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PSUSC-26494; No. of Pages 8

Applied Surface Science xxx (2013) xxx– xxx

Contents lists available at ScienceDirect

Applied Surface Science

j ourna l ho me page: www.elsev ier .com/ locate /apsusc

abrication of lotus-leaf-like superhydrophobic surfaces viai-based nano-composite electro-brush plating

ongtao Liu ∗, Xuemei Wang, Hongmin Jiollege of Materials Science and Engineering, China University of Mining and Technology, Xuzhou, Jiangsu 221116, China

r t i c l e i n f o

rticle history:eceived 16 September 2013eceived in revised form 3 October 2013ccepted 4 October 2013vailable online xxx

eywords:ano

a b s t r a c t

Superhydrophobic surface has become a research hot topic in recent years due to its excellent perfor-mance and wide application prospect. This paper investigates the method to fabricate superhydrophobicsurface on carbon steel substrate via two-layer nano-composite electro-brush plating and subsequentsurface modification with low free energy materials. The hydrophobic properties of as-prepared coatingswere characterized by a water sliding angle (SA) and a water contact angle (CA) measured by the Sur-face tension instrument. A Scanning electron microscope was used to analyze the surface structure ofplating coatings. Anti-corrosion performance of the superhydrophobic coating was characterized by a

omposite electro-brush platinguperhydrophobic surfaceotus-leaf-like

potentiodynamic polarization curve measured by the Electrochemical workstation. The research resultshows that: the superhydrophobic structure can be successfully prepared by plating nano-C/Ni and nano-Cu/Ni two-layer coating on carbon steel substrate under appropriate technology and has similarity withlotus-leaf-like micro/nano composite structure; the contact angle of the as-prepared superhydrophobiccoating can be up to 155.5◦, the sliding angle is 5◦; the coating has better anti-corrosion performancecompared with substrate.

. Introduction

Superhydrophobic surfaces have wide application prospect inany fields due to their excellent performance, such as Waterproof,

elf-cleaning, anti-icing, anti-corrosion, etc. [1–7]. The fabrica-ion and application of superhydrophobic surfaces are always theesearch hot topics. The most well-known superhydrophobic sur-aces are lotus leaves, they have excellent water repellency andelf-cleaning capability, this is due to their micro/nano scale rough-ess and the presence of a thin wax film on the leaf surface [8,9].here are two ways to fabricate superhydrophobic surfaces, one isanufacturing micro/nano scale roughness on the materials hav-

ng low surface free energy, the other is manufacturing micro/nanocale roughness on the higher surface free energy materials firstlynd then modifying the surface by low surface free energy materi-ls [10–13]. For smooth solid material, the contact angle can only bep to 120◦ even if it has the lowest surface free energy [14,15], so,he building of micro/nano scale roughness is the key to fabricateuperhydrophobic surfaces.

Please cite this article in press as: H. Liu, et al., Fabrication of lotus-leaf-like suplating, Appl. Surf. Sci. (2013), http://dx.doi.org/10.1016/j.apsusc.2013.10.0

So far, there are many methods to fabricate superhydropho-ic surfaces on metal substrate, including solution immersion [16],lectrochemical deposition [17–19], chemmical etchin [20], anodic

∗ Corresponding author. Tel.: +86 516 83591916; fax: +86 516 83591916.E-mail address: [email protected] (H. Liu).

169-4332/$ – see front matter © 2013 Elsevier B.V. All rights reserved.ttp://dx.doi.org/10.1016/j.apsusc.2013.10.030

© 2013 Elsevier B.V. All rights reserved.

oxidation process [21], chemical vapor deposition [2,22] and soon. But all of them have some deficiencies more or less, such astedious fabrication, high requirements for the equipment, limitsto large-scale production, low mechanical strength, which blocktheir practical application. Herein, we present a simple and flexiblenano-composite electro-brush plating method to create superhy-drophobic surfaces. The electro-brush plating technology is veryflexible and efficient, which can deposit different kinds of coatingsand prepare large-area coating, the binding force between coatingand substrate is strong and the required equipment is portable.Investigating the fabrication of lotus-leaf-like superhydrophobicsurfaces via Ni-based nano-composite electro-brush plating andthe anti-corrosion performance of the coatings has importantsignificance in the fabrication and practical application of super-hydrophobic surfaces.

