RESEARCH ARTICLE

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Facile Approach for Designing Icephobic Coatings Using

Polymers/Silica Nanoparticle Composites via Self-Formation
of Superhydrophobic Surfaces
Aravind H. Patil, Ngoc Le Trinh, Hackwon Do, Houda Gaiji, Youngho Kang, Joohan Lee,
Changhyun Chung,* and Han-Bo-Ram Lee*

negatively affect the efficiency of various

Ice accumulation and proliferation adversely affect the activities of various domestic and industrial applications,
residential, commercial, and polar research stations. Although significant including power transmission cables,
efforts are devoted to preventing ice adhesion to various surfaces by wind turbines, telecommunication
developing various anti-icing coatings, it is still necessary to enhance overall equipment, offshore platforms, solar
panels, and other infrastructure, thereby
performance and durability. Herein, a facile approach is proposed for leading to socioeconomic and safety
fabricating an icephobic coating on an aluminum 6061 (Al) substrate, by issues.[2–4] Anti-icing and de-icing tech-
coating a poly(dimethylsiloxane) (PDMS)/ poly(tetrafluoroethylene) (PTFE) niques are primarily classified into two
composite through a spin-coating method, followed by sprinkling of SiO2 categories: active and passive, which are
nanoparticles (NPs). Crosslinker/binder-free adhesion between PDMS and distinguished based on the use of an
external force.[1] Various conventional
PTFE is achieved by utilizing secondary-induced electrostatic dipole-dipole
active anti-icing methods for combat-
interactions, these interactions are supported by density functional theory ing icing issues include mechanical
(DFT) calculations as well as structural studies. Moreover, the controlled scrapping of ice, infrared thermal treat-
addition of PTFE powder to PDMS improves the water-repellency, mechanical ments, chemical treatments, and the
strength, and surface roughness of the coating. The self-formation of the use of antifreeze solutions and salts.[5]
superhydrophobic state of the PDMS/PTFE composite is achieved by However, these methods are ineffective,
time-consuming, energy-consuming,
sprinkling SiO2 NPs. The sprinkled SiO2 NPs are protected by the expensive, and harmful to the environ-
PDMS/PTFE composite, which serves as a stress concentrator to achieve low ment. Thus, over the last five decades,
ice adhesion. Furthermore, freezing at low temperatures can be delayed by substantial research efforts have been
controlling the heat flow rate, interfacial contact area, and surface texture. devoted to the design of durable passive
This indicates the feasibility of the proposed method for various promising icephobic surfaces.[6,7] Icephobicity can
be achieved in several ways, such as by
anti-icing applications.
lowering the ice adhesion strength (IAS,
𝜏ice), minimizing the interfacial contact
area between supercooled water/ice with
1. Introduction coating, delaying the ice nucleation, reducing the rate of heat
transfer at solid/liquid interface, and preventing the transition
Ice formation and accretion are inevitable phenomena in ex- from the Cassie–Baxter (CB) state to the Wenzel state.[8–11] Such
tremely cold environments.[1] Ice accumulation and proliferation passive icephobic coatings are expected to address long-term

A. H. Patil, N. L. Trinh, H. Gaiji, Y. Kang, H.-B.-R. Lee A. H. Patil, J. Lee, C. Chung

Department of Materials Science and Engineering Center of Technology Development
Incheon National University Korea Polar Research Institute
Incheon 22012, Republic of Korea Incheon 21990, Republic of Korea
E-mail: hbrlee@inu.ac.kr E-mail: ch.chung@kopri.re.kr
H. Do
Division of Life Sciences
The ORCID identification number(s) for the author(s) of this article Korea Polar Research Institute
can be found under https://doi.org/10.1002/admi.202300919 Incheon 21990, Republic of Korea
© 2024 The Authors. Advanced Materials Interfaces published by
Wiley-VCH GmbH. This is an open access article under the terms of the
Creative Commons Attribution License, which permits use, distribution
and reproduction in any medium, provided the original work is properly
cited.
DOI: 10.1002/admi.202300919

