Icephobic Strategies and Materials With Superwettability: Design Principles and Mechanism

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Interface Components: Nanoparticles, Colloids, Emulsions, Surfactants, Proteins, Polymers

Icephobic Strategies and Materials with
Superwettability: Design Principles and Mechanism
Muhammad Imran Jamil, Abid Ali, Fazal Haq, Qinghua Zhang, Xiaoli Zhan, and Fengqiu Chen
Langmuir, Just Accepted Manuscript • DOI: 10.1021/acs.langmuir.8b03276 • Publication Date (Web): 16 Nov 2018
Downloaded from http://pubs.acs.org on November 18, 2018
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Page 1 of 60 Langmuir
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3 Icephobic Strategies and Materials with Superwettability: Design Principles
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6 and Mechanism
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8 Muhammad Imran Jamil, Abid Ali, Fazal Haq, Qinghua Zhang*, Xiaoli Zhan and Fengqiu Chen.
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10 Zhejiang Provincial Key Laboratory of Advanced Chemical Engineering Manufacture
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Technology, College of Chemical and Biological Engineering, Zhejiang University, Hangzhou
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15 310027, China.
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18 ABSTRACT
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20 Ice formation and accretion on
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surfaces is a serious economic issue in
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25 energy supply and transports. Recent
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27 strategies for developing icephobic
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29 surfaces are intimately associated
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32 with superwettability. Commonly, the superwettability of icephobic materials depends on their
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34 surface roughness and chemical composition. This review critically categorizes the possible
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36 strategies to mitigate the icing problems from daily life. The wettability and classical nucleation
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theories are used to characterize the icephobic surfaces. Thermodynamically, the
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41 advantages/disadvantages of superhydrophobic surface are discussed to explain icephobic
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43 behavior. The importance of elasticity, SLIPSs, amphiphilicity, anti-freezing protein, organogels
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and stimuli-responsive materials has been highlighted to induce icephobic performance. In
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48 addition, the design principles and mechanism to fabricate icephobic surfaces with
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50 superwettability are explored and summarized.
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53 KEYWORDS: Icephobic surfaces, superwettability, elasticity, anti-freezing protein, organogels,
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stimuli-responsive material.
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Langmuir Page 2 of 60
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3 1. INTRODUCTION
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6 Ice build-up on surfaces is a major issue in various industries including transportation, power
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8 plants, wind turbines, and telecommunications. Icing results in injuries on road, sea and rail
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10 transportation, as well as hinders the operation of the components of aircrafts and
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telecommunication equipment.1 Icing also puts lives at risk during ice removal from
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15 hydroelectric power plants and wind turbines.2 In addition, ice accretion and frost formation
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17 dramatically affect the performance of refrigerators3 and heat exchangers.4
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20 Different icephobic strategies5 have been applied to preserve the surfaces from ice. Active
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23 methods such as electro-thermal and infrared heating systems are applied to keep the surfaces
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25 free from ice.6 These strategies are very expensive and require a lot of energy.7 Another strategy
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27 is the use of freezing point depressant salts and glycols. However, this strategy leads to
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environmental problems. De-icing techniques deal with eliminating the accreted ice from
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32 surfaces by applying mechanical forces. However, accessibility is a drawback into this
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34 technique.8 A more attractive and general strategy to combat the icing issue is to engineer the
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36 surfaces. It reduces the amount of water and adhesion of accreted ice on a surface. Bio-inspired
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39 surface materials also have great interest for icephobic application. Ice formation on solid
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41 substrates is a multiphase phenomenon which is divided into the following three main classes.
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43 (1) vapors to ice, desublimation (2) vapors to liquid to ice, condensation followed by freezing
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46 and (3) liquid to ice, freezing. It is generally known as freezing process which strongly depends
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48 on atmospheric humidity, temperature and pressure.9
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51 Literature defines the icephobicity as the capability of a surface to inhibit frost formation, reduce
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53 ice adhesion strength, delay heterogeneous ice nucleation, delay freezing time, rebound super-
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58 2
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3 cooled water droplets, inhibit the condensation of water, prevent transitions from Cassie to
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6 Wenzel state, and roll-off super-cooled water droplets easily as shown in Figure 1. 10,11,12,13
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8 Icephobicity
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super-cooled
18 drop rebound
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30 Figure 1. Current icephobic strategies. Reproduced and adapted with permission from ref. 14
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Copy right 2017, Royal Society of Chemistry.
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34 This review classifies the possible icephobic strategies and materials with superwettability into
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36 different categories. First we introduce the basic characterization parameters to design icephobic
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38 surfaces with the help of wettability and nucleation theories. Then the advantages/disadvantages
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41 of superhydrophobic surface are discussed in terms of thermodynamics to impart icephobic
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43 behavior. We have highlighted the importance of elasticity, SLIPSs, amphiphilicity, anti-freezing
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45 protein, organogels and stimuli-responsive material to induce icephobic performance. In each
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section, we have explained the design principles and mechanism to fabricate icephobic surfaces.
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50 2. WETTABILITY THEORIES
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53 Recently, the leading method to achieve icephobicity is based on controlling the wettability of
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55 surfaces. The surface wettability depends on chemical composition15 and roughness.16 The water
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58 3
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1
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3 contact angle (CA) 𝜃 is used to measure the wettability of the solid surface. Young’s17 equation 1
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6 is used to describe the CA on an ideal solid surface.18
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9 γsv = γsl + 𝛾𝑙𝑣 cos 𝜃 (1)
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12 Where γsl , γsv and 𝛾𝑙𝑣 represent the surface tensions between solid–liquid, solid–vapor and
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liquid–vapor interfaces respectively as shown in the Figure 2. Superhydrophilic (𝜃 →0°) or
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17 superhydrophobic (𝜃 >150°) surfaces are characterized according to the value of CA19. However,
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19 the Young’s equation is applied for ideally smooth surfaces and it is not possible practically. So,
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there is a need to consider the roughness parameter of the surface during the study of surface
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24 wettability. Two models Wenzel20 and Cassie-Baxter21 (Figure 2 b,c) are used to explain the
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26 relationship between surface roughness and the apparent CA. Wenzel model shows the intimate
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28 contact of water droplet with groove structured surface.22 The following equation 2 is used to
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31 describe the change in CA
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34 cos 𝜃𝑤 = 𝑟 cos 𝜃 (2)
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37 Where 𝜃𝑤 and r represent the apparent CA and ratio between the actual area to the apparent area
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39 on solid surface. The Wenzel equation shows that the hydrophilicity or hydrophobicity of the
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42 surface is enhanced by increasing the roughness of the surface.23 However, the Wenzel model
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44 becomes invalid due to the presence of trapped air in the groove structured surface. When a drop
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46 sits on a surface in a transition state and the voids are filled with air pockets then the Cassie-
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Baxter model is used24. It is described in the following equation 3 as
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52 cos 𝜃𝑐 = 𝑓𝑠 cos 𝜃𝑠 + 𝑓𝑣 cos 𝜃𝑣 (3)
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58 4
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1
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3 Where 𝜃𝑐 represents the apparent CA between the water droplet and rough surface, 𝜃𝑠 and 𝜃𝑣 are
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6 CA of the water with solid and vapor. While 𝑓𝑣 and 𝑓𝑠 represent the area fractions of vapor and
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8 solid on the surface respectively. When the droplet of water contacts with solid surface,
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11 𝑓𝑠 + 𝑓𝑣 = 1, 𝜃𝑠 = 𝜃, 𝜃𝑣 = 180° . Equation 3 can be written as
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cos 𝜃𝑐 = 𝑓𝑠 (𝑐𝑜𝑠𝜃 + 1) − 1 (4)
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18 Usually, apparent CA lies between the advancing contact angle25 𝜃𝐴 and receding contact26
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20 angle 𝜃𝑅 . The difference between 𝜃𝐴 and 𝜃𝑅 is known as the contact angle hysteresis (CAH).27,28
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22 In case of Wenzel model, the real contact area of the water droplet is greater than the projected
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25 area on the solid surface and the difference between θA and θR is high. On the other hand, in
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27 case of Cassie-Baxter state, the real contact area of water droplet is reduced than the projected
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29 area on solid surface and the difference between θA and θR is small.29
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45 Figure 2. a) Young’s model. b) Wenzel’s model. c) Cassie-Baxter’s model. Reproduced with
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47 permission18. Copyright 2018, Wiley.
