c. Although no regu- be seen on the sample surface (shown in the orange circle). Those frag-
lar micro-textures, AA obtained microstructure during the adhesive ments can be taken away easily by airflow, water flow or by mechanical
spraying process as well as nanostructure by self-assembly during the abrasion, which cause a loss of silica nanoparticles, and then,
silica dispersion spraying process. 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-
3.2. Mechanical durability of the coatings cron-sized texture of fiberglass cloth provided the coatings with
conspicuous ability of clamping silica nanoparticles. As is shown in
Abrasion tests were carried out to measure the mechanical durabil- Fig.4d, in virtue of the regular micron-sized texture of fiberglass cloth,
ity of the superhydrophobic coatings FC and AA. The substrates were only raised areas could be abraded, which was a negligible portion of
placed onto 2000 grit sandpaper upside down, while a weight of 100 g the coating surface. The adhesives deposited on the fibers prevented
was applied to the substrates. The substrates were moved for 15 cm most of the silica nanoparticles of the abraded area from being taken
with a moving speed of 30 mm/s. WCAs and WSAs were measured away. And the space between fiber pieces of the abraded areas still
after every 10 abrasion cycles. The results are presented in Fig.3, played an effective role of clamping silica nanoparticles and keeping
which illustrates that the WCAs of FC still maintained greater than superhydrophobic performance.
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 3.3. Anti-icing properties of the coating surface
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- Dynamic icing tests were performed using a custom-made low-tem-
creased to over 90° after 80 abrasion cycles. The results demonstrate perature testing device (shown in Fig.5) to characterize the anti-icing
that the fiberglass cloth coatings FC have strong abrasion resistance, properties of the coating FC. The icing conditions are shown in Table 1.
and much stronger than non-fiberglass cloth coatings AA. 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
Fig. 3. Abrasion tests of superhydrophobic coatings FC and AA. The inset is the schematic of of the edges and make sure the sample surface is uniformly heated.
the abrasion test. 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 liquid water), and the mixed ice kept developing into a 24 mm long
the applied voltages and compare the icing performance of two sam- tip at the leading edge of the sample. By contrast, only a tiny piece of
ples. We take heating power density (Pd, heating power per unit area, ice gathered at the leading edge of FC sample, and it was noticed that
W/cm2) as the criterion to judge the energy consumption. 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-
3.3.1. Anti-icing performance of FC compared to bare-Al cumulated on the surface of FC sample while a large amount of mixed
The icing performance of FC and bare-Al sample without electrical ice could still be found on bare-Al sample. During this test, in fact,
heating and the icing area fraction of the sample surfaces are shown in there were tiny pieces of ice gathering at the leading edge of FC sample,
Fig.6. Time-lapse images of the ice formation illustrate that mixed ice but periodically blown away by the wind, as is shown in Fig.8. Till the
on bare-Al sample kept developing rapidly during this test, and almost voltage was increased to 10.8 V (Pd = 1.080 W/cm2, Fig.7d), little
completely covered the sample surface in 30 s; Rime ice on FC sample mixed ice could accumulate on bare-Al sample. Repeated tests were
kept developing much slower than bare-Al sample, from the lower left conducted to eliminate the influence of accidental factors.
corner to the whole sample surface. When bare-Al sample was With the help of electrical heating, FC showed outstanding perfor-
completely covered with mixed ice, only 24% of FC sample was covered mance on anti-icing: the adhesive force between FC and ice was much
with rime ice, forming a sharp contrast. These results demonstrated that smaller than bare-Al substrate, and the accumulated ice was easy to
fiberglass cloth based superhydrophobic coatings had the ability of re- be blown away by wind. However, the mixed ice kept developing on
markably delaying ice nucleation without electrical heating. bare-Al sample throughout the test. Only when the applied voltage
The icing performance of FC and bare-Al sample with electrical was high enough (10.8 V in this test, for example), would the bare-Al
heating is shown in Fig.7. A group of tests with different heating sample be able to avoid ice accumulating. In comparison with bare-Al
power were carried out here and four typical tests were selected to re- sample, FC sample was able to avoid icing under a smaller heating
flect the key results. When the applied voltage was 5 V (Pd = power, saving 51% of the energy.
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 3.3.2. Anti-icing performance of FC compared to AA
was increased to 7 V (Pd = 0.473 W/cm2, Fig.7b), bare-Al sample was The results of the abrasion tests have demonstrated that the fiber-
half covered with mixed ice (mixture of rime ice, clear ice and even glass cloth coatings FC have better mechanical durability than non-fi-
berglass cloth coatings AA. To investigate the role of mechanical
Table 1. durability on anti-icing performance, another group of dynamic icing
Icing conditions of dynamic icing tests. tests were performed and four typical tests were selected to reflect
Icing conditions Air speed [m/s] Temperature [°C] LWC [g/m3] MVD [μm] the key results.
The icing performance of FC and AA with electrical heating is shown
10 ± 0.5 −35 ± 5 2.0 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 4. Conclusion
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 A very simple immersing-spraying method was proposed to fabri-
tests, the surface of AA was completely covered by rime ice. However, cate abrasion resistant superhydrophobic coatings based on fiberglass
the anti-icing property of FC maintained steady, and only 42% of FC sur- cloth, of which the WCA was 156.0° and the WSA was smaller than
face was covered after 5 cycles of icing tests. The results demonstrated 1.0°. The prepared coatings showed good superhydrophobicity and me-
that FC have better durability than AA. chanical durability. Little decrease of superhydrophobicity could be no-
Fig.9b shows the icing tests with different heating power: When the ticed after 60 cycles of abrasion. And we believe that the regular micron-
applied voltage was 5 V (Pd = 0.239 W/cm2) or 6 V (Pd = sized texture of fiberglass cloth, with the cooperation of the adhesive,
0.349 W/cm2), the icing area of AA was always larger than that of FC. provided the coatings with conspicuous ability of clamping silica nano-
Then the voltage was increased to 7.4 V (Pd = 0.525 W/cm2) and no particles. Dynamic icing tests were performed using a custom-made
ice accumulated on the surface of FC while some rime ice mixed with low-temperature testing device to characterize the anti-icing properties
liquid water could still be found on AA (circled with the white dotted of the coatings. And the results demonstrated that fiberglass cloth based
line). Till the voltage was increased to 7.9 V (Pd = 0.605 W/cm2), no superhydrophobic coatings had the ability of remarkably delaying ice
ice could accumulate on both samples. Repeated tests were conducted nucleation without electrical heating. And with the help of electrical
to eliminate the influence of accidental factors. heating, the FC coating showed outstanding performance on anti-
This group of dynamic icing tests demonstrated that FC have better icing: the adhesive force between the FC coating and ice was much
anti-icing performance than AA, which indicated that better mechanical smaller than uncoated surface, and the accumulated ice was easy to be
durability may markedly enhance the coatings' anti-icing performance. blown away by wind. In comparison with uncoated surfaces, FC sample
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. 8. Digital images (top view) of the ice formation on FC and bare-Al when applied
Fig. 7. Digital images (top view) of dynamic icing tests of FC and bare-Al with different voltage was 7.4 V: (a), test started; (b) and (c), tiny piece of ice gathered and blown
heating power. Heating power density of every single ceramic heater was (a) away from FC; (d), (e) and (f), tiny piece of ice slipping off the leading edge of FC.
0.239 W/cm2, (b) 0.473 W/cm2, (c) 0.525 W/cm2 and (d) 1.080 W/cm2. Mixed ice on bare-Al sample kept developing during this test.
 X. Liu et al. / Cold Regions Science and Technology 138 (2017) 18–23 23

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