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Applied Surface Science 331 (2015) 132–139

Contents lists available at ScienceDirect

Applied Surface Science

journa l h om epa ge: www.elsev ier .com/ locate /apsusc

abrication and anti-icing property of coral-like superhydrophobicluminum surface

hiping Zuoa,∗, Ruijin Liaoa, Chao Guoa, Yuan Yuanb, Xuetong Zhaoa, Aoyun Zhuanga,iYi Zhanga

State Key Laboratory of Power Transmission Equipment & System Security and New Technology, Chongqing University, Chongqing 400044, ChinaCollege of Materials Science and Engineering, Chongqing University, Chongqing 400044, China

r t i c l e i n f o

rticle history:eceived 22 October 2014eceived in revised form0 December 2014ccepted 11 January 2015vailable online 20 January 2015

a b s t r a c t

Aluminum is one of the most widely used metals in transmission lines. Accumulation of ice on aluminummay cause serious consequences such as tower collapse and power failure. Here we develop a methodto fabricate a coral-like superhydrophobic surface to improve its anti-icing performance via chemicaletching and hot-water treatment. The as-prepared surface exhibited superhydrophobicity with a contactangle (CA) of 164.8 ± 1.1◦ and the sliding angle smaller than 1◦. The static and dynamic anti-icing behaviorsof the superhydrophobic surface in different conditions were systematically investigated using a self-

eywords:luminumoral-likeot-water treatmentnti-icing property

made device and artificial climate laboratory. Results show that the coral-like superhydrophobic structuredisplayed excellent anti-icing property. The water droplet remained unfrozen on the as-prepared surfaceat −6 ◦C for over 110 min. 71% of the surface was free of ice when exposed in “glaze ice” for 30 min.This investigation proposed a new way to design an anti-icing surface which may have potential futureapplications in transmission lines against ice accumulation.

laze ice

. Introduction

Aluminum is the most abundant metal on earth and widelysed in mechanical apparatus, aerospace and overhead power

ines. Accumulation of ice on transmission lines can cause a dras-ic decrease in mechanical and electrical performance leading toerious problems such as collapse of tower, flashovers of insulatortrings, galloping of conductors and consequent power outages [1].lectrical power outages due to icing have been widely reported inany countries such as the United States, England, Canada, Norway

nd China [2–5]. Thus, research on improving the anti-icing behav-or of transmission lines is of great significance for the whole world.

The traditional methods to remove ice include manual deic-ng method, mechanical deicing method, thermal deicing methodnd so forth. However, these traditional methods involve problemsuch as time consuming, low efficiency and equipment damage.uperhydrophobic surface has attracted much attention because ofts special functions such as self-cleaning, water-repellency, anti-

orrosion and anti-icing [6–12]. Therefore, it is believed to be theotential way to realize anti-icing.

∗ Corresponding author: Tel.:+8613452325921.E-mail address: zpzuo@sina.com (Z. Zuo).

ttp://dx.doi.org/10.1016/j.apsusc.2015.01.066169-4332/© 2015 Elsevier B.V. All rights reserved.

© 2015 Elsevier B.V. All rights reserved.

The general method to fabricate a superhydrophobic surfaceinvolves two steps, namely, the construction of rough structuresand chemical modification with low-surface-energy materials[13–16]. Inspired by the lotus effect that the water droplet on theleaves can easily roll off without any contamination, many devel-oped methods have been reported such as solution-phase approach[17,18], chemical etching method [19,20], sol-gel method [21,22],vapor deposition [23], anodic oxidation [24,25], electrochemicaletching methods [26] and so forth. To date, some researchershave attempted to fabricate superhydrophobic aluminum surface[27–33]. However, few studies have focused on treating aluminumto improve its anti-icing property such as reducing the ice adhe-sion strength [20,34], delaying the ice formation [35], enhancingthe dynamic anti-icing behavior of water droplets impacting theSHP surface [36] and so forth. Apart from superhydrophobic sur-face, slippery liquid-infused porous surface (SLIPS) was introducedby Aizenberg et al. [37–40]. Nevertheless, ice is prone to accumu-late on Al and its alloy in tough freezing weather. To overcome thisbottleneck, we attempted to fabricate superhydrophobic surfaceswith excellent anti-icing property. Moreover, to the best of ourknowledge, studies about the icing process of superhydrophobic

aluminum and anti-icing property of the superhydrophobic surfacein “glaze ice” still remain relatively scarce.