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50 3. FUNDAMENTALS AND CHARACTERIZATION OF ICEPHOBICITY
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53 It still remains a challenge to evaluate and characterize the icephobic surfaces with one
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universally accepted test in the stage of laboratory work. This section focuses on basic
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3 characterization parameters to design icephobic surfaces with the help of wettability and classical
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6 nucleation theories. In literature the fundamental characterization parameters for icephobic
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8 surfaces are described such as low CAH, high receding contact angles,30 low water adhesion
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10 force, promoting homogeneous nucleation with high nucleation energy, high inhomogeneity and
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less stability at the interface of ice-substrate due to low elastic modulus.31
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16 3.1. LOW CAH AND HIGH RECEDING ANGLE. Kulinich et al. described a relation between
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18 wetting hysteresis (CAH) values and ice adhesion strength on the superhydrophobic surfaces.
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20 The low hysteresis surfaces, wetted in the Cassie-Baxter regime showed a smaller contact area
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23 between ice-substrate after freezing. While the high-hysteresis surfaces, partially wetted in
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25 Wenzel regime showed larger contact area between ice-substrate after freezing. Therefore, high
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27 hysteresis surfaces exhibit higher ice adhesion strength (IAS) and the surfaces with low CAH
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show icephobic behavior (low IAS).32,33 Meuler et al. described a direct relation between
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32 wettability parameter [1 + 𝑐𝑜𝑠𝜃𝑟𝑒𝑐 ] of water and ice adhesion strength by using 21 different
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34 polymer coatings on steel. They suggested receding contact angles 𝜃𝑟𝑒𝑐 greater than 120° cause
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to decrease the ice adhesion strength on surfaces, corresponding to this equation [1 + 𝑐𝑜𝑠𝜃𝑟𝑒𝑐 ] ≤
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39 0.5.34 Janjua et al. evaluated the ice adhesion strength of different coatings using a centrifuge
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41 device. They verified the relationship of increasing ice adhesion strength with increasing CAH
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up to 92° and lower ice-solid contact area at low CAH according to the previous study. Zero ice
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46 adhesion strength can be observed at CAH values of 25° as shown in Figure 3 A. However, high
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48 𝜃𝐴 were suggested to inhibit wetting before freezing but high 𝜃𝑅 and low CAH result a decrease
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50 in the ice adhesion strength after freezing.35
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3.2. LOW WATER ADHESION FORCE AND LESS STABLE INTERFACE. Recently, He et al.
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56 described the relationship between surface properties (water adhesion force, roughness,
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3 elasticity) and ice adhesion strength at room temperature by analyzing 24 hydrophilic and
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6 hydrophobic polymer samples. They found a direct relation between water adhesion force and
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8 ice adhesion strength, the samples with low ice adhesion strength showed very low water
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10 adhesion forces (180 to 270 μN) as shown in Figure 3 A.36 The surfaces with ice adhesion
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strength less than 10 kPa are known as super-low ice adhesion surfaces (SLIAS). The same
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15 author also demonstrated37 a novel crack initiator mechanism to fabricate SLIAS by introducing
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17 sub-structures into PDMS thin films as shown in Figure 3 B. Three mechanisms were presented
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as nano-crack initiator (NACI), micro-crack initiator (MICI) and macro-crack initiator (MACI)
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22 respectively. The macro-crack initiator (MACI) mechanism depends on the stiffness
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24 inhomogeneity and interfaces deformation incompatibility of the substrate. The crack formation
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26 at the ice-solid interface also depends on the stiffness inhomogeneity and interface deformation
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29 incompatibility of ice-substrate. Super-low ice adhesion surfaces can be designed by increasing
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31 the crack driving forces and the crack length 𝛼 at the ice-substrate interface. The ice adhesion
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33 strength 𝜏𝑐 on different substrates can be calculated by using the following equation 5.
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37 𝐺𝐸 ∗
𝜏𝑐 = √ (5)
38 𝜋𝛼𝐶
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40 Where E*, G, 𝛼 represent Young’s modulus, surface energy and the length of crack respectively.
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Chen et al. used poly methyl methacrylate and Al alloy with pits filled with low freezing point
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45 solutions compared to water. The swelling force of solution caused to decrease the stability of
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47 the ice-substrate interface and very low ice adhesion strength was observed due to the
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49 deformation at the interface.38
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4 A b)
a)
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33 Figure 3. A) (a) Ice adhesion versus contact angle hysteresis on coated and uncoated substrates
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35 Reproduced with permission.35 Copyright 2017, Elsevier (b) ice adhesion strength against water
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37 adhesion force Reproduced with permission.36 Copyright 2017, Nature. B) Schematic overview
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40 of ice cylinders on PDMS substrates with sub-structures (a) before and (b) during shear loading.
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42 The deformations in (a) have been ignored. Reproduced with permission.37 Copyright 2017,
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44 Royal Society of Chemistry.
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47 3.3. PROMOTING HOMOGENOUS NUCLEATION WITH HIGH NUCLEATION ENERGY.
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50 When ice nucleation occurs within water droplet, it is known as homogeneous ice nucleation
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52 while the heterogeneous ice nucleation occurs at the solid-liquid interface as shown in Figure 4
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54 A. The heterogeneous nucleation is more favorable for hydrophilic surfaces compared to
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3 superhydrophobic surfaces due to large contact area between water droplet and hydrophilic solid
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6 surface. It is possible to promote homogeneous nucleation by creating surface roughness with
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8 radius of nanoparticles less than 10 times compared to the critical ice nuclei size.39,40 Therefore,
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10 icephobic surfaces can also be designed by promoting homogeneous nucleation (responsible for -
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25 °C ice nucleation temperature of water on a surface) with high nucleation energy.41 The
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15 Figure 4 A show that how the water molecules aggregate to overcome the Gibbs free energy at
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17 critical ice embryo radius and change into new phase to initiate the ice growth.14 Gao et al.
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covalently grafted a series of copolymer/silica nano-composites on different substrates having
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22 C–H bonds under UV irradiation as shown in Figure 4B. They revealed the defining parameter f
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24 (heterogeneous and homogeneous nucleation free energy barrier ratio) to determine the
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26 icephobic/anti-icing ability of nano-spherical rough superhydrophobic surfaces. The author
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29 observed low icing probability on surfaces with small radius of nano-particles and high
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31 nucleation energy barrier. According to Figure 4B, the high nucleation free energy barrier ratio f
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33 (0.862) at 35 nm radius of nanoparticle show excellent anti-icing property.42 Cao et al. sprayed
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the composites of silica nanoparticle with butyl methacrylate, styrene and glycidyl methacrylate
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38 on the superhydrophobic surface to analyze the freezing process of super-cooled water. They
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40 also explained the role of nanoparticles size during ice formation with the help of heterogeneous
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nucleation theory. According to the equation 6, the free energy barrier for heterogeneous
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45 nucleation (ΔGc) around a spherical particle is reduced by a factor f (0 to 1) compared to
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47 homogeneous nucleation (ΔGc homo).
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50 ∆𝐺𝑐 = ∆𝐺𝑐ℎ𝑜𝑚𝑜 𝑓 (6)
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53 1 1 1−𝑚𝑥 3 𝑥3 𝑥−𝑚 𝑥−𝑚 3 3𝑚𝑥 2 𝑥−𝑚
54 f= + ( ) + [3 ( )+( ) ]+ ( − 1) (7)
2 2 𝑤 2 𝑤 𝑤 2 𝑤
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58 9
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1
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3 According to results, a gradual increase in icing probability was observed as the size of
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6 nanoparticle increased from critical ice nucleus radius 21.6 nm.43 The radius of the critical ice
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8 nucleus (rc) can be calculated using the following equation.
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11 𝑟𝑐 =
−2𝛾𝜈
(8)
12 Δ𝐺
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Here rc, γ, and ν represent the critical nucleus radius, water-ice interfacial tension and the molar
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17 volume of water respectively. Lo et al. also controlled the free energy barrier for nucleation on
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19 the rough silicon surface. They observed the longest ice-wrapping time and the shortest dwell
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time on V-shaped microgroove surface compared to plain and nanowire silicon surface.44 Zheng
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24 et al.45 fabricated superhydrophobic surface by deposition of silver on the copper plate followed
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26 by modification with 1-dodecanethiol coating at 69 % humidity. They explained the direct
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28 relationship between the contact angle 𝜃 and the nucleation energy barrier. The prepared surface
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31 showed a delay in freezing point due to high nucleation energy barrier ∆G and lower nucleation
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33 rate J according to the following equations.
