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Zwitterionic polymer brush coatings with excellent

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anti-fog and anti-frost properties†

Cite this: RSC Adv., 2016, 6, 61695
Metwally Ezzat and Chun-Jen Huang*

Received 12th May 2016
Accepted 22nd June 2016
DOI: 10.1039/c6ra12399f
www.rsc.org/advances
The formation of fog and frost on transparent surfaces can lead to many problems in our daily life. To
address these problems, polymer brushes based on two zwitterionic analogues, poly(sulfobetaine
methacrylate) (pSBMA) and poly(sulfobetaine vinylimidazole) (pSBVI), have been prepared by surface-
initiated atom transfer radical polymerization (SI-ATRP). Hydrophilic and superhydrophilic pSBMA and
pSBVI polymer brushes were prepared by controlling the thickness of the coatings to study the effect of
wettability on the anti-fog and anti-frost properties. X-ray photoelectron spectroscopy (XPS),
ellipsometry and atomic force microscopy (AFM) were respectively used to determine the interfacial
elemental composition, the thickness and the morphology of the brushes. The wettability of the polymer
brushes was measured using a water contact angle goniometer. Their anti-fog and anti-frost capabilities
were determined visually and tested quantitatively by UV-vis spectroscopy. The results indicated that the
optical transmittance of substrates modified with superhydrophilic polymer coatings under both hot and
cold fogging conditions was very high. Additionally, no visible frost was formed on the superhydrophilic
substrates after storage in a freezer at
20  C for the duration of the experiment. These results
convincingly demonstrated that the resistance of the modified substrates to fogging and frosting is
strongly correlated to the surface wettability. Moreover, there is no considerable difference in the
performance of pSBMA and pSBVI polymer brushes, but the former is preferred because SBMA
monomer is commercially available and requires short polymerization time to obtain superhydrophilicity.

hydrophilic inorganic nanoparticles such as SiO2 and

Introduction
Condensation of water droplets or ice crystallization on surfaces
in a variety of environmental conditions causes fog and/or frost
formation, which in turn interferes with the light path and
reduces optical transmission. This may lead to many problems
for the use of eyeglasses, windows, mirrors, goggles, and optical
instruments.1–4 Over the last few decades, an extensive research
studies have been reported to prevent the formation of fog and
frost on solid surfaces by different approaches including
superhydrophobic coatings,5–7 superhydrophilic coatings8,9 and
combinations of both hydrophilic and hydrophobic properties
in the coating.10–15 Hydrophilic surfaces that have a water
contact angle of less than 5 exhibit excellent anti-fog properties
because they allow water droplets to spread uniformly to form
a thin water lm, which reduces light scattering.9,16,17 In general,
superhydrophilicity can be obtained by various chemical and
physical methods.18 One common approach is to coat
Department of Biomedical Sciences and Engineering, National Central University,
Jhong-Li, Taoyuan 320, Taiwan. E-mail: cjhuang@ncu.edu.tw
† Electronic supplementary information (ESI) available: Detailed procedure for
the preparation of the initiator and SBVI monomer, 1H-NMR spectra for the
initiator and SBVI monomer, CA measurements, and digital images for hot
fogging aer exposure to hot water vapour for 30 s and 60 s. See DOI:
10.1039/c6ra12399f
TiO2.12,19,20 However, the fabrication methods for these mate-
rials involve multiple steps including seed growth, one dimen-
sion nanomaterial prefabrication and post treatments.21 In
addition, they typically require exposure to UV light to induce
photocatalytic activity and superhydrophilicity.22
On the other hand, hydrophilic polymers can be used as
coating materials for the preparation of superhydrophilic
surfaces. For instance, a polymer-based anti-fog coating cova-
lently graed onto glass surfaces by means of a multistep
process that includes spin coating of poly(ethylene-maleic
anhydride) (PEMA) and poly(vinyl alcohol) (PVA) layers has
been reported.1 The results showed that the PEMA/PVA coating
not only prolonged the initial period required for fog formation,
but also decreased the rate of light transmission decay. Addi-
tionally, these PEMA/PVA coatings remained stable and their
anti-fog properties were preserved aer immersion in water for
24 h. Moreover, Lee and co-workers demonstrated that a zwitter-
wettable surface prepared by layer-by-layer (LbL) assembly of
PVA and poly(acrylic acid) (PAA) functionalized with poly
(ethylene glycol methyl ether) (PEG) segments afforded
a signicantly enhanced anti-fog and anti-frost properties.23
Recently, we have developed a facile superhydrophilic surfaces
with signicant anti-fog and self-cleaning properties via sila-
nization of zwitterionic sulfobetaine silane (SBSi) on oxidized