In this work, a method to fabricate a coral-like superhydropho-bic surface on aluminum foil was investigated. CuCl2 solution

Z. Zuo et al. / Applied Surface Science 331 (2015) 132–139 133

ergy m

wsstsaipda

2

2

(N

2

wdCi5ca

2

Mdawa

Fig. 1. Water CAs on bare aluminum surface modified with low-surface-en

as used to etch the sanded aluminum surface and form micro-tructures, and hot-water treatment was adopted to generate aurface with micro/nano binary roughness. The fabrication, charac-erization, and evaluation of anti-icing behavior of the as-prepareduperhydrophobic aluminum surface were given. The dynamicnti-icing behavior of the as-prepared aluminum surface in glazece was demonstrated under an artificial climate laboratory. Theresent study, hopefully, could help to provide a new strategy toesign a structured anti-icing surface and favor the potential futurepplications of aluminum in anti-icing area.

. Experimental

.1. Materials

A 30 mm × 50 mm × 5 mm aluminum foil (1060 Al), CuCl2·2H2O99%, Shanghai Kechuang Chemicals Co. Ltd), emery paper No. 400,o. 600 and No.1000 were used in this study.

.2. Sample preparation

Aluminum foil was first sanded using emery paper, and thenashed with ethanol followed by distilled water and subsequentlyried. The clean aluminum foil was immersed in the 1 mol/LuCl2 solution for 8 s, ultrasonically cleaned, and dipped upright

n hot water at 90 ◦C with a temperature-controlled hot plate for0 min. Finally, the etched foil was modified with 2 wt.% hexade-yltrimethoxy silane for 60 min at ambient temperature and heatedt 90 ◦C for 30 min.

.3. Sample characterization

The CA and sliding angle were measured using a CA meter (Dropeter A-100, China) with an image and video capture system. Five

ifferent spots for one sample were measured each time and theverage value was adopted as the CA. The water volume usedas 8 �L. The ambient temperature was measured at 25.3 ± 2 ◦C

nd relative humidity was at 48 ± 10%. The crystal structure and

aterials (a,b) and as-prepared superhydrophobic aluminum surface (c,d).

surface morphology of the as-prepared samples were character-ized by X-ray diffraction (XRD; Panalytical Empyrea, Netherlands)and scanning electron microscopy/energy dispersive spectrometer(SEM/EDS; Tescan Vega3, Czech Republic), respectively.

3. Results and discussion

3.1. Wettability

The wettability of the aluminum surface was measured by con-tact angle meter at ambient temperature (25.3 ± 2 ◦C) and relativehumidity (48 ± 10%). The bare aluminum foil modified with low-surface-energy materials exhibited a CA of 103.6 ± 1.7◦ as shownin Fig. 1a, whereas the as-prepared aluminum surface exhibitedsuperhydrophobicity with a CA of 164.8 ± 1.1◦. The as-preparedsurface also shows a considerable superhydrophobic propertyon various volumes of water droplets (Fig. 1d). The relationshipbetween surface wettability at heterogeneous surfaces was pro-posed by Cassie and Baxter’s [41,42] such as the equation:

cos �� = f1 cos � − f2 = cos � − f2(cos � + 1) (1)

where f1 and f2 are the fractions of aluminum solid surface andair in composite surface and f1 + f2 = 1. �� and � are CAs on roughaluminum foil and the bare surface, respectively. The f2 value of themicro- and nano- structure was estimated to be 0.9543. The lowvalue of f1 indicates that only about 4.57% of the water surface is incontact with the aluminum surface. Except for water contact angle,the superhydrophobic surface should also have a sliding angle lessthan 10◦. The water droplet would be pinned on the surface withhigh sliding angle and cannot slide easily [41,43]. The as-preparedaluminum surface has a low sliding angle less than 1◦ for a dropletof 8 �L (Supplementary Video.1). The droplet can easily roll off thesurface by slightly tilting the sample.