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36 (2−3 cos 𝜃+ 𝑐𝑜𝑠 3 𝜃)
37 ∆G= π σlv 𝑟 *2 (9)
3
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40 ∆𝐺
41 𝐽 = 𝐽0 𝑒 −𝐾𝑇 (10)
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44 The equation 10 shows the inverse relation between nucleation rate J and nucleation energy
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46 barrier ∆𝐺 . Jung et al. evaluated the freezing process and motion of super-cooled (-15 °C) water
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drops on superhydrophobic substrates at -15 °C. The homogeneous nucleation was observed at
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51 the gas–liquid interface due to evaporative cooling under unsaturated humidity conditions. They
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53 also predicted the transition between homogeneous and heterogeneous nucleation with the help
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55 of nucleation theory and heat transfer analysis under high humidity.46
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4 b)
A a)
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17 a bbB
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a
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27 C
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30 D
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32 Figure 4. A) (a) Schematic diagram shows the regions within a water droplet where homogenous
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and heterogeneous ice nucleation occurs. Reproduced with permission.39 Copyright 2015,
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37 American Chemical Society (b) Gibbs free energy barrier during freezing process against the ice
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39 embryo radius. Below critical size, the ice embryo is metastable and above critical size, the ice
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41 embryo is stable to initiate the freezing process Reproduced with permission.14 Copyright 2017,
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44 Royal Society of Chemistry B) (a) covalent attachment of a copolymer/nanoparticle composite to
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46 C–H containing substrates. (b) The relationship between nanoparticle radius (R) and the ratio (f)
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48 i.e free energy barrier between heterogeneous and homogeneous nucleation on spherical surface.
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51 Reproduced with permission42. Copyright 2016, Royal Society of Chemistry.
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3 4. DESIGN PRINCIPLES, MECHANISM AND CLASSIFICATION OF ICEPHOBIC
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6 SURFACES
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9 4.1. SUPERHYDROPHOBIC SURFACES. Superhydrophobic surfaces mimicking mosquito
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11 compound eyes, lotus leaves47 and legs of water strider48 show contact angle of a liquid droplet
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13 greater than 150°. The air pockets are trapped inside the surface textures due to the micro-
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16 nanostructure roughness. Superhydrophobic surfaces have the ability to control the boiling,
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18 freezing and phase-change phenomena of water.49 Quéré et al. revealed the superhydrophobic
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20 surfaces for icephobic applications by allowing the deposited water droplets to fall off due to
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23 gravity at subzero conditions before freezing.
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26 4.1.1. SHORT CONTACT TIME AND SMALL RADIUS OF WATER DROPLET. Richard et al.
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28 measured the short contact time with small radius of a bouncing droplet on superhydrophobic
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30 surfaces at different Weber number (W) without any effect of impact velocity as shown in the
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33 Figure 5 A.50 Bird et al. explored non-axisymmetric recoiling of the water droplet to reduce the
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35 contact time on superhydrophobic surfaces. They also observed the redistribution in mass and
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37 change in the hydrodynamics of water droplets as shown in Figure 5B.51 Tsai et al. investigated
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the drop impact dynamics onto polymeric micropatterns composed of PDMS elastomer and
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42 rough carbon nanofibers superhydrophobic surfaces. The splashing impact with several satellite
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44 droplets was observed on rough carbon nanofibers at large Weber number. The rough carbon
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nanofibers showed better ice-phobic behavior due to reduce contact time of satellite droplets.52
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49 Liu et al. established the pancake bouncing on the copper superhydrophobic surface and
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51 observed a four-time reduction in contact time as compared to conventional complete
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53 rebounding. The capillary energy stored in the penetrated liquid is considered the main factor for
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56 pancake bouncing to lift the drop as shown in Figure 5B.53
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58 12
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3 4.1.2. THERMODYNAMICALLY DELAY IN FREEZING POINT OF WATER. The delay in
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6 freezing point of water droplet in contact with superhydrophobic surface54 depends on the heat
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8 transfer rate between the water droplet and the substrate. The following equation 11 describe the
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10 heat transfer rate between two surfaces.41
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13 𝑑𝑄 𝑑𝑇
14 = −𝑘𝐴 ( ) (11)
𝑑𝑡 𝑑𝑥
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16
17 𝑑𝑄
Here , k and A, represent the heat transfer rate, coefficient of thermal conductivity and
18 𝑑𝑡
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20 interfacial area respectively while
𝑑𝑇
is temperature gradient. Therefore, superhydrophobic
21 𝑑𝑥
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23 surfaces in Cassie-Baxter state delay the ice formation due to the following reasons: (i) small
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25 𝑑𝑄
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interfacial area A and low heat transfer rate between water droplet and superhydrophobic
𝑑𝑡
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28 surface, (ii) presence of insulated air pockets between water droplet and substrate (iii) low
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probability of heterogeneous nucleation at the water-substrate interface. Tourkine et al used
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33 superhydrophobic copper plates and showed delay in freezing of deposited water due to the
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35 presence of thermally insulated air pockets.55 Inspired by the butterfly wings, Guo et al.
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37 synthesized a robust icephobic surface with CA 150° using ZnO and
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40 heptadecafluorodecyltripropoxysilane (FAS-17) and obtained micro/nanostructures (MN) instead
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42 of individual microstructures or nanostructures, or smooth. They observed delay freezing time of
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44 7200 sec on the MN-surfaces at –10 °C due to the high ratio of air pockets between the drop and
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MN-surface. Thermodynamically, the drop on MN-surface absorbs heat from air through thermal
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49 radiation and contact heat conduction. Then the heat of drop gets transferred to cold MN-surface
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51 in the form of thermal radiation and contact heat conduction through nano hairs. The following
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equation shows the heat gain and loss in unit time
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58 13
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1
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3 ∆h = ℎ𝑔 + ℎ𝑔′ − ℎ𝑙 − ℎ𝑙′ (12)
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The heat loss in the form of thermal radiation and contact heat conduction in MN-surface is
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9 small due to less contact area between liquid–solid and large proportion of trapped air. Thus the
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11 value of Δh on the MN-surface is greater compared to the nano, micro and smooth surfaces i.e.,
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13 Δh (MN) >Δh (N) > Δh (M) >Δh (S). The value of Δh is inversely proportional to the
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16 decrease/change in temperature of drop tf according to the following equation 13. The
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18 decrease/change in temperature of the drop is expressed as
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21 𝜌𝑤 𝐶𝑝 (𝑡𝑜 −𝑡𝑠 )
22
𝑡𝑓 = (13)
∆ℎ
23
24
25 Where ρw, Cp represents the density and heat capacity of water at a constant pressure while to is
26
27 the initial temperature of the drop; and ts is the sample surface temperature. The equation 13
28
29
30
indicates that a large Δh would cause a small tf. Thus the temperature change of a drop is smaller
31
32 on the MN surface as compared to smooth surfaces.56 Wang et al. used Kelvin’s law and
33
34 Clapeyron equation to explain the delay in freezing process on the superhydrophobic surface.
35
36
Kelvin’s law is given below
37
38
39 2γVm
40 𝑃𝑟 = P exp ( ) (14)
RTr
41
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43 Where P and Pr indicate the saturated vapor pressure and vapor pressure at temperature T. R, Vm,
44
45
46 γ and r represent the gas constant, molar volume, surface energy and radius of droplet
47
48 respectively. It is obvious from the equation that the vapor pressure and radius of a droplet on the
49
50 superhydrophobic surface are inversely related to each other. Thus the small radius of a water
51
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53 droplet on the superhydrophobic surface causes large Pr value. So, the superhydrophobic surface
54
55 has a small amount of condensed water than that of the hydrophilic surface.
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58 14
59
1
2
3 The integrated Clapeyron equation is given below
4
5
6 𝑇2 ∆𝑠 𝑉𝑚
7 𝑙𝑛 = (𝑃2 − 𝑃1 ) (15)
𝑇1 ∆𝑠 𝐻𝑚
8
9
10 where ΔsHm and ΔsVm represent the enthalpy and volume change during the freezing process.