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issues with undesired ice formation by allowing ice to be re-
moved by simple perturbations of natural forces such as gravity
and wind.[12]
To date, various research groups have used poly(dimethy-
lsiloxane) (PDMS) to develop passive low ice adhesion
coatings[13–16] because of its tunable mouldability, hydropho-
bicity, low surface energy (19–21 mN m−1 ),[17] and viscoelastic
nature.[13] These exceptional properties of PDMS render it
a promising material for applications in the fields of super-
hydrophobicity and icephobicity. However, PDMS has low
mechanical strength, which restricts the ice prevention from its
coating to considerably fewer icing and de-icing cycles.[18] To
overcome this issue, it is necessary to improve the mechanical
strength of the coating without losing its softness and elastic
nature.[19] Soft elastic coatings produce deformation incompati-
bility at the ice/coating interface owing to the mismatch of the
elastic moduli, which promotes easy detachment of ice from the
coating surface.[20] In addition, the mechanical strength of the
coating is a crucial factor for maintaining the superhydrophobic
CB state for several icing and de-icing cycles under prolonged
exposure to extremely low temperatures and harsh conditions.
In the literature, there are reports on the integration
of polymers such as poly(vinylidene fluoride) (PVDF),[21]
poly(tetrafluoroethylene) (PTFE),[22] and polyhedral oligomeric
silsesquioxane (POSS)[23] into PDMS, which improved the me-
chanical strength and superhydrophobicity/icephobicity of the
coatings. Moreover, the covalent bonding strategy has also been
implemented to improve the mechanical robustness of the super-
hydrophobic state. Particularly, the hydrolyzed glycidoxypropy-
ltrimethoxysilane was used as a connecting layer for coating the
hexamethyldisilazane-modified SiO2 NPs on a hydrophilic Al
substrate.[24] Among them, PTFE is the best fluoropolymer with
high mechanical strength, low surface energy (18 mN m−1 ),[25]
hydrophobic nature, and low frictional coefficient.[26] Addition-
ally, PTFE (Teflon) is widely used in the non-stick cookware
industry.[27] Owing to its unique characteristics, PTFE is an
excellent candidate for lowering ice adhesion, improving me-
chanical strength, and maintaining the thermal stability of coat-
ings at extremely low temperatures. Various approaches, includ-
ing RF-sputtering,[28] plasma treatment,[29] and chemical vapor
deposition,[30] have been employed to prepare PDMS/PTFE com-
posites. However, these techniques are expensive and unfeasible
for large-scale applications.
In our previous work, we successfully developed simple
methods for preparing superhydrophobic and icephobic coat-
ings by sprinkling micron-sized SiO2 particles onto PDMS and
PDMS/PVDF surfaces.[21,31] These studies demonstrated that the
sprinkling of SiO2 particles was responsible for the creation of
micro-nanoscale surface roughness. Moreover, self-formation of
superhydrophobic surfaces was achieved through interfacial en-
ergy engineering between the PDMS solution and SiO2 parti-
cles. Coatings with smaller particle sizes exhibited higher sur-
face roughness and lower corresponding IAS. However, because
we used micro-sized SiO2 particles, which produced only limited
surface roughness, we could not further reduce the IAS. Particu-
larly, the PDMS/PVDF/SiO2 composite coating with 1.3 μm size
of SiO2 particles showed an IAS of 46 kPa at −35 °C and 55% hu-
midity. The integration of PVDF into PDMS resulted in improved
hydrophobicity and mechanical strength of the coating.[21] The
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presence of the fluorinated ligand (─CF2 ) within PVDF signif-
icantly contributed to the reduction in IAS. However, aiming to
reduce the surface energy of the coating further and enhance me-
chanical strength, we have chosen PTFE, which is recognized as a
superior fluoropolymer compared to PVDF. PTFE exhibits excep-
tional properties, such as excellent hydrophobicity, low surface
energy, and robust mechanical strength derived from its unique
molecular structure composed solely of ─CF2 ligands.[26,27] Thus,
to address limitations regarding surface roughness improvement
and surface energy reduction, we introduced SiO2 NPs along with
PTFE. Subsequently, PDMS/PTFE/SiO2 NPs composite coatings
were prepared and investigated to assess the effect of SiO2 NP
sizes on superhydrophobicity, freezing delay time, and icepho-
bicity (Table 1).
In this study, a simple method is developed to prepare su-
perhydrophobic/icephobic coatings on Al substrate by coating
PDMS/PTFE composite through the spin-coating method, fol-
lowed by sprinkling of SiO2 NPs on it. A controlled amount
of PTFE powder was added to the viscous PDMS to lower the
surface energy, improve mechanical strength, and maintain the
viscoelasticity of the coating. Additionally, we demonstrated ex-
perimentally and theoretically that the electrostatically driven
induced dipole-dipole interactions between the H atoms (pos-
itively charged) of PDMS and F atoms (negatively charged) of
PTFE were responsible for the binder-free adhesion in PDMS
and PTFE. Surface morphology analysis revealed that the for-
mation of porous 3D micro-nanostructured surfaces of the
PDMS/PTFE/SiO2 NPs composite were highly textured surfaces
with several trapped air voids. These air voids minimized the sur-
face contact area with water droplets or ice, thereby improving
the water contact angle (WCA) and reducing the IAS. Moreover,
the relationship between IAS and surface wettability was inves-
tigated for various coating surfaces. Furthermore, we provide ex-
perimental insights into the ice freezing delay time (FDT) for var-
ious surface wettabilities.
2. Results and Discussion
2.1. Density Functional Theory Calculations and Structural
Analyses
The impact of the relative orientation of the PDMS and PTFE
polymeric chains on the adhesive and mixing properties was ex-
amined using DFT calculations. Different possible orientations
of the polymeric chains were used to compute the interaction en-
ergies between
PDMS and PTFE. The interaction energy was calculated using
Equation (1).
( )
Einteraction = EPTFE+PDMS − EPDMS + EPTFE (1)
As shown in Figure 1a, DFT calculations illustrate that the in-
teraction energy mainly depends on the relative orientation of the
PDMS and PTFE chains. The oriented geometry with the highest
possibility of interactions between the F and H atoms exhibited
the lowest physisorption energy of −0.5 eV (configurations #2
and #5). This phenomenon is attributed to the positive charge
of the H atom and the negative charge of the F atom. However,
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Table 1. Comparison of present work with relevant previous reports.

Coating Synthesis technique Temperature WCA [°] IAS [kPa] Reference

[°C]

PDMS/PTFE/SiO2 NPs Self-formation of porous 3D −15 ± 1 163.9 ± 0.2 27 ± 3 Present work

micro-nanostructure by sprinkling SiO2 NPs
on PDMS/PTFE surface
PDMS/PVDF/SiO2 microparticles Self-formation of superhydrophobic surface by −35 161 ± 0.5 46 [21]
sprinkling micron-sized SiO2 on the
PDMS/PVDF
Porous PDMS Curing and phase separation method −18 120.3 40 [32]
Carbon nanowire/PDMS composite Laser etching −10 155.4 ± 0.5 39.55 [33]
Carbon nanotube/PDMS composite Shear dispersion and ambient curing −10 ± 2.6 160.7 ± 1.5 38.4 [34]
1H,1H,2H,2H-heptadecafluorodecyl)- Acid etching and thermal treatment −20.5 170.5 ± 1 25.3 [35]
trimethoxysilane and PDMS

when F and O atoms face each other, the interaction energy be-
tween PDMS and PTFE is observed slightly higher (−0.2 eV; con-
figurations #4 and #6). This is because F and O atoms are neg-
atively charged. Moreover, the electron density isosurface is col-
ored based on electrostatic potentials, with an isosurface level of
Figure 1. Results of DFT calculations a) Interaction energies (in eV) for six
possible configurations, and b) the interaction between PDMS and PTFE
polymeric chains and their electron-density isosurfaces colored according
to electrostatic potentials, with an isosurface level of 0.025a0 −3 .
0.025a0 −3 , shown in Figure 1b. Specifically, for configuration #5,
the electrostatic potential ranges from −10.81 Ry (blue) to +1.97
Ry (red). The electrostatic potentials around the H atoms in both
polymeric chains are relatively low; the color is close to green, in-
dicating hydrogen is positively charged. Whereas, those around
the F and O sites are higher; the color is close to red, indicating
they are negatively charged. Overall, DFT calculations reveal that
PDMS and PTFE polymeric molecules are attracted to each other
via induced dipole-dipole electrostatic interactions between F and
H atoms.[36]
The microstructure and chemical composition of the
PDMS/PTFE composite were analyzed using X-ray diffrac-
tion (XRD), Fourier-transform infrared (FTIR) spectroscopy,
and X-ray photoelectron spectroscopy (XPS). Figure 2a shows
the XRD patterns of PDMS, PTFE, and the PDMS/PTFE com-
posite. In the XRD pattern of bare PDMS, the presence of a
low-intensity wide single peak at 11.77° confirms the formation
of amorphous PDMS.[37] In the XRD pattern of the bare PTFE,
the diffraction peaks at 18.03°, 31.50°, and 36.59° correspond to
the (100), (110), and (107) crystal planes of the hexagonal crystal
structure of PTFE, respectively.[37] Moreover, in the XRD pattern
of the PDMS/PTFE composite, the amorphous peak of PDMS
is present at 11.77°; other diffraction peaks of PTFE are also
present. The XRD results are well consistent with previously
published reports.[37,38]
Figure 2b shows the FTIR spectra of PDMS, PTFE, and the
PDMS/PTFE composite. The peaks located at 867 and 914 cm−1
correspond to the asymmetric rocking of the ─CH3 groups of
PDMS. The peaks at 1008 and 1255 cm−1 are assigned to silox-
ane backbone Si-O-Si asymmetrical stretching vibrations and
bending vibrations of the CH3 groups of PDMS. Importantly, in
the FTIR spectra of the PDMS/PTFE composite, the absorption
peaks at 1208 and 1160 cm−1 correspond to the ─CF2 bond of
PTFE.[36] In PDMS/PTFE composite spectra, the peaks at 2160
and 2962 cm−1 are attributed to the C─H asymmetric and CH3
asymmetric stretch respectively, which are assigned to PDMS.[36]
The FTIR and DFT results demonstrate that no primary bonds
are formed between PDMS and PTFE, indicating that the com-
posite is formed owing to secondary interactions between them.
Furthermore, XPS analysis was performed to obtain informa-
tion on the chemical valence states and corresponding binding
energies (BEs) of PDMS, PTFE, and the PDMS/PTFE composite.