3.2. Surface morphology

Fig. 2 shows the SEM images of bare aluminum and as-preparedsuperhydrophobic surfaces at different magnifications. The

134 Z. Zuo et al. / Applied Surface Science 331 (2015) 132–139

F ydrop

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tts(bstdt

2

2

bwi

ig. 2. SEM images of the sanded aluminum surface (a) and the as-prepared superh

urfaces are relatively smooth after sanding, as shown in Fig. 2a.he as-prepared superhydrophobic surface is rather rough and isovered with many micro particles and pits (Fig. 2b). The result inig. 2c further indicates that many coral-like structures formed inhe superhydrophobic surface. It was found that the corals werepproximately several micrometers in length and none-uniformistributed on the surface. Some corals grow diagonally and otherrow in the direction normal to the aluminum substrate. Theurface of each coral seems rough indicating the formation ofano-structures. To examine further the morphology of the corals,igh magnification SEM image (Fig. 2d) was obtained. Fig. 2devealed the corals were covered with hundreds of petal-likeanosheets. The nanosheets were slightly curved and about sev-ral hundreds of nanometers in length and tens of nanometers inidth. It is evident that the nanosheets were densely packed on

he surface and relatively uniform in size.The general mechanism of the formation of micro-nano struc-

ures can be described as Fig. 3. After sanding, the oxide layer ofhe aluminum surface was moved off. When etching in the CuCl2olution, the substitution reaction occurs as shown in Eqs. (2) and3). Moreover, the presence of H2 bubbles prevented Cu depositionecause of the absence of Cu2+, leading to the micrometer-scaleurface roughness. Large numbers of grain boundaries and disloca-ion exist in common polycrystalline. These areas are prone to beissolved due to their relatively high surface energy, which leadso the generation of the deep ravines.

Al + 3Cu2+ → 2Al3+ + 3Cu (2)

Al + 6H+ → 2Al3+ + 3H2 ↑ (3)

Alwitt et al. [44] reported that pseudoboehmite oxide film coulde grown on aluminum at temperature ranging from 50 ◦C to 100 ◦Chere the film growth process was defined in three stages includ-

ng an incubation period (1–2 s), a period of rapid growth and

hobic aluminum surface at 1000× (b), 5000× (c), 50000× (d) magnifications.

followed by a slow growth stage after the first few minutes ofimmersion. The detailed mechanism of formation of this nanoscaleroughness remains unclear. It is believed that the reaction startswith the dissolution of aluminum and is followed by the depositionof hydroxide colloidal particles to form hierarchical porous struc-tures [45]. Both the immersion time and temperature affected theformation processes. The reaction between Al and H2O at the initialstage can be described in Eq. (4) [45,46]. Moreover, the generatedAl2O3·xH2O can react with H2O further to form AlO(OH) [47,48].It can be clearly concluded that the micro-nano-binary structurescan trap a large amount of air, which can prevent the penetrationof the water into the grooves and also bestow superhydrophobicityon the surfaces.

Al + H2O → Al2O3 · xH2O + H2 ↑ (4)

3.3. Chemical composition

EDS is used to analyze chemical composition of the as-preparedsurface. In Fig. 4a, the EDS spectrum shows no other peaks apartfrom Al. It was suggested that the oxides were completely removedfrom the aluminum surface in the sanding process. The EDS spec-trum of as prepared superhydrophobic aluminum surface in Fig. 4breveals the presence of C, O, Al and Si. The appearance of Si andC indicates that the silane film has successfully attached to thealuminum surface after modification. XRD is used to further ana-lyze the as-prepared superhydrophobic surface as shown in Fig. 5.Three diffraction peaks of the etched Al surfaces are found andassigned to the Al(200), Al(220) and Al(311) planes of Al (JCPDSCard No. 04-0787). Small peaks corresponding to AlO(OH) were

also observed for the treated aluminum which confirms the con-version of a small amount of Al to AlO(OH) crystals. From theresults of the EDS and XRD, it was considered that the success-ful attachment of the hexadecyltrimethoxy silane to the surface.

Z. Zuo et al. / Applied Surface Science 331 (2015) 132–139 135

Fig. 3. Schematic illustration of fabrication micro-nano binary structures on aluminum.

um (a

ThatmSpbapi

3

td(said

Fb

Fig. 4. The EDS images of the sanded alumin

he aluminum surface etched by CuCl2 solution and modified withexadecyltrimethoxy silane exhibited a CA of 154◦ and slidingngle of 19◦ (Supplementary Fig. S1). It was found that most ofhe aluminum surface (prepared by using CuCl2 etching and silane

odification) was covered with microscale particles and pits (Fig.1a). Nevertheless, after adding hot-water treatment, hundreds ofetal-like nanosheets formed on the as-prepared superhydropho-ic aluminum surface whose CA increased up to 164.8◦ and slidingngle decreased down to 1◦ as shown in Figs. 1 and 2. Thus, theresence of Al and minimal amount of AlO(OH) may play a key role

n structuring the superhydrophobic surface.