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surfaces.24 These surfaces exhibited long-term stability under
exposure to heat and UV irradiation. The SBSi glasses main-
tained high optical transmittance due to the rapid formation of
coalesced water thin lms on surfaces in contact with vapour
and moisture.25,26
Zwitterionic poly(sulfobetaine methacrylate) (pSBMA) and
poly(sulfobetaine vinylimidazole) (pSBVI) are widely used as
anti-fouling materials in marine and biomedical applica-
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tions.27–30 Sulfobetaine pendant groups have strong hydration
capacity due to the ionic solvation.31–34 The use of surface-
initiated atom transfer radical polymerization (SI-ATRP) for
the preparation of polymer brushes enables precise control of
their architectural features, such as the graing density, the
thickness and the composition; therefore, the interfacial prop-
erties of polymer lms can be tuned exibly.35,36
It is important to explore the structure–property relationship
of sulfobetaine-based polymer brushes for better under-
standing of their correlation with the formation of fog and frost
on these surfaces. In this study, pSBMA and pSBVI polymer
brushes were prepared and the surface wetting properties were
altered by controlling the lm thicknesses. The tests for the fog
and frost formation were performed under both hot and cold
fogging conditions to verify the effect of the interfacial proper-
ties on water coalescence and frost densication. To the best of
our knowledge, this is the rst work to systematically investigate
and employ the zwitterionic pSBMA and pSBVI as anti-fog and
anti-frost coatings with an attempt to explore the structure–
property relationship.
Experimental section
Materials
[2-(Methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium
hydroxide (SBMA), N,N-dimethylformamide (DMF), copper(I)
bromide (99.999%), and 2,20 -bipyridyl (Bpy) were purchased
from Sigma-Aldrich. Tetrahydrofuran (THF, anhydrous) was
obtained from TEDIA. Triethylamine (TEA) and 2-bromoisobu-
tyryl bromide (BIBB) were purchased from Acros Organics. (3-
Aminopropyl)triethoxysilane, 1-vinylimidazole, and 1,3-pro-
panesultone were purchased from Alfa Aesar. All other chem-
icals were analytical grade reagents and used without any
further purication. Standard glass microscope slides (Green
cross medical) and silicon wafers (Semiconductor Wafer Inc.,
Taiwan) were cut into 2.5 cm  2.5 cm pieces before use.
Surface immobilization of ATRP initiator
The slides were cut into 2.5 cm  2.5 cm, and then sonicated in
ethanol and water for 15 min each and treated with piranha
solution (70 : 30 H2SO4 : H2O2) for 30 min at 100  C. Subse-
quently, the slides were immersed in hydrochloric acid solution
(1 : 6 HCl : H2O) for 15 min at room temperature and washed
thoroughly using ethanol and water before drying in a N2
atmosphere. The slides were immersed in a solution of 40 mM
of the initiator in THF for 24 h at room temperature. Finally, the
slides were washed sequentially with THF, ethanol, and water
and dried under nitrogen before polymerization.
61696 | RSC Adv., 2016, 6, 61695–61702
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SI-ATRP of SBMA and SBVI
For the synthesis of pSBMA brushes, 7.5 g of SBMA was dis-
solved in 50 mL H2O and MeOH (1 : 3). The solution was
bubbled with nitrogen for 3 h to remove oxygen, and then 332.5
mg of Bpy and 152.5 mg of CuBr were added in the solution to
achieve [SBMA] : [CuBr] : [BPy] molar ratio of 25 : 1 : 2. This
solution was further degassed using three freeze–pump–thaw
cycles. The mixture was transferred to vessels containing the