11
12
13 According to equation 15 the temperature and vapor pressure are inversely proportional to each
14
15 other. In other words, the small value of r (radius of a condensed water droplet) and its high
16
17 vapor pressure would lower the freezing temperature of a droplet on superhydrophobic surface.57
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20
Birjandi et al. revealed that plant leaves (kale and lettuce) delay the ice formation due to their
21
22 surface microstructures. The author observed quick change in the temperature of water drops on
23
24 a lettuce leaf as compared to the kale leaf. The kale leaf showed delay in heat transfer and initial
25
26
freezing process than that of lettuce leaf as shown in Figure 5C.58 He et al. observed the delay in
27
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29 the freezing of water and retardation in frosting at the metastable three-phase line region on
30
31 superhydrophobic isotactic polypropylene film.59 Bezdomnikov et al. also observed ten hours
32
33 freezing delay of super-cooled water droplets deposited on the textured superhydrophobic
34
35
36 surface of silicone rubber at -18 °C.60 Nguyen et al. fabricated superhydrophobic surface using
37
38 polystyrene beads via lithography and showed longest freezing delay with smallest ice adhesion
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40 strength on sample with 30 nm top diameter (irrespective to its height) compared to the bare and
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43
high top diameter substrate.61 Zhan et al. synthesized a superhydrophobic anti-icing coating by
44
45 grafting silica nanoparticles with fluorinated polymers via ATRP. The silica nano-composite
46
47 coating of flurinated copolymer of butylacrylate helped for the easy removal of droplets as well
48
49
as showed the delay in the freezing time due to the depression of crystallization point.62 Wu et al.
50
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52 established a transparent anti-icing coating on wood boards on the basis of a bio epoxy resin and
53
54 showed icing delay with 50 kPa ice adhesion strength at -20 °C.63 Jin et al. fabricated an efficient
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58 15
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1
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3 anti-icing superhydrophobic surface on Al by etching followed by surface modification with a
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6 fluoroalkylsilane film which delayed the freezing process about six times.64
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9 A d
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25 B a b
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45 Figure 5. A) (a-c) Hitting of a water droplet on superhydrophobic solid with different Weber
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47
numbers (W) (d-e) Contact time of a bouncing droplet versus drop radius and impact velocity.
48
49
50 Reproduced with permission.50 Copyright 2002, Springer Nature. B) (a) Non-axisymmetric
51
52 retraction in which the center of the film assists in the recoil Reproduced with permission.51
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54 Copyright 2013, Springer Nature. (b) Pancake bouncing of a droplet on the tapered surface.
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58 16
59
1
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3 Reproduced with permission.53 Copyright 2014, Springer Nature. C) Freezing process of a water
4
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6 droplet on lettuce and kale leaves at -10 °C. Reproduced with permission.58 Copyright 2017,
7
8 Springer Nature.
9
10
11 4.1.3. DRAWBACKS OF SUPERHYDROPHOBIC SURFACES.
12
13
14 Superhydrophobic surfaces also have some drawbacks about their icephobic behavior in
15
16
17
particular conditions. Kulinich65, Varanasi66 and Farhadi67 et al. observed the frost nucleation on
18
19 top and between asperities of the superhydrophobic surface as shown in Figure 6 A. The frost
20
21 formation resulted, to increase the ice-surface contact area, increase in ice adhesion strength and
22
23
ultimately loss of superhydrophobic properties due to transition from Cassie ice to Wenzel ice.
24
25
26 Jung et al evaluated the icephobicity of hydrophilic and superhydrophobic surfaces. The freezing
27
28 process was found to be delayed significantly on surfaces with roughness similar to the critical
29
30 ice nucleus radius at -20 °C. When the roughness of hydrophilic surface was comparable to the
31
32
33 critical ice nucleus radius, it showed longer freezing delay time compared to superhydrophobic
34
35 surface.68 Yizhou Shen et al. fabricated the hierarchical micro-nanostructure superhydrophobic
36
37 surfaces (HN-Surface) on Al substrate and compare its anti-icing efficiency with single
38
39
40
nanostructure (SN-Surface). The results showed poor anti-icing efficiency of HN-Surface due to
41
42 the accumulation of super-cooled microdroplets into the micrometer textures and caused the
43
44 quick ice formation as shown in the Figure 6 B.69 The same author also revealed the pinning of
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46
the contact line on the cold superhydrophobic surface as shown in the Figure 7b. The transfer of
47
48
49 heat from water droplet to the cold surface caused a loss of moving ability of the molecules of
50
51 water at the triple-phase. Moreover, the van der Waals and electrostatic interactions are also
52
53 caused the pinning of contact line.70
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58 17
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A a) b)
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18 B a
19 b
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33 Figure 6. A) ESEM images of frost formation on a superhydrophobic surface at -13 °C
34
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Reproduced with permission.66 Copyright 2010, AIP B) (a) Schematic diagram shows the
37
38 accumulating and freezing process of super-cooled micro-droplets on the hierarchical
39
40 superhydrophobic surface with micro-nanostructure and single nanostructure Reproduced with
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42
permission.69 Copyright 2017, Wiley. (b) Schematic illustration of contact line pinning on the
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45 cold superhydrophobic surface. Reproduced with permission.70 Copyright 2018, American
46
47 Chemical Society.
48
49
50 4.2. ELASTIC SURFACES. Elastomers are the latest class of materials to induce icephobicity.
51
52
53
The elastomers reduce the contact time of water droplets due to elasticity and produce stresses at
54
55 the interface of ice-coating to remove the ice easily.71 Weisensee et al. explained the springboard
56
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58 18
59
1
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3 effect and showed a two-fold reduction in contact time of water droplets impacting on an elastic
4
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6 superhydrophobic surface compared to equivalent rigid surface. The upward force of elastic
7
8 substrates completely detach the droplets by converting the surface energy into kinetic energy.
9
10 Harmonic motion is also observed on the elastic/flexible substrate due to its oscillation at normal
11
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13
frequency just after the water droplet impact. It causes to early lift-off of the droplet from the
14
15 surface in a pancake bouncing i.e springboard effect as shown in Figure 7a.72,73 Vasileiou et al.
16
17 deposited the dispersions of (poly(vinylidene fluoride) in (N-methyl-2-pyrrolidone),
18
19
poly(methyl methacrylate) and hydrophobic fumed silica onto the flexible substrates (low-
20
21
22 density polyethylene). The prepared flexible superhydrophobic surface showed short contact
23
24 time, no impalement into the texture and minimum droplet spreading with no breakup compared
25
26 to the rigid superhydrophobic substrate as shown in Figure 7b. Moreover, the author explained
27
28
29 more water repellency on butterfly wings due to the flexibility of wings. The repellency of
30
31 viscous and super-cooled droplets has been observed on flexible substrates due to the absorption
32
33 and modification of the K.E of the droplet by the flexible surface.74
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37 a)
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46 b)
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57 c)
58 19
59
1
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3 Figure 7. (a) Harmonic oscillation of elastic substrate and early lift-off droplet with pancake
4
5 72
6 shape during the droplet impact. Reproduced with permission Copyright 2016, Nature (b)
7
8 Comparison of impalement resistance between rigid and flexible superhydrophobic substrates.
9
10 Reproduced with permission.74 Copyright 2016, Nature.
11
12
13
Beemer et al. fabricated low ice adhesion 𝛕𝐢𝐜𝐞 = 5 kPa) PDMS gels by hydrosilylation of vinyl-
14
15
16 terminated PDMS with hydride-terminated PDMS as shown in the Figure 8 A. The author
17
18 explained the mechanism of ice separation from PDMS gels with the help of Kendall and
19
20 Chaudhury’s equation 16. Here 𝛕𝐢𝐜𝐞 represents the critical shear stress required to detach a rigid
21
22
23 body (ice) from a thin film
24
25
26 𝑊𝑎𝑑ℎ 𝜇
27
𝜏𝑖𝑐𝑒 ∝ √ (16)
𝑡
28
29
30 Wadh , 𝜇 and t show adhesion work between ice and material, modulus of the material and film
31
32
33 thickness respectively.75 According to Equation 16 the soft materials with low modulus
34
35 μ are required for ultra-low adhesion and adhesive failure of ice. However, the surfaces with
36
37 liquid lubricants have negligible shear modulus μ ≈ 0 and leads to a cohesive failure of liquid
38
39
40
lubricant during the removal of ice as shown in Figure 8 B. Yeong et al. fabricated a durable self-
41
42 lubricating elastomer icephobic coating by infusing silicone oil into the elastomer to minimize
43
44 the ice adhesion in harsh conditions.76 Wang et al. used ZnO nano-rods-coated PDMS surface
45
46 followed by modification with FAS-17 to fabricate a robust icephobic surface at -30 °C and
47
48
49 showed its fast recovery to original state due to elasticity.77,78 Zhuo et al. also designed self-
50
51 healing icephobic material by selecting an elastomer of Fe-pyridine dicarboxamide-containing
52
53 PDMS (Fe-Py-PDMS) due to its low surface energy and modulus. The prepared icephobic
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58 20
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1
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3 material showed durability and retained 12.2 kPa ice adhesion strength after fifty icing-deicing
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6 cycles.79
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10 A
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23 B
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38 Figure 8. (A) Schematic shows the fabrication of PDMS gels. (B) Schematic shows the cohesive
39
40 and adhesive failure during ice separation from soft material. Reproduced with permission.75