2. Experiments

2.1. Materials

NaOH, Na3PO4, NaCl, NiCl2·6H2O, Na3C6H5O7·2H2O, H3C6H5O7,(NH4)2C2O4, NiSO4·6H2O, CH3COOH, HCl(30%), NiSO4·7H2O,

perhydrophobic surfaces via Ni-based nano-composite electro-brush30

NH3·H2O(25%–28%), (NH4)3C6H5O7, CH3COONH4, NaC12H25SO4,Additive X, Nano-C particles (spherical particle with smoothsurface, 35 nm), Nano-Cu particles (spherical particle with smoothsurface, 200 nm), Deionized water. All the materials cited above

dx.doi.org/10.1016/j.apsusc.2013.10.030


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Table 1Electrolytic cleaning solutions.

Chemical composition Content (g/L)

NaOH 25.0Na2CO3 21.7Na3PO4 50.0NaCI 2.4

Table 2No.2 activation solutions.


HCI 25.0NaCI 140.0

Table 3No. 3 activation solutions.


NiCl2·6H2O 3.0Na3C6H5O7·2H2O 142.2H3C6H5O7 94.2NaCl 0.1

Table 4Preplating solutions.


NiSO4·7H2O 400NiCl2·6H2O 20CH3COOH 68HCl (30%) 20

Table 5Nano-C/Ni composite plating solutions.

Chemical composition Content

NiSO4·6H2O 254 g/LNH3·H2O (25%–28%) 105 mL/L(NH4)3C6H5O7 56 g/LCH3COONH4 23 g/LCH3(CH2)10CH2OSO3Na 0.1 g/L

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Table 6Nano-Cu/Ni composite plating solutions.

Chemical composition Content

NiSO4·6H2O 254 g/LNH3·H2O (25%–28%) 105 mL/L(NH4)3C6H5O7 56 g/LCH3COONH4 23 g/LCH3(CH2)10CH2OSO3Na 0.1 g/LC H N O ·H O 0.1 g/L

C2H8N2O4·H2O 0.1 g/LC nanoparticles 15 g/L

ere used for preparing brush electroplating solution. Absolutethanol and 1H,1H,2H,2H-Perfluorooctyltrimethoxysilane weresed for preparing solution to decrease the free energy of platingoatings. All materials were used as received. E355DD carbonteel was used as the substrate and the dimensions of samples are0 mm × 45 mm × 7 mm.

.2. Fabrication of the superhydrophobic coating

Preparation process of nano-composite coating is as follows:Firstly, the E355DD carbon steel substrate was polished to have

surface roughness height value of about 0.80 �m, rinsed witheionized water, degreased in ethanol and dried in a dry box.

The electrolytic cleaning solutions (Table 1), activation solutionsTables 2 and 3), preplating solutions (Table 4), nano-C/Ni compos-te plating solutions and nano-Cu/Ni composite plating solutionsTables 5 and 6) needed for nano-composite electro-brush platingere prepared.

Nano-composite coatings were prepared through co-


epositing nano particles and pure Ni by electro-brushlating (EBP) on E355DD carbon steel substrate. The EBPas conducted in the following steps: electrical clean-

ng → activation → preplating → plating of nano-C/Ni composite

2 8 2 4 2

Cu nanoparticles 5 g/LAdditive X 56 g/L

coating → plating of nano-Cu/Ni composite coating. After eachstep, the sample should be rinsed with deionized water. Themain parameters are shown in Table 7. After EBP, the sample wasultrasonically rinsed in ethanol for 30 min and dried in a dry boxat 60 ◦C for 60 min.

A micro/nano scale roughness was built on the sample sur-faces after EBP, but the surface free energy is too high, in order toobtain the superhydrophobic surface, the sample should be modi-fied by the low free energy materials. So, the simple was immersedinto 1H,1H,2H,2H-Perfluorooctyltrimethoxysilane ethanol solu-tion with a concentration of 2 wt.% for about 40 min at 60 ◦C, thendried in a dry box at 100 ◦C for 60 min.