.4. Anti-icing effect

Ice would accumulate on the metal surfaces when exposed toough weather. In this study, the anti-icing property of the superhy-rophobic aluminum surfaces was investigated. A self-made deviceSupplemental Fig. S3) is used to simulate the freezing weather. The

ample temperature was set at −6 ◦C. The ambient temperature wast 17.6 ± 2 ◦C and relative humidity was at 53 ± 10%. The static anti-cing behavior of water droplets on aluminum was investigated byropping six water droplets on the surface each time.

ig. 5. The XRD image of the sanded aluminum and the as-prepared superhydropho-ic aluminum surface.

) and the as-prepared aluminum surface (b).

Fig. 6 is the freezing process of water droplets on bare alu-minum surface and superhydrophobic surface. The water turns intoice when it becomes opaque. The first two water droplets on thebare aluminum surface became ice in 107 s, and all of the waterdroplets froze in 187 s. The bare aluminum surface covered witha thick layer of frost changed from shiny to white surface within107 s. However, no evident frost was found on the superhydropho-bic aluminum surface during the first 10 min, after which, the frostbegan to grow from the edges towards the center. Most of the super-hydrophobic surface remained free of frost in 110 min. The averagedelayed freezing time of six water droplets is 150 min and the lastwater droplet in the center of the surface did not freeze until thefrost covered the surface at 207 min which is much longer thanthe previous report [49] and the aluminum surface prepared byCuCl2 etching and hexadecyltrimethoxy silane modification (Fig.S2). The frost contacting the droplet would act as crystallizationnucleus which accelerates its freezing process. It is interesting thatsome small droplets appeared on the surface at 30 min and mostof the surface was covered with new droplets of various volumesin 70 min, which is quite different from the bare aluminum sur-face. Although the as-prepared surface could not completely getrid of the frost, it still showed evidently anti-frost and delay-icingproperty comparing with the bare aluminum. In addition, a spe-cial camera was applied to investigate the formation of new tinywater droplets. The self-transfer phenomenon was clearly shownin Fig. 7. Two tiny water droplets were aggregated into a big droplet.This phenomenon demonstrates that the as-prepared surface canmaintain good dynamic performance even at −6 ◦C. The time forthe droplets to freeze can be expressed as [50,51]

�t ∝ �wCP(T0 − TS)�h

(5)

where �w and CP are the density and heat capacity of pure water,respectively, T0 is the initial temperature, TS is the temperature of

the surface, and �h is the heat loss per unit time. The heat that thedroplet loses per unit time can be expressed as �h = hl + hl′ − hg −hg′ , where, hl and hg are the heat lost and gained through contactheat conduction per unit time, and hl′ and hg′ are the heat lost and

136 Z. Zuo et al. / Applied Surface Science 331 (2015) 132–139

re alu

gsmhwti

tfwsds

Fig. 6. Freezing process of water droplets on ba

ained through thermal radiation per unit time. Due to the effect ofolid–liquid–air interface, the as-prepared superhydrophobic alu-inum surface has the lower solid–liquid contact area (4.57%), less

eat will be transferred from the water droplet to the solid surface,hich results in longer delaying time for icing. The self-transfer of

he tiny droplets can sweep away the smaller ones and effectivelynhibit the formation of frost.

In the previous report [52], when water condensed on the ver-ical nano-needles, a narrow gap can produce a higher Laplaceorce for water in Wenzel state. The force will make the condensedater move out automatically, and therefore change the Wenzel

tate into Cassie state. The surface of corals was covered with aense layer of petal-like nanosheets, which is probably the rea-on for the appearance of tiny water droplet on the as-prepared

Fig. 7. The images showing the self-transf

minum surface and superhydrophobic surface.

superhydrophobic surface. The nano-scale roughness minimizesthe nucleation density of condensate and enables the majority ofnucleating condensate to grow over the roughness in the ener-getically favorable Cassie state before coalescing with other drops[53–55]. Due to the release of the total surface energy, the self-transfer phenomenon happens on the superhydrophobic surface[56,57]. The self-transfer phenomenon can sweep the as-preparedsurface clean and dry, thus effectively inhibited the inward frostcrystal propagation on the micro-nano binary structures by delay-ing the ice-bridging process [58] (Supplementary Fig. S4). The waterin Cassie state presents a perfect sphere, and the reduction of sur-

face energy is the biggest, so they get a larger kinetic energy forself-transfer. Based on the self-propelled movement of the con-densed microdrops and evaporation-induced gaps between frozen

er of the superhydrophobic surface.