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Figure 2. a) XRD, b) FTIR, c) XPS survey spectra of PDMS, PTFE, and PDMS/PTFE composite d) C1s spectra e) F1s spectra of PTFE and PDMS/PTFE
composite, and f) schematic for secondary interaction between PDMS and PTFE.

As shown in Figure 2c, the survey spectrum of the PDMS/PTFE
composite confirms the presence of Si2p, Si2s, C1s, O1s, and
F1s characteristic peaks corresponding to the BEs of 98.31,
150.97, 281.38, 529.54, and 687.80 eV, respectively.[39] As shown
in Figure 2d, the core-level spectrum of C1s (PDMS/PTFE
composite) reflects two peaks at BEs of 282.22 and 290.27 eV,
corresponding to the Si─C bond of PDMS and ─CF2 bond of
PTFE, respectively.[40,41] The peak corresponding to the ─CF2
bond in the C1s spectrum of the PDMS/PTFE composite is
slightly shifted toward a lower BE of ≈0.58 eV, compared with
bare PTFE, as shown in Figure 2d. Additionally, in the high-
resolution F1s spectra of PTFE and the PDMS/PTFE composite,
the F1s peak is observed at 688.14 and 687 eV, respectively, as
shown in Figure 2e. The F1s peak of the PDMS/PTFE composite
is shifted toward the lower BE of 1.14 eV as compared to bare
PTFE. The BEs of the characteristic peaks of bare PDMS, bare
PTFE, and the PDMS/PTFE composite are summarized in Table
S1 (Supporting Information). In particular, shifts in the F1s and