initiator-immobilized slides and sealed under nitrogen. The
reaction was carried out in a water bath at 60  C for 24 h.
Following a similar procedure, SI-ATRP of SBVI was performed
at [SBVI] : [CuBr] : [BPy] molar feed ratio of 30 : 1 : 2 in 1 : 2
H2O/DMF mixture at 60  C. The concentration of monomers in
the reaction solvents was 15% (w/v). To ensure that both glass
slides and silicon wafers were graed under the same condi-
tions, the polymerization was carried out in the same reaction
vessel. The polymerization was halted aer the specied reac-
tion time and the slides were repeatedly washed with warm
water and methanol, and dried under nitrogen.
Characterization
NMR spectra were recorded on a Bruker DRX-600 instrument.
The water contact angles were measured by the sessile-drop
method using an optical CA goniometry (Phoenix mini,
Surface Electro Optics) at ambient temperature. The volume of
the droplets from a microsyringe was 5 mL, and the measure-
ments were performed in triplicate at random positions on the
samples to characterize the average wetting properties of the
coatings. The brush thickness was measured using ellipsometry
(Angle Stokes Ellipsometer LSE, gaertner scientic) on silicon
wafers at ambient lab conditions in air. A light source with
a wavelength in 400–800 nm range at incidence angle of 70 was
used to scan the sample surface. The refractive index for the
polymer brushes (n ¼ 1.45) was measured automatically by
ellipsometry. The atomic force microscopy (AFM) images were
recorded on a commercial instrument (JSPM-5200) in tapping
mode under ambient conditions. The chemical composition
was detected by X-ray photoelectron spectroscopy (XPS) using
a VG Sigma Probe spectroscope using an Al Ka excitation source
(25 W, 15 mm) in a vacuum of 2  10
8 Pa. XPS spectra were
acquired with a pass energy of 58.8 eV. Scans were performed at
a take-off angle of 90 and the binding energy (BE) was esti-
mated to be accurate within 0.2 eV. The UV-vis transmission
spectra were measured using a UV-vis spectrophotometer (V-
630, Jasco).
Anti-fog and anti-frost tests
Both hot and cold fogging tests were used to quantify the anti-
fog properties of the polymer brush coatings. For the hot
fogging test, the coated glass slides were placed 5 cm above hot
water (80  C), and held for different time periods. Photographs
were then taken immediately aer the samples were removed
from the water vapour and compared to bare glass as a control
sample for each case. More aggressive conditions were used to
assess the anti-fog and anti-frost capabilities of the brushes. In
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brief, the samples were stored in a freezer at
20  C for 30 min
and 24 h, and photographs were taken immediately aer the
samples were removed from the freezer to visually estimate the
frost formation, which turns to fog aer exposure to ambient
conditions. The light transmittance in the range of 400–700 nm
was also recorded on UV-vis spectrophotometer during the
fogging and frosting experiments to quantitatively evaluate the
anti-fog and anti-frost properties of polymer brushes.
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brushes were grown from the graed initiators under appro-
priate conditions. In this work, pSBMA and pSBVI brushes with
similar dry thicknesses were used. In order to achieve this,
different polymerization times were conducted at a monomer
concentration of 0.5 M. The brush thicknesses (d) are shown in
Table 1. The brush thickness of pSBMA was 44 nm aer poly-
merization for 8 h, and 105 nm aer 24 h. Similar results were
obtained for pSBVI with d ¼ 45 nm and 134 nm aer poly-