41
42 Copyright 2016, Royal Society of Chemistry.
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44
45 4.3. SLIPPERY LIQUID-INFUSED POROUS SURFACES
46
47
48 The natural Nepenthes pitcher plant inspired slippery liquid-infused porous surfaces (SLIPSs)
49
50 have been involved in anti-icing and antifouling properties due to their excellent liquid
51
52 repellency.80,81 Although the water droplet motion on a slippery surface is typically slower
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55
compared to the superhydrophobic surface, its smooth surface and stability under high humidity
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58 21
59
1
2
3 and pressure make the SLIPS an encouraging strategy alternative to the superhydrophobic
4
5
6 surface in particular conditions. Moreover, the elimination of possible ice nucleation sites82 due
7
8 to the homogeneous interface83 and delay in freezing time also make the SLIPS a favorable
9
10 substitute to the superhydrophobic coatings8. Vogel et al. improved the stability of SLIPS by a
11
12
13
closed-cell architecture. The prepared SLIPS showed nine months stability with a very low value
14
15 of ice adhesion strength.84 Kim et al. developed SLIPS by electrodeposition of textured
16
17 polypyrrole followed by infusing perfluoroalkylether as a lubricant on aluminum substrates.
18
19
These SLIPSs removed both the condensed water droplets and accreted ice easily.85 Irajizad et al.
20
21
22 covered the Si substrate with oil-based ferrofluid of iron oxide nanoparticles (10-20 nm) to make
23
24 self-healing magnetic slippery surfaces MAGSS as shown in Figure 9a. The magnetic liquid-
25
26 liquid interface offered a low-energy interface for heterogeneous ice nucleation with the Gibbs
27
28
29 energy barrier near to homogenous limit. The MAGSS showed a delay in ice formation, high
30
31 mobility for liquids, low shear strength of ice and stability even at 105 Reynolds number. In this
32
33 approach, the author exploited the magnetic volumetric force to dismiss the role of the liquid-
34
35
36
solid interface during ice formation.86 Zhang et al. synthesized a robust double layered SLIPS
37
38 anti-icing coating on Mg alloy substrate. The prepared SLIPS showed delay in freezing point of
39
40 water with a low value of ice adhesion strength due to the inhibition of heterogeneous ice
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42
nucleation.87 Tao et al. developed an efficient and durable slippery icephobic coating based on
43
44
45 polysiloxane by hydrosilylation of polymethylvinylsiloxane, polymethylhydrosiloxane and
46
47 fluorinated polyhedral oligomeric silsesquioxanes. The prepared coating showed ultra-low 3.8
48
49 kPa ice shear strength and maintained the icephobicity after fifteen icing and deicing cycles.88
50
51
52 Coady et al. prepared the SLIPS by infusing the porous Al oxide with silicone oil as shown in
53
54 Figure 9b. The UV cross-linked siloxane resins were infused to enhance the slippery and
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56
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58 22
59
1
2
3 icephobic behavior with less than 10 kPa ice adhesion strength.89 Wang et al. also fabricated a
4
5
6 robust self-cleaning, slippery anti-icing coating with low ice adhesion strength by pouring a
7
8 SiO2-UHMWPE (ultra-high molecular weight polyethylene) suspension with kerosene oil on
9
10 different substrates.90 Chen et al. fabricated slippery surfaces by cellulose lauroyl ester (CLE)
11
12
13
solution and perfluoropolyether lubricant. The nanoparticle suspension of CLE was sprayed on
14
15 the glass to get nanoporous CLE film as shown in Figure 9c. The delay in ice nucleation was
16
17 found on prepared slippery films compared to superhydrophobic films.91 Liu et al. developed
18
19
one-step, transparent and omniphobic SLIPS coating by penetrating fluorinated lubricant into
20
21
22 PTFE nano particles as shown in Figure 9d. The prepared SLIPS showed decrease in ice
23
24 adhesion strength, icing-delay, anti-corrosion and self-cleaning properties.92 According to Anand
25
26 et al. the major drawbacks of SLIPSs are poor stability (due to evaporating or leaking of organic
27
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29 lubricant) and high prices of perfluorinated lubricants.93
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24 c)
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30 d)
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41 Figure 9. (a) A droplet of water on the superhydrophobic and liquid-infused surface makes a
42 solid-water interface to promote heterogeneous ice nucleation. However, in MAGSS, the droplet
43 of water makes a magnetic liquid-water interface with lower interfacial energy than in the solid-
44
45 water interfaces. Reproduced with permission.86 Copy right 2016, Nature. (b) Process diagram
46 for the fabrication of UV-cured SLIPS. Reproduced with permission.89 Copy right 2018,
47 American Chemical Society (c) Schematic diagram of the fabrication of slippery cellulose
48
49 lauroyl ester surfaces. Reproduced with permission.91 Copyright 2014, American Chemical
50 Society. (d) Schematic diagram for the fabrication of SLIPSs. Reproduced with permission 92
51 Copy right 2018, Elsevier.
52
53 4.3.1. SLIPSs WITH AQUEOUS LUBRICATING LAYER. Inspired by ice skating, Chen et al.
54
55
56 revealed an anti-ice coating with a self-sustainable lubricating layer of water between the ice and
57
58 24
59
1
2
3 solid surface. They proposed the idea that melting due to the pressure and frictional heating
4
5
6 breaks down the hexagonal structure of ice and lubricate the blade with a thin layer of water to
7
8 allow the skaters to spin easily as shown in Figure 10a. The aqueous lubricating layer is formed
9
10 during the freezing process at low temperature and stays as long as ice remains atop. This
11
12
13
strategy does not have durability problem due to the resupply of water from moisture and melted
14
15 ice. Therefore water is certainly an ideal lubricant to mitigate the icing problems. The author
16
17 used adhesive dopamine (DA) and hyaluronic acid (HA) due to their ability to absorb moisture
18
19
and measured the ice adhesion strength by changing the thickness and viscosity of aqueous film.
20
21
22 The lowest ice adhesion 61 kPa was observed at 20 nm film thickness with 0.33 mole ratio of
23
24 HA to DA.94 The same author used photolithography and grafted the cross-linked poly acrylic
25
26 acid inside the micropores of the silicon wafer as shown in Figure 10b. The hydrophilic self-
27
28
29 lubricating liquid water layer (SLWL) surfaces showed low ice adhesion value above -25 °C but
30
31 the sudden increase in ice adhesion was observed below -25°C due to the phase transition of
32
33 lubricating water into ice. The phase transition temperature can be lowered by changing the
34
35
36
concentration and type of hygroscopic polymer.95 Dou et al. also measured the strength of ice
37
38 adhesion by mixing polyurethane with different ratio of dimethylolpropionic acid (hydrophilic
39
40 component). They observed three stages of the freezing of free water, bound water and
41
42
completely disappearance of lubricating water layer: (1) In range of -15°C to -53°C the ice
43
44
45 adhesion retained about 27 kPa due to freezing of free water in aqueous lubricating layer, (2) at -
46
47 53°C to -60°C the value increased quickly up to 200 kPa due to freezing of bound water and (3)
48
49 after -60°C the value increased abruptly up to 700 kPa due to complete disappearance of the
50
51
52 aqueous lubricating layer. At -53 °C, 200 kPa ice adhesion was observed, which was similar to
53
54 that of polyurethane without hydrophilic component.96
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58 25
59
1
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3 Chen et al. also studied the fraction of non-freezable, freezable and free water within a
4
5
6 hydrophilic conjugate of poly acrylic acid and dopamine (PAA-DA) as shown in Figure 10c. The
7
8 non-freezable water (responsible to prevent water from freezing) makes hydrogen bonding with
9
10 the hydrophilic groups and freezable water present nearby the attached molecules of water.97 The
11
12
13
fraction of two kinds of water was changed by changing the cross-linkage of hydrophilic
14
15 polymer.98 The author scrutinized the effect of cross-linking on ice adhesion strength by
16
17 exploring the conjugation efficiency (f) of DA to PAA (mole ratio between PAA and DA). The
18
19
increase in conjugation efficiency (f) of DA to PAA steadily reduce the ice adhesion till τice = 30
20
21
22 kPa due to the increase in the fraction of unfreezable water Cunf which act as a lubricant in the
23
24 network. Therefore, the synergistic effect of an increase in the fraction of unfreezable water Cunf
25
26 and depression in freezing point of freezable water steadily decreased the ice adhesion strength.