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Figure 3. a) FESEM images of bare PDMS and 9:1 to 5:5 weight percent ratio of PDMS to PTFE, b) WCA and WSA, and c) RMS surface roughness and
ice adhesion strength.
C1s (─CF2 bond) spectra are observed because of the interaction
of the H atom of PDMS with the highly electronegative F atom
of PTFE.[36] These shifts in the BE positions of the characteristic
peaks suggest that the PTFE particles interact with the PDMS
chains through secondary interactions, which is consistent with
the DFT calculation results shown in Figure 2f.
2.2. PDMS/PTFE Composites
Figure 3a shows the surface morphology and elemental mapping
analysis of the bare PDMS and PDMS/PTFE coatings with vari-
ous weight percent ratios in the range of 9:1–5:5. The surface of
the bare PDMS coating is observed flat, uniform, and smooth, as
shown in Figure 3a.
As the weight percent ratio of PDMS to PTFE varied from 9:1
to 5:5, bright-contrast PTFE particles are observed in the field
emission scanning electron microscopy (FESEM) images. The
average particle size of bare PTFE particles determined using
FESEM analysis is ≈166 ± 3 nm (see Figure S1, Supporting In-
formation). The elemental mapping images revealed that bare
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PDMS contains C, O, and Si, whereas the PDMS/PTFE compos-
ite contains F from PTFE in addition to C, O, and Si (see Figure
S2a,b, Supporting Information). The weight percentage of F in
the composite coatings increased from 5.74% to 35.12% as the
weight ratio of PDMS to PTFE changed from 9:1 to 5:5. The FE-
SEM results showed good dispersion of the PTFE particles in the
PDMS chains, as expected from the DFT calculations and struc-
tural analysis results.
Figure 3b shows the WCA and water sliding angle (WSA) of the
bare PDMS and PDMS/PTFE composite coatings. The WCA and
WSA of the bare PDMS coating were 114.8 ± 0.7° and 23 ± 1°, re-
spectively. As the amount of PTFE increased in PDMS, the WCA
increased linearly from 114.8 ± 0.7° to 118.2 ± 0.5°. This sug-
gests that the addition of PTFE to PDMS results in a slight in-
crement in the hydrophobicity of the composite. However, no
significant change is observed in the WSA after the addition of
PTFE to PDMS. Figure 3c depicts the root mean square (RMS)
surface roughness and IAS of bare PDMS and PDMS/PTFE com-
posite coatings with various weight percent ratios (9:1–5:5). The
bare PDMS coating exhibited a considerably low surface RMS
roughness of 8.55 nm and IAS of 225 ± 3.6 kPa. The bare Al
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Figure 4. FESEM images of a) PDMS/SiO2 NPs, b) PDMS/PTFE/SiO2 NPs (8:2), and c) PDMS/PTFE/SiO2 NPs (6:4).
substrate exhibited the highest IAS of 614 ± 4 kPa because of
the high contact angle hysteresis, hydrophilic nature, and hard-
ness properties of the Al substrate (see Table S2, Supporting In-
formation). In contrast, the PDMS/PTFE (6:4) coating showed
IAS of 202 ± 3.6 kPa. The IAS of PDMS/PTFE (6:4) is reduced
by approximately three times compared to that of bare Al, likely
owing to the elastic nature,[42] hydrophobicity, and low surface
energy ─CF2 and ─CH3 ligands of the PDMS/PTFE composite.
The elastic nature of the coating promotes the easy detachment
of ice by creating deformation incompatibility at the coating and
ice interface.[13] Additionally, as the amount of PTFE in the com-
posite increased from 9:1 to 5:5 weight percent ratio, the corre-
sponding surface roughness increased gradually from 13.32 to
63.22 nm. The increase in surface roughness can be attributed to
the higher volume fraction of PTFE particles creating nanoscale
peaks and valleys at the coating surface.[43] This slight change in
surface roughness due to the addition of PTFE to PDMS also af-
fected the IAS. Moreover, the coating with a PDMS:PTFE weight
ratio of 5:5 exhibited superior properties, such as hydrophobic-
ity and IAS, compared to the other composites. However, as ob-
served in synthesis, after mixing a 5:5 weight percent ratio of
PDMS (viscous) to PTFE (solid), the viscosity of the resulting mix-
ture was highly increased. Owing to its high viscosity, it was not
appropriate to produce a uniform film by spin-coating.
2.3. Synthesis Mechanism and Surface Morphology
As described in the Introduction, we reported an easy process
for fabricating superhydrophobic and icephobic surfaces using
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microscale SiO2 powder, PDMS, and PDMS/PVDF composites.
Similar to our previous studies,[21,31] SiO2 NPs with various sizes
were added to the PDMS/PTFE composite samples at mixing
ratios of 8:2 and 6:4. Figure 4a–c shows the FESEM images of
PDMS, PDMS/PTFE (8:2), and PDMS/PTFE (6:4), respectively.
As shown in Figure 4a, the SiO2 NPs are perfectly covered by
PDMS of all sizes, and the morphological features of the NPs are
still observed on the surface. For both the PDMS/PTFE samples
as shown in Figure 4b,c, the SiO2 NPs are also covered by the
composite layer, but the surface roughness from the morpholog-
ical features is considerably higher than that of the PDMS sam-
ple.
Surface roughening was achieved by sprinkling SiO2 NPs
over the PDMS/PTFE composite surface, and the interactions
between them were theoretically calculated to understand the
self-formation mechanism. The interaction and self-formation
mechanism of the porous 3D micro-nanostructure of the
PDMS/PTFE/SiO2 NPs composite is described based on Stokes’
law and the Washburn equation. We assumed the interaction of a
single SiO2 particle with viscous PDMS. After the SiO2 NPs were
sprinkled onto the surface of the viscous PDMS, the SiO2 parti-
cles started to sediment because of their higher density. The sedi-
mentation velocity of a single SiO2 particle in viscous PDMS was
calculated using Stokes’ law of viscosity (Equation 2) as follows.
[ ]
𝜌s − 𝜌l
v = g D2 (2)
18𝜇
Where v is the terminal (sedimentation) velocity of SiO2 NPs in
m s−1 , 𝜌s and 𝜌l are the densities of SiO2 NPs (2.4 g cm−3 ) and
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PDMS (0.965 g cm−3 ), respectively, μ is the viscosity of PDMS
(3.5 Pa s), g is the acceleration due to gravity (9.8 m s−2 ), and
D is the diameter of SiO2 NPs in nm. The calculated sedimen-
tation velocities for SiO2 NPs with diameters of 65, 25, 15, and
10 nm were ≈0.94, 0.14, 0.05, and 0.022 pm s−1 , respectively.
Moreover, another interaction mechanism involves the drawing-
up of PDMS into the stacked SiO2 NPs due to the capillary imbi-
bition phenomenon. The capillary penetration length (L in μm) of
PDMS was calculated using Washburn’s Equation (3) as follows.
√ composite surface reduces the physical contact area with the wa-
𝛾rtCos𝜃
L = (3)
2𝜇
Where, 𝛾, r, t, μ, and 𝜃 are the surface tension of PDMS
(22.1 mJ m−2 ), average pore radius (nm), time (s), dynamic vis-
cosity (3.5 Pa s), and contact angle (0°) between the viscous PDMS
and the solid SiO2 NPs, respectively. After sprinkling SiO2 NPs
on the PDMS surface, the viscous PDMS immediately begins to
penetrate under capillarity action and drawing up to the stacked
SiO2 NPs. The calculated penetration lengths for SiO2 NPs with
diameters of 65, 25, 15, and 10 nm were ≈7.94, 5.62, 3.93, and
1.68 μm, respectively. The calculated sedimentation velocities and
penetration lengths are summarized in Table S3 (Supporting In-
formation). Overall, from comparing the calculated sedimenta-
tion velocity and penetration length values for PDMS and SiO2
NP systems, the capillary imbibition dominates the sedimenta-
tion velocity. The SiO2 NPs attain considerably low sedimentation
velocity in the order of 10−12 m s−1 ; however, the excellent dis-
persion of PDMS and SiO2 was observed. This is because of the
excellent wetting nature of PDMS and the larger specific surface