merization for 12 h and 24 h, respectively.

Results and discussion
Synthesis and characterization of polymer brushes
The fabrication process of zwitterionic pSBMA and pSBVI is
illustrated in Scheme 1. The glass or silicon substrates were
rstly modied with ATRP initiator via self-assembly of the
initiator in anhydrous THF for 24 h, and then the polymer
The wettability of polymer brushes was measured using
a water CA goniometer and the results are summarized in Table 1
and ESI (Fig. S3†). The results showed a CA of 33 for the
unmodied glass with a negligible change aer immobilizing the
initiator. However, the CA decreased sharply aer graing both
pSBMA and pSBVI for respective polymerization times of 8 and 12
h and the surfaces became completely wet (CA < 5 ). On the other

Scheme 1 Synthesis procedure of pSBMA and pSBVI polymer brushes via SI-ATRP polymerization.

Table 1 Polymerization time (t) for SI-ATRP, dry film thickness (d), contact angle (CA) and surface roughness (Ra) of hydrophilic (H) and
superhydrophilic (SH) pSBMA and pSBVI grafted on silicon wafer substrates

t
Brush type (h) da (nm) CA Rab (nm) N/S ratio (theoretical) N/S ratio by XPS

pSBMA-SH 8 44 <5 0.27 1 0.9

pSBMA-H 24 105 15  3 0.45 — —
pSBVI-SH 12 45 <5 0.66 2 2.3
pSBVI-H 24 134 15  3 1.40 — —
a
Measured by ellipsometry. b Measured by AFM.

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Fig. 1 XPS spectra for: (a) initiator-modified silicon wafers, pSBMA and pSBVI polymer brushes, (b) high resolution scan of Br3d, (c) high resolution
scan of N1s region, and (d) high resolution scan of S2p region.

hand, hydrophilic brushes (CA 15  3 ) were obtained by

increasing the brush thicknesses via increasing the polymeriza-
tion time.
Herein, superhydrophilicity was observed aer 4 h for pSBMA
with d ¼ 23 nm. The polymerization time for pSBMA was, there-
fore, increased to 8 h to obtain a similar thickness to that of pSBVI
brushes. The superhydrophilic pSBMA and pSBVI coatings are
respectively named pSBMA-SH and pSBVI-SH. Upon increasing the
polymerization time to 24 h, both pSBMA and pSBVI brush coat-
ings became hydrophilic, pSBMA-H and pSBVI-H, owing to the
increase in thickness of the brushes. It has been reported that
zwitterionic polymer brushes with a thickness less than 50 nm
possess very strong interaction with water molecules, and so they
are very hydrophilic, while thicker brushes (thickness > 50 nm) lead
to an increase in the hydrophobicity.32,37,38 Azzaroni et al. studied
the correlation between the wettability of sulfobetaines and brush
thickness. It was found that the polyzwitterionic brush exhibits
a transition in the wetting characteristics, from non-associated
hydrophilic regime to self-associated hydrophobic regime, which
produces a completely collapsed self-associated state due to reor-
ganization processes within the macromolecular lm.37 In this
study, we could nd that thinner brushes are superhydrophilic,
while the hydrophobicity increases with increasing the thickness
due to the strong inter- and intrachain associations.37
XPS broad survey spectra for the initiator-modied silicon
wafers and both pSBVI and pSBMA polymer brush samples are
Fig. 2 Tapping-mode AFM images in air (0.5 mm  0.5 mm): (a) bare
presented (Fig. 1). The surface initiator was successfully immo- silicon wafers (Ra ¼ 0.23 nm), (b) initiator-modified silicon wafers (Ra ¼
bilized on silicon wafers and glass substrates, as conrmed by 0.54 nm), (c) pSBMA-SH (Ra ¼ 0.27 nm), (d) pSBMA-H (Ra ¼ 0.45 nm),
the detection of the characteristic XPS signals for N1s (BE ¼ 402.0 (e) pSBVI-SH (Ra ¼ 0.66 nm), and (f) pSBVI-H (Ra ¼ 1.4 nm) polymer
eV) and Br3d (BE ¼ 70.0 eV), as shown in Fig. 1a. It is worth noting brushes grafted on silicon wafers.
that the bromine signal detected on the initiator surface was
weaker than that of the nitrogen signal (0.12% of Br vs. 2.41% of other researchers and was attributed to the instability of C–Br
N) and this does not match their 1 : 1 stoichiometric ratio in the bonds under X-ray irradiation.29,39 Anywise, high resolution XPS
initiator. This discrepancy was also observed by Liu et al. and prole of Br3d is shown in Fig. 1b, which demonstrates successful