27
28
29 According to Flory equation (17), they calculated the gradual depression in freezing temperature
30
31 Tc of water with the increase in fraction of polymer φp within the network.
32
33
34 1 1 𝑅 𝜑𝑝 1⁄
− = {[−𝑙𝑛(1 − 𝜑𝑝 ) − 𝜑𝑝 − χ𝜑𝑝 2 ] + [ 𝜌𝑒 ( − 𝜑𝑝 3 )]} (17)
35 𝑇𝑐 𝑇𝑐 0 ∆𝐻𝑚 2
36
37
38 Where Tc0 , ΔHM, R, χ, and ρe represent the pure water freezing temperature, molar enthalpy of
39
40 crystallization, gas constant, interaction parameter of polymer with water and cross-link density
41
42
43 respectively.99 Ozbay et al. impregnated the hydrophilic and hydrophobic solvents onto
44
45 polypropylene and cellulose surfaces. The hydrophilic porous surfaces impregnated with
46
47 hydrophilic solvent (water-85%glycerin) showed depression in freezing point of a super-cooled
48
49
50
water droplet and very low ice adhesion at -2 °C.100 Chernyy et al. used the SI-ATRP method to
51
52 synthesize superhydrophilic anti-icing coatings of polyelectrolyte brush. The cationic and
53
54 anionic polyelectrolyte brushes were exchanged with different ions. The Li+ and Na+ counter-
55
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58 26
59
1
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3 ions showed the reduction in ice adhesion strength by 40% and 25%, respectively at -18 °C.101
4
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6 Tao et al. synthesized the transparent zwitterionic anti-icing and antifogging coating of poly
7
8 (methacryloxyethy sulfobetaine-co-hexafluorobutyl methacrylate-co-allyl methacrylate) with
9
10 different amounts of oligoethylene glycol dimethacrylate. The strong hydrogen bonding between
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13
zwitterion and water molecules would generate non-freezable bound water.102.103
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16 b)
a)
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30 c)
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46 Figure 10. (a) Ice skating inspired anti-icing coating. Reproduced with permission.94 Copyright
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2014, Wiley. (b) (1) Fabrication of silicon wafer surface by using photolithographic technique.
50
51 (2) Grafting the micro-pore with hygroscopic polymers. (3) Formation of self-lubricating liquid
52
53 water layer due to condensation. (4) Formation of ice on the top of self-lubricating liquid water
54
55 95
layer. (5) shedding off the ice due to wind action. Reproduced with permission Copyright
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58 27
59
1
2
3 2013, American Chemical Society (c) Synthesis and fabrication of mussel-inspired PAA-DA
4
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6 conjugate for anti-icing coating with self-sustainable aqueous lubricating layer. Reproduced with
7
8 permission.99 Copyright 2017, American Chemical Society.
9
10
11 4.4. AMPHIPHILIC SURFACES. Amphiphilic polymers consist of hydrophobic and
12
13 hydrophilic components, the amphiphilic polymer based coatings disperse the water molecules
14
15
16 and decrease the ice adhesion strength due to their hydrophilic and hydrophobic groups
17
18 respectively. Upadhyay et al. revealed the decrease in ice adhesion strength on polyurethane-
19
20 based amphiphilic coatings of hydrophobic PDMS and hydrophilic PEG.104 Van Dyke et al.
21
22
23 fabricated the biphilic surfaces by photolithography to mask the hydrophilic spots with a
24
25 deposition of a self-assembled monolayer of octadecyltrichlorosilane. The prepared biphilic
26
27 surface not only suppressed the freezing point of water at 60% humidity but also changed the
28
29
size and number of drops.105 Zigmond et al. also established amphiphilic hyperbranched
30
31
32 fluoropolymers, crosslinked through a nucleophilic reaction between the amino group of bis(3-
33
34 aminopropyl) terminated PEG. The author observed -25 °C and 0 °C freezing point of bound and
35
36 free water respectively within the HBFP(III)-PEG matrix through DSC analysis.106 Li et al.
37
38
39 observed anti-fogging along with the delay in freezing point of water on amphiphilic coating of
40
41 polyhedral oligomeric silsesquioxane (POSS-PDMAEMA-b-PSBMA) as shown in Figure 11A.
42
43 The low surface energy POSS groups impart hydrophobicity to the surface and zwitterionic
44
45
46 groups Poly(sulfobetaine methacrylate) PSBMA in copolymer make hydrogen bonding with
47
48 non-freezable bound water to form aqueous lubricating layer.107
49
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51 Chen et al. also synthesized the self-lubricating icephobic coating of an amphiphilic copolymer
52
53 of (PDMS)-(PEG) and observed low ice adhesion than that of smooth and hydrophobic surfaces.
54
55
56 They explained the mechanism of low ice adhesion strength on the amphiphilic surfaces on the
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58 28
59
1
2
3 basis of interaction with ice/water molecules and proved the presence of density-depleted region
4
5
6 between the water and the hydrophobic surface as shown in Figure 11B. The author calculated
7
8 the ice adhesion strength 𝜏𝑎 on amphiphilic surface with the help of following equation 18.
9
10
11 𝜏𝑎 =
𝐴
(18)
12 6𝜋𝐷3
13
14 Where D is the thickness of the depletion layer which increased by increasing the hydrophobicity
15
16 of the surface and A is the constant. The surface hydrogen-bonded water molecules remained
17
18
19 non-frozen, even below the freezing point of water and served as a self-lubricating interfacial
20
21 liquid-like layer to reduce the ice adhesion strength with amphiphilic surface. The existence of
22
23 non-frozen water molecules at the ice-solid interface was confirmed by solid-state nuclear
24
25
26
magnetic resonance spectroscopy. NMR analysis also measured the high viscosity of the non-
27
28 frozen water molecules which delayed the heterogeneous ice nucleation on amphiphilic
29
30 coatings.108 Liu et al prepared poly [2-(Methacryloyloxy)ethyl] trimethylammonium chloride
31
32 (PMETA) brushes via SI-ATRP and changed the wettability from a hydrophilic to a hydrophobic
33
34
35 by changing the ions like Cl-1, ClO4-, PF6-, PFO-2. The author explained the mechanism of the
36
37 establishment of water depletion region to suppress the ice propagation on dehydrated
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39 polyelectrolyte surfaces with hydrophobic counter-ion as shown in Figure 11C. The amount of
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42 freezable water within the polyelectrolyte brush was found to be decreased significantly by
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44 increasing the hydrophobicity of counter-ions.109 Zhang et al. also fabricated an amphiphilic anti-
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46 icing and thermotropic deicing coating based on photo-thermo responsive magnetic nanoparticles
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with P(poly(ethylene glycol) methyl ether methacrylate-co- glycidyl methacrylate. The -36.8 °C
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51 depression in freezing point of water with 0.1 kPa ice adhesion was observed on prepared
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53 coating.110
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Figure 11. A) (a) Structure of POSS-PDMAEMA-b-PSBMA. (b) Antifogging/anti-icing
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35 performance of amphiphilic coatings containing POSS-PDMAEMA-b-PSBMA along with a
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37 cross-linked PEGDMA network. Reproduced with permission 107
Copyright, 2017 American
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39 Chemical Society. B) Proposed mechanisms responsible for low ice adhesion on two distinct
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42 types of surfaces: (a) Reduction of van der Waal’s interaction between ice and hydrophobic
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44 surface due to increased thickness (D) of the water depletion layer (b) Reduction of ice adhesion
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46 strength due to the presence of non-frozen quasiliquid-layer (QLL) lubricant on PDMS+PDMS-
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49 PEG surface. Reproduced with permission 108 Copyright 2017 American Chemical Society C) (a-
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51 b) Ice propagation mechanisms on hydrophilic PMETA-Cl and hydrophobic PMETA-PFO brush
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53 surfaces Reproduced with permission.109 Copyright 2017, Royal Society of Chemistry.
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3 4.5. ANTI-FREEZING PROTEINS.