area (130–600 m2 g−1 ) of smaller spherical SiO2 NPs.[44] There-
fore, it is clearly seen that SiO2 NPs of all sizes are completely
covered by PDMS and the SiO2 particles are seen underneath the
PDMS, as shown in Figure 4a.
In the case of the PDMS/PTFE composite, owing to the pres-
ence of solid PTFE, the viscosity of the mixture increases com-
pared to that of bare PDMS. Therefore, the viscosity of the
PDMS/PTFE mixture exerts an upthrust force on the SiO2 NPs,
which affects their sinking rate. For 65 nm SiO2 NPs, the calcu-
lated sedimentation velocity is in the order of 10−12 m s−1 and the
penetration length L is 7.94 μm (for t = 1 s). This suggests that the
sinking velocity is negligible compared with the penetration rate.
Therefore, capillary imbibition dominates over sedimentation for
all particle sizes. Consequently, viscous PDMS quickly covers the
SiO2 NPs. Additionally, it could be possible that the secondary-
induced electrostatic interactions between the PDMS and PTFE
particles cause the PDMS chains to pull the PTFE particles.[36]
Hence, the SiO2 NPs are confined within the PDMS/PTFE com-
posite. Thus, capillary imbibition is the driving force responsible
for the self-formation of the porous 3D micro-nanostructure of
the PDMS/PTFE/SiO2 NP composite, as shown in Figure 4b,c.
Furthermore, a similar but compact formation of porous 3D
micro-nanostructures is observed for the 6:4 weight ratio, as
shown in Figure 4c. Additionally, the superhydrophobic nature of
PDMS/PTFE/SiO2 NPs coatings is discussed as follows: the main
reason for the superhydrophobic nature lies in the synergistic
effects aroused by the porous 3D micro-nanostructured surface
morphology coupled with low surface energy properties of ─CH3
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and ─CF2 ligands within the PDMS/PTFE composite.[21] As de-
scribed in the mechanism of self-formation superhydrophobic
surface, the sprinkling of SiO2 NPs is mainly responsible for
creating a porous 3D micro-nanostructured surface. Owing to
the sprinkling of SiO2 NPs over viscous PDMS/PTFE composite,
the surface morphology significantly altered from flat to rough
(Figures 3 and 4). This significant change in the surface rough-
ness is attributed to the creation of interconnected peaks and val-
leys within the interface of the PDMS/PTFE/SiO2 NPs composite
(Figure 4c). The presence of several trapped air voids within the
ter droplet. Overall, this formation of a rough surface, coupled
with the low surface energy PDMS/PTFE, leading to the com-
posite surface with a high WCA and low contact angle hysteresis,
facilitates the easy roll-off capabilities to water droplets.
2.4. Surface Wettability and Ice Adhesion Strength
Measurements
Figure 5a depicts the WCA analysis of the 10, 15, 25, and 65 nm
sizes of SiO2 NPs sprinkled on PDMS and the PDMS/PTFE com-
posites. The PDMS/SiO2 NP coatings exhibited the WCA greater
than 150° for all the sizes of SiO2 NPs. The WCA was increased
slightly for the PDMS/PTFE/SiO2 (8:2) samples compared to the
PDMS/SiO2 samples. The coatings with a 6:4 weight ratio ex-
hibited the highest WCA of 153.6°, 159.3°, 163.9 ± 0.2°, and
156.9 ± 0.6° for 10, 15, 25, and 65 nm SiO2 NPs, respectively.
Additionally, the WSA of the PDMS/PTFE/SiO2 NP (6:4) coating
was reduced by approximately twofold compared to that of the
PDMS/SiO2 NPs (Figure 5b). Overall, the results imply that by
increasing the amount of PTFE in PDMS, the coatings exhibited
an increase in WCA and a decrease in WSA. As the volume frac-
tion of PTFE in PDMS increases, the quantity of ─CF2 ligands
from PTFE on the surface also increases. PTFE is a widely rec-
ognized polymer with exceptional hydrophobicity and extremely
low surface energy, which is attributed to the presence of ─CF2
ligands and its non-polar nature.[26] When the interaction of wa-
ter molecules occurs at the coating interface, these low surface
energy ─CF2 ligands which have a surface energy of 18 mJ m−2
create a large interfacial energy difference with water molecules
(water-air interfacial energy 𝛾 wa = 72.8 mJ m−2 ).[6] Thus, a signif-
icant energy difference is generated at the coating-water interface
owing to the PTFE particles, which facilitates an increase in the
WCA and easy roll-off of the water droplet capabilities of coating.
As shown in Figure 5a, the WCA was increased gradually
as the size of SiO2 NPs increased from 10 to 25 nm; however,
above 25 nm, the WCA decreased. Particularly, the coatings with
10 nm SiO2 NPs exhibited lower WCA and higher WSA than
those with other sizes. This is due to the 10 nm size of SiO2
NPs sprinkled over PDMS and PDMS/PTFE composite surfaces,
created comparatively more closely packed and flatter micro-
nanostructured surfaces owing to their smaller size and larger
surface area, as shown in Figure 4. However, the WCA was de-
creased for the 65 nm size of SiO2 NPs. This is likely due to the
change in surface roughness over a specific size range of the SiO2
NPs. As shown in Figure 4, for 65 nm particles, the surface rough-
ness is slightly reduced compared to that of the 25 nm samples.
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Figure 5. a) WCA, b) WSA, c) ice adhesion strength of PDMS/SiO2 NPs, PDMS/PTFE/SiO2 NPs (8:2), and PDMS/PTFE/SiO2 NPs (6:4) coatings, and
d) Schematic of the interaction of minimized contact area of a frozen water droplet on superhydrophobic surface.
Figure 5c shows the IAS analysis of PDMS and PDMS/PTFE
composites integrated with 10, 15, 25, and 65 nm SiO2 NPs.
The PDMS/SiO2 NPs coatings exhibited IAS of 101 ± 5, 76 ± 5,
60 ± 5, and 87 ± 5 kPa for 10, 15, 25, and 65 nm sprinkled
NPs, respectively. However, the IAS was reduced slightly for
PDMS/PTFE/SiO2 (8:2) coatings, as compared to PDMS/SiO2
NPs coatings. In comparison, the PDMS/PTFE/SiO2 (6:4) coat-
ings exhibited the lowest IAS of 38 ± 2, 31 ± 7, 27 ± 3, and
29 ± 2 kPa for 10, 15, 25, and 65 nm SiO2 NPs, respectively.
From Figure 5c, it is evident that increasing the amount of
PTFE in PDMS leads to a decrease in IAS. This is because of
the increased volume fraction of PTFE particles in PDMS, re-
sulting in more ─CF2 ligands on the coating surface. The ─CF2
ligands from PTFE exhibit excellent characteristics, such as hy-
drophobicity, low surface energy, low frictional coefficient, and
non-polar nature, which facilitate low interfacial shearing stress
at the coating/ice interface.[26] Additionally, when freezing initi-
ates, the interaction between ─CF2 ligand with the surface en-
ergy of 18 mJ m−2 and ice with the interfacial energy of 𝛾 ia ≅
75 mJ m−2 occurs at the coating interface, resulting in a signif-
icant interfacial energy difference at the coating/ice interface.[6]
Thus, the increased volume fraction of PTFE in PDMS generates
a significant energy difference at the coating/ice interface, which
promotes the easy detachment of ice from the 6:4 weight ratio’s
coating surface.
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Furthermore, as shown in Figure 5c, the IAS of the coatings
varied with the particle size of the SiO2 NPs; the IAS reduced
as the particle size increased from 10 to 25 nm but increased
slightly to 65 nm. This is primarily due to changes in the surface
morphology, effectiveness in the formation of interconnected air
voids, and the contact area between the coating surface and ice at
the interface with variations in particle sizes of SiO2 NPs. Specif-
ically, the 10 nm size of SiO2 NPs exhibited the highest IAS in
comparison with the other particle sizes. The 10 nm size of SiO2
NPs created more compact, densely packed, and flatter surfaces,
as shown in Figure 4, owing to their smaller particle size and
larger surface area. Such compact surface microstructures failed
to create effective air voids on the coating surface, resulting in