Z. Zuo et al. / Applied Surface Science 331 (2015) 132–139 137

Fcs

dastpa

swsei3stptit3bcpawfobitahel

3

spa

ig. 8. The description of the artificial climate laboratory:(a) layout of the artificiallimate laboratory. (b) The inner schematic of the artificial climate laboratory toimulate glaze ice.

roplets and condensed microdrops [58,59], the frost crystals prop-gate inwardly at a slow rate. The as-prepared surface maintainsuperhydrophobicity at −6 ◦C, and the possibility of self-transfer isherefore greater than bare aluminum surface. As a result, the as-repared superhydrophobic surface demonstrated a better staticnti-icing property.

Both the field investigations and the laboratory investigationshow that the glaze ice is the most dangerous type of ice associatedith the highest probability of flashover in transmission lines [1],

o in this paper, “glaze ice” was simulated and the anti-icing prop-rty of the as-prepared superhydrophobic surface was investigatedn the artificial climate laboratory as shown in Fig. 8a. Water at

± 1 ◦C was sprayed onto the aluminum surface about 10 L/h. Theize of spraying water was about 100 �m and the inner ambientemperature was at −5 ± 1 ◦C. Both the tilting angle of the sam-le about 60◦ and the size of spraying water were smaller thanhe previous report [60], which can better demonstrate the anti-cing behavior of the as-prepared superhydrophobic surface underough snowy weather. Fig. 9 shows entire icing process within a0-min duration. Evidently, water droplets quickly adhered to theare aluminum surface in 10 min, and a relatively thick layer of iceovered the entire aluminum surface at 30 min. Conversely, the as-repared surface kept dry and clean during the first 20 min, andbout 71% of the whole surface still remained unfrozen at 30 min,hich is larger than that of reported results in Ref. [60]. It was

ound that only a small amount of ice accumulated at the bottomf the superhydrophobic surface. The thickness of the ice on theare aluminum is larger than that of the as-prepared surface. The

ce on the as-prepared superhydrophobic surface was 2.3 g (37% ofhe bare aluminum foil’s), indicating the effective inhibition of iceccumulation by superhydrophobic surface. Although the super-ydrophobic surface cannot completely prevent ice, it still exhibitsvident anti-icing property and can effectively reduce the accumu-ation of ice.

.5. Stability

To evaluate the mechanical stability of the as-prepareduperhydrophobic surface, abrasion tests were conducted (Sup-lemental Fig. S5). Firstly, shear abrasion test was conductedccording to literatures process [18,61]. The superhydrophobic

Fig. 9. The freezing process of superhydrophobic aluminum surface (left) and barealuminum surface (right) in glaze ice.

aluminum surface subjected to a normal pressure (∼5 kPa) slid ona common cotton fabric (40s × 40s) by 25 cm in one direction. Afterthe abrasion test, the CA decreased down to 152.7 ± 1.9◦. Sandgrains (8 g, 80–200 �m in diameter) were dropped onto the tiltedsample from a height of 30 cm [62,63]. After sand-impact abrasion,the SHP surface still exhibited superhydrophobicity with a CA of150.2 ± 2◦. These results demonstrate the considerable resistanceof mechanical abrasion.

4. Conclusion

The coral-like superhydrophobic surface is fabricated by chemi-cal etching and hot-water treatment in this paper. The as-preparedsurface exhibited a CA of 164.8 ± 1.1◦ and sliding angle less than 1◦.EDS and XRD images show that the as-prepared surface consistsmainly of Al and small amounts of AlO(OH). The as-prepared alu-minum surface can effectively reduce the accumulation of ice anddelay freezing process. The micro-nano binary structure designedis ideal for anti-icing property due to the following two aspects: on

one hand, the micro-nano binary structure can absorb more air andtherefore reduce the fraction of solid–liquid interface which slowsdown the heat transfer from the water droplet to the surface; on theother hand, the petal-like nanosheets on the corals can provide a

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arger Laplace force which moves the condensed water droplet outf the micro-nano textures. Due to the effect of the binary textures,he tiny droplets can move off the surface automatically and sweephe surface clean and dry. The present study, hopefully, opens aovel way to design structured surface to realize anti-icing, whichas a potential application on transmission lines in anti-icing area.

cknowledgments

We gratefully acknowledge the financial support from Nationalatural Science Foundation of P.R. China (project No. 51377177).

ppendix A. Supplementary data

Supplementary data associated with this article can beound, in the online version, at http://dx.doi.org/10.1016/j.apsusc.015.01.066.

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