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Anti-freezing proteins are capable to adsorb on ice surface to inhibit its further growth and delay
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9 the freezing time by lowering the temperature at which ice growth occurs.111,112 Anti-freezing
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11 proteins consist of two types, the antifreeze glycoproteins (AFGPs) and the antifreeze proteins
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13 (AFPs). The AFGPs are made of a tri-peptide repeating unit as shown in Figure 12 A but AFPs
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16 have different size and structures. These unique compounds survive the organisms below zero
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18 temperatures by inhibiting the ice growth.113
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21 4.5.1. MECHANISM ACTION OF AFPs. The mechanism by which biological antifreeze adsorb
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to ice crystal and inhibit its further growth has been discussed with great interest in last decade.
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26 Knight et al. considered the biological ‘antifreeze’ as solutes that stick to the ice crystals in
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28 super-cooled water and inhibit their further growth.114 Generally accepted adsorption-inhibition
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30 mechanism explain the phenomenon of ice growth in presence of AF(G)Ps. The round flat
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33 crystals are produced due to the adsorption of AF(G)Ps in the ice plane but the curvature of the
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35 crystals remain unaffected without AF(G)Ps. This increase in surface curvature resulted, increase
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37 in vapor pressure and decrease in melting point of water molecules.115 AFPs are also useful in
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inhibiting the accumulation of ice particles in engineering applications. Grandum et al. inhibited
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42 the accumulation of ice particles by adding 5 mg/ml AFP to ice slurries. The ice slurries
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44 containing AFP flowed in a pipe almost similar to that of liquid water.116 Zhang et al. designed
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twelve amino acid peptides as antifreeze protein mimetic to observe its antifreeze activity.
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49 According to the adsorption-inhibition mechanism, the antifreeze protein mimetic adsorbed to
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51 the surface of ice crystal and produced micro-curvatures on the surface of ice crystals which
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53 resulted in depression of freezing point due to Kelvin effect.117
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6 Gwak et al. observed delay in ice formation on Al metal by fusing Al-binding peptide with
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8 Chaetoceros neogracile (Cn-AFP) as shown in Figure 12B. Cn-AFP-coated Al showed the
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10 inhibition of ice growth and lowering in freezing point due to the thermal hysteresis of Cn-AFP.
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In addition, trehalose coating of Cn-AFP-Al delayed the denaturation of AFP on aluminum with
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15 no effect on its anti-freezing property. This trehalose-fortified AFP coating method is applied to
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17 different metals especially in aircraft industry.118 Liu et al prepared an anti-icing coating with
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ice-binding face (IBF) and the non-ice-binding face (NIBF) of anti-freezing protein by
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22 incorporating the AFPs from Microdera punctipennis dzungarica beetle into polydopamine
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24 (PDA) and (3-glycidoxypropyl)methyldimethoxysilane (GOPTS) as shown in Figure12C. They
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26 confirmed that the IBF can facilitate ice nucleation and NIBF can depress ice nucleation on
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29 silicon substrate. As shown in Figure 12(D-E) that ice nucleation occurred on non-ice-binding
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31 face NIBF surface and IBF surface at 2254 sec and 8 sec respectively.119 Meister et al found the
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33 presence of ice-like water layers at the ice-binding site of the protein in aqueous solution at
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temperatures above the freezing point. They observed the increase in the amount of ice-like
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38 water at low temperature of the protein (0 °C to -2 °C) and suggested that the ordered ice-like
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40 water layers along with protein also play their role for the recognition and binding to ice.120 Anti-
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freezing proteins are not always fit for practical applications due to their high price, toxic in
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45 nature, isolation and purification problems.121 The polyampholytes with positive and negative
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47 charge groups on a single chain are known as good anti-freezing protein analogs. Recently, He et
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49 al. studied the behavior of heterogeneous ice nucleation on different ion-modified poly(butylene
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52 succinate) (PBS) surfaces. Inspired by anti-freezing proteins, the author produced various PBS-
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54 based polyampholyte coatings with1:1ratio of -NH2 to -COOH groups. The PBS-based
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3 polyampholyte coatings showed a large inhibition of ice nucleation and freezing delay on various
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6 substrates. Moreover, the polyampholytes PBS-CN28 (carboxyl and amino groups ratio) surface
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8 showed higher ice nucleation inhibition efficiency than the coatings of self-assembled
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10 monomers, polymer brushes, and polyelectrolyte multilayers, revealed its performance near to
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anti-freezing proteins in inhibiting the ice nucleation as shown in Figure 12F.122
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Figure 12. A) (a) Chemical structure of anti-freezing glycoproteins (AFGPs) B) Secondary
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49 trehalose coating of ABP-Cn-AFPG on Al plate. Reproduced with permission.118 Copyright
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51 2015, Nature. C) Diagram of antifreeze proteins from an insect (Microdera punctipennis
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53 dzungarica) and selectively tethered MpdAFPs on the PDA and GOPTS surfaces. D-E) Delay in
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56 freezing time (D) on the NIBF surface than that of PDA surface (E) on the IBF surface than that
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3 of GOPTS surface. Reproduced with permission.119 Copyright 2016, Nature. F) Thermal
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6 hysteresis comparison on PBS-CN28 with different antifreeze proteins and other materials based
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8 on different surface modifying strategies. Reproduced with permission. Copyright 2017,122
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10 American Chemical Society.
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13 4.6. ORGANOGELS. Generally, the organogels are semisolids in which an adequate amount of
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16 organic liquid is infused in the cross-linked network, which act as a reservoir to sustain the
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18 durability of surface.123 Yao et al. described the switching of water adhesion on n-paraffin
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20 swollen PDMS elastomer due to the phase change property of n-paraffin. At T > Tm (melting
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23 temperature of n-paraffin) the PDMS surface showed low-adhesion with water drop owing to the
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25 attraction between liquid paraffin and PDMS. Whereas, at T < Tm, paraffin became the part of
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27 the solid surface due to its solidification and caused to rough the gel surface which resulted in
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high water adhesion (i.e Wenzel state). The increase in the viscosity of paraffin near the melting
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32 temperature also affected the mobility of drops.124 Wang et al. synthesized a durable organogel
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34 anti-icing coating by swelling cross-linked PDMS network with liquid paraffin (LP). The
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36 swelled PDMS showed very low ice adhesion strength 1.7 ± 1.2 kPa compared to flat PDMS
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39 146.3 ± 9.3 kPa. The LP swelled phenyl silicone and butyl rubber also showed 60 and 20 times
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41 reduction in ice adhesion strength compared to their dry polymers. The author also found the LP
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43 swelled organogel maintained the ice adhesion strength 0.7 kPa at -60°C.125 The same author also
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46 revealed the durable ice-phobic surface of solid organogel due to the regenerability of the
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48 sacrificial alkane layer as shown in Figure 13. The icephobic property did not fade after
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50 sandpaper abrasions and twenty icing/deicing cycles.
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53 In addition, the durable solid organogel surface showed no change in its icephobic property
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56 during 100-day storage because the material of the surface neither evaporated nor contaminated
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58 34
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3 by other surfaces.126 Therefore, the infused liquids can be replaced with solid regenerable
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6 sacrificial layers. Golovin et al. suggested the insertion of small miscible polymeric chains to
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8 induce lubricating layers and interfacial slippage at the interface. The author obtained ultra-low
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10 ice adhesion (0.15 kPa) organogels by changing the crosslink density of PDMS.127 The same
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author also designed more than a hundred icephobic surfaces and built a framework to predict
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15 the ice adhesion strength of icephobic polymers. Organogels are preferred due to their ultra-low
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17 ice adhesion and durability.128 Han et al. prepared a durable anti-freezing and anti-heating
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hydrogel by UV-initiated copolymerization of acrylamide with acrylic acid in a binary solvent
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22 (glycerol-water). Polydopamine-CNTs were incorporated as nano-reinforcements to induce
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24 conductivity and strength to the hydrogel.129
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39 Figure 13. Schematic illustration of the principle of solid organogel materials for the easy
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41 removal of foreign materials atop and the mechanism for the regeneration of the solid alkane
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43 layer. Reproduced with permission.126 Copyright 2017, Wiley.
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46 5. SMART AND STIMULI-RESPONSIVE ICEPHOBIC SURFACES
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The smart and stimuli-responsive icephobic surfaces130 are desirable in extreme environment;
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52 such surfaces can be obtained by using the stimuli-responsive materials having both passive anti-
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54 icing and active deicing functions. Therefore, it is need of the hour to use temperature, light131,
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3 pH and humidity responsive materials to achieve the active deicing application. Ramachandran
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6 et al. examined the roughness and wetting properties of thermo-genic plant skunk cabbage due to
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8 its ability to melt snow. They developed a heat transfer model to observe icephobic performance.