an increase in the contact area with ice. Hence, the coatings with
10 nm particle size exhibited relatively higher IAS. The 25 nm
particle size produced a more porous 3D micro-nanostructured
rough surface with highly effective air voids, resulting in a greater
reduction in the contact area compared with the 10 nm particles,
as shown in Figure 5d. The particle sizes of 10, 15, 25, and 65 nm
with coating layers have occupied the contact areas with 10 μL wa-
ter droplets of ≈0.23, 0.15, 0.1, and 0.18 mm2 , respectively (see
Table S4, Supporting Information). The PDMS/PTFE/SiO2 (6:4)
coatings exhibited the IAS of 38 ± 2, 31 ± 7, 27 ± 3, and 29 ± 2 kPa
for 10, 15, 25, and 65 nm SiO2 NPs, respectively. The contact areas
at the interface between the water and coating, calculated from
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the volume of water droplet, WCA, and surface roughness, are
consistent with the IAS results. From Figure 5a–c, a consistent
correlation is observed between the IAS measured at low tem-
peratures and the surface wettability analysis performed at room
temperature for parameters, such as the WCA and WSA.[45]
Overall, after sprinkling SiO2 NPs of various sizes over
PDMS and the PDMS/PTFE composite, the surface topogra-
phy significantly changed from flat to rougher and more porous
3D micro-nanotextures. Thus, for the superhydrophobic sur-
faces, the contact area between the coating surface and the wa-
ter droplet is significantly reduced compared to that for the
PDMS and PDMS/PTFE hydrophobic flat/smooth surfaces (see
Table S4, Supporting Information). Additionally, from the high-
magnification inset images shown in Figure 4a–c, the forma-
tion of interconnected peaks and valleys in the porous 3D micro-
nanostructures is observed. The peaks are attributed to the SiO2
NPs confined in the PDMS/PTFE composite, which serves as a
stress concentrator. When a water droplet freezes on a superhy-
drophobic CB surface, it exerts an adhesive force on its peaks. As
illustrated in Figure 5d the schematic of a frozen water droplet
interacting with the peaks of an elastic superhydrophobic sur-
face. Therefore, most of the adhesive force (stress) of the ice is
concentrated on the peaks of PDMS/PTFE/SiO2 . The peaks bear
most of the stress and induce deformation incompatibility as well
as the presence of air voids, which reduce the surface contact
area with water droplets or ice.[20,46] Thus, such porous 3D micro-
nanostructured morphologies are favorable for minimizing the
contact area of water/ice with the coating surface, which facili-
tates an overall reduction in the ice shearing stress.
2.5. Freezing Delay Time
FDT experiments were performed to investigate the freezing de-
lay performance of water droplets for various surface wettabilities
and material compositions. Figure 6 shows the photographs of
the phase transition of water to ice at −15°C with respect to time.
Photographs of different stages of water droplets until freezing
and producing a sharp spike shape on the top of the ice and
the WCA at room temperature are compared. In ice FDT mea-
surements, it is necessary to consider the differences between
real freezing and experimental FDT analysis conditions. The sur-
rounding temperature is an important factor that can affect the
ice growth and freezing time. Thus, it is important to consider
Equation (4),[47] which relates the effect of the temperature dif-
ference between the surrounding and freezing temperatures on
the ice growth.
ΔT T f − Ta
V̇ ∝ Q̇ ∝ = (4)
R R
Where V, ̇ Q,
̇ and R are the volumetric growth of ice, heat flux,
and thermal resistance at the ice front, respectively. Moreover,
∆T = Tf – Ta , ∆T is the difference between the freezing tem-
perature (Tf ) and the surrounding temperature (Ta ). During
FDT analysis for all the samples, ∆T maintained remains con-
stant. If ∆T is constant, then the FDT of ice mainly depends
on thermal resistance (R). As, V̇ is inversely proportional to R;
therefore, a surface with a lower thermal resistance provides a
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higher release rate of latent heat (good thermal conductivity, e.g.,
bare Al), leading to a rapid freezing rate, and vice versa (e.g.,
PDMS/PTFE/SiO2 superhydrophobic surfaces).
As shown in Figure 6, the FDT for bare Al, PDMS,
and PDMS/PTFE (6:4) composite were recorded ≈28 ± 4.16,
93.5 ± 5.67, and 108 ± 3 s, respectively. Bare Al substrate is
a metal with excellent thermal conductivity of 167 W mK−1 ,[48]
hydrophilic nature, and high surface energy. Hence, the water
droplet on the Al surface freezes within a very short span, and
the freezing rate is rapid. Although the PDMS and PDMS/PTFE
composite coatings are hydrophobic in nature, the PDMS/PTFE
composite exhibited a slightly higher FDT than PDMS. This can
be attributed to the slight change in the contact area and the
reduction in the heat transfer rate of the water droplet on the
PDMS/PTFE composite surface. The graphical representation
of FDT versus WCA for distinct thermal conductivities is illus-
trated in Figure S7 (Supporting Information). On the other hand,
for superhydrophobic surfaces, the FDT values of 357 ± 8.83,
452 ± 7.12, 441.32 ± 12, and 404 ± 4.24 s were recorded for SiO2
particles with sizes of 10, 15, 25, and 65 nm, respectively.
As shown in Figure 6, the FDT for 10 μL water droplets
on different surfaces follows the order of PDMS/PTFE/SiO2 >
PDMS/PTFE > PDMS > Al. The bare Al, PDMS, and PTFE
have thermal conductivities of 167, 0.16, and 0.25 W mK−1 ,
respectively.[48–50] The calculated contact areas for bare Al,
PDMS, and PDMS/PTFE (6:4) composite are ≈15.43, 5.45, and
5.19 mm2 , respectively (see Table S4, Supporting Information).
Whereas, for superhydrophobic surfaces, the PDMS/PTFE com-
posite with SiO2 NPs of sizes 10, 15, 25, and 65 nm have occu-
pied the contact areas of ≈0.23, 0.15, 0.1, and 0.18 mm2 , respec-
tively (see Table S4, Supporting Information). Based on quanti-
fied terms such as the thermal conductivity of coatings and the
contact area of a water droplet with the surface, it is worth point-
ing out that the FDT mainly depends on the rate of heat transfer
dQ
( dt ), interfacial contact area between the water droplet and coat-
ing surface (A), thermal conductivity of the coated material (k),
and temperature gradient ( dT dx
). Equation (5) depicts the Fourier’s
law of heat transfer rate.[51]
( )
dQ dT
= −kA (5)
dt dx
Overall, the PDMS/PTFE/SiO2 (6:4) coated Al samples exhib-
ited around fourfold increment in FDT compared to that of the
PDMS/PTFE composite. This is because of the formation of
porous 3D micro-nanostructures and the creation of interfacial
air voids. The presence of air between the water droplet and the
micro-textured coating surface lowers the thermal conductivity
and decreases the heat transfer rate. Therefore, a significant in-
crease in the FDT for superhydrophobic surfaces is observed be-
cause a reduction in the contact area due to an increase in air
voids between the water droplet and the coating surface results
in a reduced rate of heat transfer.
Additionally, when the freezing process begins at the water
and CB surface interface, the air present in the voids initiates
upward migration into the water droplet owing to the Marangoni
force,[52] which arises because of the surface-tension gradient at
the interface between distinct fluids at low temperatures.[52] In
the present case, water and air are the two fluids present at the
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Figure 6. The comparison of water contact angle and photographs of freezing delay time at −15 °C temperature of bare Al, PDMS, PDMS/PTFE (6:4),
PDMS/PTFE/SiO2 (10 nm), PDMS/PTFE/SiO2 (15 nm), PDMS/PTFE/SiO2 (25 nm), and PDMS/PTFE/SiO2 (65 nm).