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Fig. 3Digital photos of different samples: (a) bare glass, (b) pSBMA-SH, (c) pSBMA-H, (d) pSBVI-SH, and (e) pSBVI-H after exposure to hot water
vapour for 15 s under ambient lab conditions (temperature 21  C, 88% relative humidity).

immobilization of the initiator on the substrates. XPS spectra of
pSBMA and pSBVI show an increase in the intensities of S2p and
N1s for both pSBMA and pSBVI compared to initiator-graed
substrates (Fig. 1a); however, a weak Si signal originating from
the underlying initiator and/or substrates was observed. High-
resolution scans for both N1s and S2p (BE ¼ 167.0 eV) are also
shown (Fig. 1c and d). The ratios between N and S were 0.9 and
2.3 for pSBMA and pSBVI, respectively, which are accordingly
approximate to their stoichiometric ratios of 1 and 2 (Table 1).
The surface morphology of the samples was measured by AFM
(Fig. 2) and the corresponding roughness values are shown in
Table 1. The surface morphology of silicon wafers was at and
smooth with a low roughness value of 0.23 nm (Fig. 2a). Aer the
initiator was immobilized on the substrates, the roughness
increased to 0.54 nm (Fig. 2b). The surface roughness values were
0.27 and 0.45 nm for pSBMA-SH and pSBMA-H (Fig. 2c and d),
respectively, and the roughness values were 0.66 and 1.4 nm for
pSBVI-SH and pSBVI-H (Fig. 2e and f), respectively. The data
suggest that the surface roughness of the polymers graed onto
the substrate surfaces increases proportionally with the
thickness.
Anti-fog performance
The primary factor to determine the ability of a surface to
prevent fog formation is the equilibrium of a droplet in contact
with a surface as described by the Young's equation.40
Furthermore, it has been proved that the anti-fog property of
a surface is governed by its hydrophilicity where very hydro-
philic surfaces can maintain good optical transmission.41 In
this regard, pSBMA and pSBVI graed glass substrates were

Fig. 4 Light transmission at the normal incident angle for various samples (a) before, (b) after 15 s, (c) after 30 s and (d) after 60 s exposure to hot
water vapour (5 cm above 80  C water bath) under ambient conditions (temperature 21  C, 88% relative humidity).

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Fig. 5 Digital photos of different samples: (a) bare glass, (b) pSBMA-SH, (c) pSBMA-H, (d) pSBVI-SH, and (e) pSBVI-H, after storage in a freezer at

20  C for 30 min (upper) and 24 h (bottom), taken immediately after transfer to ambient lab conditions (temperature 21  C, 88% relative
humidity).
Fig. 6 Light transmission at the normal incident angle for various
samples after: (a) 30 min, and (b) 24 h storage in a freezer at
20  C,
immediately after transfer to ambient lab conditions (temperature 21