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10 The heat produced by the plant maintained a thin water layer and air pockets between ice and the
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leaf surface. This helped to slip off the ice easily due to its own weight.132 Recently Karim et al
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15 made glass fibre roving and coated with conductive ink of graphene for de-icing applications.
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17 The conductive glass fibre roving was also combined with epoxy composites by knitting to heat
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them with desired temperature as shown in Figure 14 A. They dipped the conductive epoxy
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22 composite into an ice-bucket to observe its deicing ability with the increase of temperature. The
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24 temperature of bucket having only ice remained same after half an hour but the bucket with
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26 conductive graphene composite showed -0.1 °C to 28 °C increase in temperature within five
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29 minute and removed the ice from coated surface as shown in Figure 14 B.133
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35 Figure 14. A) Schematic diagram for synthesis of graphene-based glass/epoxy composites for
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37 de-icing applications. B) (a) Change in temperature on graphene-based glass composite at
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39 different voltages (b) the comparative change in temperature of only ice bucket without coating
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and the ice bucket containing graphene composite. (c) Before heating: (i) ice bucket without
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44 coating (ii) ice bucket with graphene coating (d) after heating at 10 V: (i) ice remained same in
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46 the bucket without coating (ii) melting of ice due to joule heating of graphene-based coating.
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48 Reproduced with permission133. Copyright 2018, Royal Society of Chemistry.
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52
Yin et al. fabricated a photo-thermal responsive icephobic film by filling the polystyrene
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54 microspheres template with PDMS-Fe3O4. The porous film was infiltrated with
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56 perfluoropolyether lubricants after the removal of the template as shown in the Figure 15. The
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3 uniformly dispersed magnetic Fe3O4 nanoparticles imparted thermogenesis deicing capability to
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6 the film by converting the optical energy of a NIR laser into thermal energy.134
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40 Figure 15. Schematic diagram for the fabrication of photothermal icephobic film. Reproduced
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42 with permission.134 Copyright 2017, Wiley.
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45 Urata et al. also developed thermo-responsive, transparent, self-lubricating organogels (SLUGs)
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47 by using crosslinked PDMS with organic liquids. The author controlled the syneresis rate from
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50 the gel matrices by changing the ratio of PDMS with organic liquids. The SLUGs showed 0.4
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52 kPa adhesion force with ice and ice pillars formed on SLUGs easily slide off by small tilting as
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54 shown in Figure 16 A.135 Cheng et al. also reported thermo-responsive superhydrophobic de-
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3 icing coating of fluorinated magnetic nanocomposite.136 Raji et al. used conductive composites
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6 of epoxy filled with graphene nano-ribbon for de-icing applications. The author delivered 0.5
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8 W/cm2 power density to remove 14 g of ice from the rotor of a helicopter at -20 °C.137 Chen et
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10 al. also showed 70% better de-icing performance of graphene coating due to its thermal
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conductivity and reduced the consumption of energy on helicopter rotor.138 Wang et al. prepared
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15 a superhydrophobic perfluorododecylated graphene nanoribbon film by a spray-coating method
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17 to inhibit the freezing of super-cold water at -14 °C and the heat of applied voltage caused to de-
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ice the film below -14 °C. The prepared superhydrophobic anti-icing film was switched into the
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22 slippery de-icing mode after spraying the lubricant as shown in Figure 16 B.139 Valentini et al.
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24 prepared the rubber composites by introducing thermally reduced graphene oxide and
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26 multiwalled carbon nanotubes for low ice adhesion surface.140 Hazarika et al. used in situ method
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29 without catalyst and solvent to fabricate an anti-icing and antifogging waterborne polyester-CD
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31 TiO2 nanocomposite.141 Bao et al. used molecular dynamic simulations to prove a low ice
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33 adhesion strength on single-walled carbon nanotube array (CNTA) surface and found a linear
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relationship between the ice detachment stress and interaction energy of oxygen-carbon on
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38 CNTA.142 Chen et al. developed the photo and pH-responsive self-healing water-based
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40 superhydrophobic anti-icing coatings by using emulsion polymerization of styrene, 2-(N,N-
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diethylamino)ethyl methacrylate, divinylbenzene and perfluorooctyltriethoxysilane with TiO2
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45 nanoparticles as shown in Figure 16 C.143 Zhu et al. observed delay in freezing point of water on
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47 phase-change microcapsules with vulcanized silicone rubber coating due to the release of latent
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49 heat from the microcapsules at low temperature.144 Sun et al. fabricated the bilayer epidermis-
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52 dermis coating by spraying superhydrophobic hydro beads onto a nylon membrane and
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54 underlying dermis was infused with propylene glycol. The outer superhydrophobic layer worked
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3 as anti-icing to roll off the water droplets. However, when superhydrophobic surface was
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6 covered with ice due to condensation frosting, the designed coating reacted (stimuli-responsive)
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8 by releasing the stored antifreeze liquid to inhibit the formation of ice for a long time and
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10 showed thermal deicing with increase in sample temperature as shown in Figure 16 D.145
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A B
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39 Figure 16 A) Petri dishes with thermo-responsive icephobic organogels. (a) Formation of ice
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41 pillar on horizontal surface at -15 °C and after tilting at 20. Reproduced with permission135
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43 Copyright 2015 Royal Society of Chemistry. B) Schematic diagrams for the fabrication of
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46 perfluorododecylated graphene films. Reproduced with permission.139 Copyright 2016,
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48 American Chemical Society. C) Schematic diagrams for the fabrication of self-repairing
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50 waterborne superhydrophobic coatings. Reproduced with permission.143 Copyright 2017 Royal
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Society of Chemistry D) Schematic diagram of the bilayer architecture of a poison dart frog skin
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55 with secretion of antifreeze liquid due to stimuli-response. The porous SHB epidermis separates
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3 the antifreeze infused dermis from the environment b) Secretion of antifreeze liquid through the
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6 pores in response to contact with ice or frost, which results in melting of ice. Reproduced with
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8 permission.145 Copyright 2015, Wiley.
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11 6. SUMMARY AND FUTURE PERSPECTIVES
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14 The possible icephobic strategies and materials with superwettability along with their design
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principles and mechanism are classified into different sections. On the basis of wettability and
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19 nucleation theories the fundamental characterization parameters for icephobic surfaces i.e low
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21 CAH, high receding contact angles, low water adhesion force, promoting homogeneous
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nucleation at high nucleation energy, high inhomogeneity and less stability at the interface of
24
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26 ice-substrate are discussed. The superhydrophobic surfaces are described for their short contact
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28 time with small radius of water droplet and thermodynamically delay in freezing point of water.
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30 The poor anti-icing efficiency of the superhydrophobic surface is mentioned due to the
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33 accumulation of super-cooled micro droplets and pinning of contact line at the interface. The
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35 springboard effect is explained by elastomers to impart icephobic behavior. The elimination of
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37 possible ice nucleation sites due to the homogeneous interface of the SLIPS coating and delay in
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freezing time on the SLIPS is also discussed. The non-freezable water (responsible to prevent
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42 water from freezing) make hydrogen bonding with the hydrophilic groups of SLIPSs (aqueous
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44 lubricating layer), amphiphilic and anti-freezing protein is debated. The organogels are discussed
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46
due to their extremely low ice adhesion strength and finally the stimuli-responsive materials are
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49 highlighted for active anti-icing purpose. Future trends in icephobic surfaces may see by
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51 approaching homogeneous nucleation (suppress ice nucleation up to -25 °C) through surface
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53 nanotexturing with radius of curvature less than 10 times the critical nuclei size. The soft
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56 materials with suitable roughening, is also a promising approach to make icephobic surfaces due
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58 41
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3 to their excellent water and ice repellency under harsh conditions. Future work should also focus
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6 on self-healing, stimuli-responsive smart icephobic surfaces by using the materials having both
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8 passive anti-icing and active deicing functions.
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10
11 AUTHOR INFORMATION
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Corresponding Authors
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14 *E-mail: qhzhang@zju.edu.cn (Q.Z.).
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16 ACKNOWLEDGMENTS
17 This work was supported by the National Natural Science Foundation of China (No. 21576236,
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19
21676248 and 21878267).
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21
22
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Icephobic Strategies and Materials With Superwettability: Design Principles and Mechanism

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