coating interface. When the temperature of the stage reaches
−15 °C, some air dissolves into the water droplet because air
solubility increases at low temperatures, and the remaining
air escapes from the water droplet. This reveals that, at low
temperatures, the permeation of water into the air voids of
the microstructure is possible. However, the spacings between
peaks or grooves on the microtextured surface morphology of
superhydrophobic surfaces play a crucial role.[46] Specifically,
if the spacing between peaks or grooves exceeds 20 μm, the
possibility of permeating water droplets into the voids of rough
surfaces is enhanced significantly.[46] Therefore, the utilization
of SiO2 NPs of size less than 65 nm in PDMS/PTFE/SiO2 NPs
composite favorably maintained the spacings between peaks or
grooves at approximately less than 2 μm, as shown in Figure 4.
Thus, the smaller spacing minimized the possibility of water
droplets permeation into the voids. Moreover, during freezing,

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ice embryos begin heterogeneous nucleation on the coating
surface, attempting to adhere to it by establishing van der Waals
and electrostatic bonds with the surface.[53] However, the elastic
moduli of PDMS/PTFE composite and ice are 3.2 MPa and
3.6 GPa,[54] respectively, which results in deformation incompat-
ibility due to a mismatch of elastic moduli. This capability of the
composite may be favorable for the easy detachment of ice from
the coating surface. After dethatching the ice from the coating
surface, the coating maintains its original dimensional stability
and durability owing to its reasonable mechanical strength.
2.6. Mechanical Property Analysis
The mechanical properties of icephobic coating are vital param-
eters because coating should withstand challenging conditions
such as extremely cold weather, frosting destruction, and high-
speed wind. The stress–strain curve of the bare PDMS and 9:1
to 5:5 weight ratios of PDMS to PTFE coatings are depicted in
Figure S9 (Supporting Information). The bare PDMS coatings
have shown 48% tensile strain and 0.9 MPa tensile stress. Fur-
thermore, as the quantity of PTFE from 1 to 4 weight percent
was added to the PDMS, the tensile strain and tensile stress of
the resulting PDMS/PTFE composite increased gradually. The
PDMS: PTFE (6:4) coating sample exhibited tensile stress and
tensile strain of 3.2 MPa and 129%, respectively. The tensile
fracture strength and stress-bearing capacity of the PDMS/PTFE
(6:4) composite were enhanced by 174% and 170%, respec-
tively, compared to bare PDMS. The bare PTFE has an excel-
lent Young’s modulus of 766 ± 29 MPa[55] and a low frictional
coefficient of 0.04–0.2.[56] In this study, the reinforcement of
PTFE particles into the matrix of polymeric PDMS chains con-
sequently improved the mechanical strength of the PDMS/PTFE
composite.[57,58] As the composite coating withstood with 3.2 MPa
of optimum elastic moduli, it provides the deformation incom-
patibility owing to the elastic moduli mismatch of the hard and
brittle nature of ice (Young’s modulus of ice is 0.3–3.6 GPa)[54]
and the soft elastic nature of PDMS/PTFE composite. This mis-
match in elastic modulus between ice and PDMS/PTFE coat-
ing can result in significant deformation incompatibility under
stress during ice removal. Additionally, the mechanical strength
of superhydrophobic surfaces is also a serious concern for long-
term exposure to extreme cold conditions. Thus, owing to the
excellent mechanical strength of PTFE, the integration of PTFE
into PDMS improves the coatings mechanical strength. Conse-
quently, it maintains the robustness of the superhydrophobic CB
state.
3. Conclusion
This study conveys new insights into the fabrication of icepho-
bic coatings based on the self-formation of superhydrophobic
surfaces using SiO2 NPs, surface wettability analysis, ice FDT,
and stress concentrator concepts. DFT calculations and struc-
tural studies revealed that the adhesion in PDMS and PTFE
originated from the stable induced dipole-dipole electrostatic in-
teraction between them; therefore, siloxane and the fluoropoly-
mer exhibited excellent miscibility. The integration of PTFE with
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PDMS played a vital role in improving the hydrophobicity, and
mechanical strength, and decreasing the surface energy of the
composite coatings. Surface morphology studies revealed that
the formation of porous 3D micro-nanostructured surfaces re-
duced the water/ice contact area by creating air voids. Further-
more, we successfully demonstrated that the ice FDT mechanism
mainly depended on the rate of heat transfer, thermal conductiv-
ity, and interfacial contact area of the coating surface. Overall,
the PDMS/PTFE/SiO2 coatings of size 25 nm exhibited the min-
imum IAS of 27 ± 3 kPa at −15 ± 1 °C. The proposed approach is
facile, cost-effective, and suitable for the large-scale preparation
of icephobic coatings.
4. Experimental Section
Materials: All coatings were applied on the Al substrate. The Sylgard
184 base and curing agent were purchased from Dow Corning. PTFE pow-
der (free-flowing) with a particle size of 1 μm was purchased from Sigma–
Aldrich. SiO2 NPs with sizes of 10, 15, 25, and 65 nm were obtained from
Sigma–Aldrich and US Research Nanomaterials, Inc. In this work, the
fumed SiO2 NPs of all sizes were utilized without any additional function-
alization. All chemicals used in the experiments were of analytical grade
and used as received.
Coating of PDMS/PTFE/SiO2 NPs: All coatings were fabricated under
ambient conditions (24 °C and 60% humidity). Before coating, the Al sub-
strate (20 mm × 20 mm × 2 mm) was polished with #2000-grit metal-
lographic abrasive paper and cleaned by ultrasonication. Subsequently, it
was washed with ethanol and deionized (DI) water, and dried at 80 °C for
30 min. All coatings were deposited using a laboratory-scale spin coater
(HS-EZ4, Zhengzhou TCH Instrument Co., Ltd.).
First, a Sylgard 184 base and a curing agent were mixed in the weight
percent ratio of 10:1 to prepare the PDMS viscoelastic solution. This mix-
ture was homogeneously mixed by hand for 5 min using a spatula. Bub-
bles were generated during mixing, and degassing was performed at am-