C, 88% relative humidity).
placed above hot water vapour for different time periods and
digital images were taken immediately aer transfer to ambient
lab conditions. The unmodied glass was severely fogged aer
15 s exposure to hot water vapour (Fig. 3a), so did both pSBMA-
H and pSBVI-H graed glasses (Fig. 3c and e). On the contrary,
no fog formation was observed at all for pSBMA-SH and pSBVI-
SH samples (Fig. 3b and d). Exposure to hot water vapour for
longer periods (i.e. 30 s and 60 s) further exhibited similar
performance, which indicated that pSBMA-SH and pSBVI-SH
could maintain good anti-fog property over long-term test
61700 | RSC Adv., 2016, 6, 61695–61702
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(Fig. S4 in ESI†). When the exposure time increased for pSBMA-
H and pSBVI-H, the absorption capacity of water increased and
consequently led to the formation of free water domains on the
surfaces resulting in more fogging occurrence.
UV-vis spectrophotometer was used to quantitatively assess
the anti-fog performance. According to the ASTM procedure F
659-06,19 a coating is dened to be anti-fog if it can maintain
a light transmittance over 80% aer exposure to hot water
vapour for 30 s. The light transmittance values of bare glass
and the graed polymer brushes are comparable (91–92%,
Fig. 4a) before the fogging and frosting tests. In a different
manner, when the samples were exposed to hot water vapour
for 15, 30, and 60 s (Fig. 4b–d), low light transmittance was
observed for unmodied glass (<56%), but all of the graed
polymer brushes maintained very high transparency (>87%).
The nding conrms that both hydrophilic and super-
hydrophilic brush coatings can retain an optically clear
surfaces, even though the condensation of water virtually
occurs during hot fogging test.
Anti-frost performance
The frost forms when the temperature of a substrate falls below
its dew point, where water vapour can evade the liquid phase
and transform directly into ice.5,10 In this work, the samples
were stored in a freezer at
20  C for 30 min and 24 h to study
the frost-resistance. Digital images were taken immediately
aer the samples were removed from the freezer (Fig. 5). The
bare glass lost its transparency completely (Fig. 5a), because of
severe frosting formation, which turned into fog aer exposure
to ambient lab conditions due to the thermal gradient.42 Also,
pSBMA-H and pSBVI-H brushes (Fig. 5c and e) showed similar
behaviour to that of bare glass due to frost nucleation on the
substrates. On the contrary, neither frost nor fog was formed on
pSBMA-SH and pSBVI-SH brushes which attained very high
transparency throughout the test even aer 24 h storage at
20

C (Fig. 5b and d). This conrms the excellent anti-fog and frost-
resistance of the superhydrophilic brushes.
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Table 2 Summary of anti-fog and anti-frost performance of various
samples under different conditions
Sample Anti-fog Anti-frost
Bare glass No No
pSBMA-SH Yes Yes
pSBMA-H No No
pSBVI-SH Yes Yes
pSBVI-H No No
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Additionally, UV-vis spectroscopy was used to monitor the
transmittance soon aer removing the samples from the freezer
aer being stored at
20  C for 30 min (Fig. 6a) and 24 h (Fig. 6b).
It is obvious that the optical transmittance of bare glass was
signicantly reduced to less than 15% owing to severe frosting on
surfaces. Furthermore, there was a decrease in the transmittance
of hydrophilic brushes (<50% for pSBVI-H and 30% for pSBMA-
H), due to the condensation of water on the brush surfaces.
The lower transmittance of hydrophilic coatings compared to
superhydrophilic coatings can be likely due to surface wetting
property and surface roughness. The roughness values of pSBMA-
H and pSBVI-H coatings are higher than that of pSBMA-SH and
pSBVI-SH brushes; therefore, frost can nucleate on the former
brush surfaces more easily. Jung et al. found that hydrophilic
surfaces with a minimal roughness, 1.4–6.0 nm, have the longest
freezing delay times when compared to rougher surfaces.43
On the other hand, the transmittance values of super-
hydrophilic coatings were as high as that before fogging and
frosting tests. These results can emphasize the role of the surface
wetting properties on the coalescence of adsorbed water and ice
nucleation. A comparison of the anti-fog and anti-frost results for
both hydrophilic and superhydrophilic polymer brushes is
summarized in Table 2 as compared with bare glass samples.
Conclusions
The SI-ATRP method was used to prepare hydrophilic and
superhydrophilic zwitterionic pSBMA and pSBVI brushes by
precisely controlling the thicknesses of the polymer thin lms.
Only superhydrophilic polymer brushes could attain an excellent
anti-fog and anti-frost properties even under an aggressive fogging
and frosting conditions. However, hydrophilic brushes could not
afford a good capability to resist the formation of fog and frost.
Here we could nd that the main factor that affects the ability of
pSBMA and pSBVI to prevent the fog formation and frost nucle-
ation is the wettability of the coatings rather than the chemical
structures. Importantly, the relation between the structure and
the property of sulfobetaine polymers was determined using water
molecules at different phases and under various conditions. This
will certainly drive further studies towards the fabrication of
decorated surfaces with novel properties and applications.
Acknowledgements
The authors acknowledge the Ministry of Science and Tech-
nology (MOST 104-2221-E-008-108 and 104-2119-M-194-004) for
nancial support of this project.
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