bient conditions for 20 min. Thereafter, 400 μL of the PDMS solution was
dropped on the Al substrate, and it was spin-coated at 400 rpm for 90 s.
To improve the mechanical strength of the coating, a controlled quantity
of PTFE powder (density = 2.15 g cm−3 ) was added to the PDMS solu-
tion (density = 0.965 g cm−3 ). PDMS-to-PTFE weight-to-weight % ratios
of 9:1, 8:2, 7:3, 6:4, and 5:5 were prepared to optimize PTFE addition as
a thixotropic agent to maintain the viscosity of the PDMS/PTFE compos-
ite for uniform film formation. Subsequently, each weight percent ratio of
the PDMS/PTFE composite was dropped onto the Al substrate and spin-
coated for 90 s at 500 rpm. The complete scheme of coatings fabrication
is depicted in Figure S3 (Supporting Information). Homogeneous film for-
mation of the PDMS/PTFE composite was observed (see Figure S4, Sup-
porting Information). To create the micro-nanoscale surface roughness on
the PDMS and PDMS/PTFE viscoelastic composites, SiO2 NPs with sizes
of 10, 15, 25, and 65 nm were sprinkled individually on bare PDMS and
PDMS/PTFE composites with different weight percent ratios (8:2 and 6:4).
A #60 copper mesh was used to sprinkle SiO2 NPs. The samples were then
kept under ambient conditions for 1 h to promote sedimentation and self-
formation of PDMS, PDMS/PTFE, and SiO2 NPs. After the sedimentation
of the SiO2 NPs in the PDMS and PDMS/PTFE composites, the loosely
bound SiO2 NPs were gently detached by blowing nitrogen air. Finally, all
of the coatings were cured in an oven for 12 h at 80 °C in the air.
Theoretical Calculation: To investigate the secondary interactions
between PDMS and PTFE, DFT calculations were performed using
the Vienna ab initio simulation package (version 5.4.4).[59–63] Van der
Waals (vdW) interactions are crucial for molecular adsorption on solid
surfaces. Therefore, the Perdew–Burke–Ernzerhof exchange-correlation
function[64,65] was employed with vdW interactions using the DFT-D2
method.[66,67] The projector-augmented wave method was used with a
cut-off energy of 400 eV. All the slab models included at least a 10 Å
vacuum region to avoid interaction between periodic atomic images along
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the vertical direction. A (2 × 2 × 1) Monkhorst–Pack mesh[68] was used
for k-point sampling after convergence testing. All the atomic structures
were relaxed until all atomic forces became less than 10−2 eV Å−1 and the
wave function converged to 10−6 eV.
Analysis: The surface property measurements, such as WCA, WSA,
contact angle receding (𝜃 rec ), and contact angle hysteresis were performed
on a contact angle goniometer (SDL200TEZED, Femtobiomed). Each
measurement was conducted by pouring 10 μL of DI water on the coat-
ing surface. The anti-icing performance of all the coatings was recorded
by analyzing the IAS and FDT. IAS measurements of all the coatings were
performed as described in the previous report.[21] The temperatures for
the ice adhesion test were maintained at −15 ± 1 and −2 ± 1 °C for the
cold Peltier plate and ice chamber (refrigerator), respectively. The real-time
temperature and humidity in the ice chamber were monitored using a tem-
perature and humidity sensor (UA10 RADIONODE, DEKIST Co., Ltd.).
Throughout the measurement process, the humidity of the ice chamber
varied in the range of 35–95 ± 5% (see Figure S5, Supporting Informa-
tion).
The FDT measurement setup mainly consisted of a temperature con-
troller stage (THMS600/720 with LNP95, Linkam Scientific Instruments,
temperature range of the THMS600 stage = −196–600 °C), IR camera (Re-
veal series, Seek Thermal with temperature range from −40 to +330 °C),
and a digital camera (Canon EOS 6D) with a macro lens (Focal length
100 mm, f/5.6, exposure time 1/40 s, ISO-250) (see Figure S6, Supporting
Information). The ice FDT measurements were performed as follows: 1)
The sample was put on a temperature controller stage, and the tempera-
ture of the stage was cooled down to −15 °C; 2) the surrounding tempera-
ture and humidity were maintained at 24 ± 3 °C and 60 ± 5%, respectively;
3) the delay in freezing of water on various substrates were recorded using
the digital camera; 4) the non-destructive IR thermometry imaging tech-
nique was used to record temperature and capture a thermal image of
phase transition, 5) after maintaining the surface temperature at −15 °C,
the water droplet of volume 10 μL was dropped on the coating surface us-
ing a micropipette (ARA, France, capacity = 2–20 μL), and 6) the FDT was
recorded. The change in the phase transformation from water to ice on all
the coating surfaces was recorded until the formation of a sharp tip (spike
shape) at the top of the ice.[69]
The microstructure of the coating layer was analyzed using XRD (Smart-
Lab, Rigaku). The functional groups of PDMS and PDMS/PTFE compos-
ites were confirmed using a FTIR spectrometer (Bruker VERTEX 80 V). The
chemical compositions of the PDMS and PDMS/PTFE coatings were in-
vestigated by using XPS (PHI 5000 Versa Probe II, ULVAC-PHI). Surface
morphology and elemental mapping analyses of all the coatings were per-
formed by FESEM (JSM-7001F, JEOL at 18 kV). The RMS surface rough-
ness of all coatings was measured on Bruker DEKTAK XT-E at 1 Å vertical
resolution. The stress–strain curve of coatings was performed on a uni-
versal tensile test tester (Instron-3342).
Supporting Information
Supporting Information is available from the Wiley Online Library or from
the author.
Acknowledgements
This work was supported by Korea Institute of Marine Science & Tech-
nology Promotion (KIMST) grant funded by the Ministry of Oceans and
Fisheries (KIMST-20210629). This work was supported by the Research
Assistance Program (2019) at the Incheon National University.
Conflict of Interest
The authors declare no conflict of interest.
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Data Availability Statement
The data that support the findings of this study are available from the cor-
responding author upon reasonable request.
Keywords
freezing delay time, icephobicity, PDMS/PTFE, SiO2 NPs, superhydropho-
bicity
Received: November 2, 2023
Revised: January 12, 2024
Published online:
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