2.3. Characterizations

The water contact angle (CA) was measured by the JC2000C-3Surface tension instrument with 5 �L deionized water dropletsapplied to five different points for each coating. The measurementmethod of contact angles was angle measurement way. The waterslide angle is the slope of the coating surface relative to the horizon-tal, on which a loose water droplet starts to slide; the SEM images ofsuperhydrophobic coatings were obtained by a Scanning electronmicroscope (Hitachi Limited; 3-3000N); anti-corrosion ability ofthe superhydrophobic coating was evaluated by a potentiodynamicpolarization curve measured in 3.5 wt.% NaCl aqueous solution bythe Electrochemical workstation (C350).

3. Results and discussion

All experiments were carried out at room temperature. Themaximum working voltage used for experiment was 15 V, becausewhen the working voltage was too high, the side-effects increased,and the workpiece would be heated seriously, which resulted inthe production of lots of water vapor and hydrogen, the mechanicalproperties of the coating would be decreased seriously.

3.1. Comparison of single-layer coating and the two-layercomposite coating

This paper investigates the hydrophobic properties of single-layer coatings which prepared with different kinds of nanoparticles.Measurement shows that after modification with 1H,1H,2H,2H-Perfluorooctyltrimethoxysilane, the contact angle of single-layernano-C/Ni composite coating can only be up to 126.6◦, single-layernano-Cu/Ni composite coating can only be up to 135.7◦, and waterdroplets are hard to slip from the surface. It is difficult to fabri-cate superhydrophobic structure via single-layer nano-compositeelectro-brush plating. Based on the topography of single-layercoatings, two-layer composite coating was studied. The experimentresults shows that the superhydrophobic structure can be fabricate


on carbon steel substrate via two-layer nano-composite electro-brush plating under appropriate technology, after modification, thecontact angle of two-layer coating can be up to 155.5◦, the slid-ing angle is 5◦. Fig. 1 shows the SEM images of different kinds of




H. Liu et al. / Applied Surface Science xxx (2013) xxx– xxx 3

Table 7Main parameters of electro-brush plating.

Working procedure Voltage (V) Time (s) Relative velocity (m/min)

Electrical cleaning +6 30 4–8No. 2 activation −6 30 5–10No. 3 activation −8 30 5–10Preplating +10 90 6–8Plating of nano-C/Ni composite coating +15 90 6–8Plating of nano-Cu/Ni composite coating +15 90 8–12

F ingle-layer nano-C/Ni composite coating, (b) single-layer nano-Cu/Ni composite coating,(

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ig. 1. The SEM images of different kinds of coatings at 1000× magnification. (a) Sc) two-layer nano-composite coating.

oatings. Among them, Fig. 1(a) is the surface topography of single-ayer nano-C/Ni composite coating, Fig. 1(b) is that of single-layerano-Cu/Ni composite coating, Fig. 1(c) is that of correspondingwo-layer nano-composite coating. As seen in Fig. 1, compared withingle-layer composite coatings, the surface of two-layer compos-te coating is rougher, has higher porosity and the grains of it arener. It can be found from Fig. 1 that the finer the grains, the lowerhe porosity and the rougher the surface, the more conducive to theabrication of superhydrophobic structure.

.2. Influence of working voltage on hydrophobic properties

This paper also investigates the influence of plating processarameters and Cu nanoparticle concentrations on hydrophobicroperties of two-layer coatings. Process parameters of the ante-ior five steps and C nanoparticle concentrations were the same, ashown in Table 7. The contact angles of coatings prepared at dif-erent working voltage are shown in Fig. 2 and the correspondingEM images are shown in Fig. 3. The deionized water used to mea-ure the contact angles was 100 �L. The brush speed was 8 m/min,


rush plating time was 1.5 min, concentration of Cu nanoparticlesas 10 g/L. As seen in Fig. 2, the contact angle increases along with

he working voltage while the voltage varies between 10 V and 15 V.hen working voltage is 10 V, the contact angle is only 109.8◦, but


Fig. 2. Contact angles of coatings prepared at different working voltage.





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Fig. 3. Surface topography of coatings prepared at different wo

hen the voltage is 15 V, the contact angle increases to 145.6◦. Itan be seen in Fig. 3 that the coating surface presents the typi-al “cauliflower head” morphology and each “cauliflower head” isomposed of a large number of small grains. It is because the pro-uberances at micro level caused by preferentially deposited unitsroduce the “tip effect”, the current density here increases, which

eads to faster deposition, and eventually the “cauliflower head”orphology is formed. Different deposition rate results in pores

etween the cauliflower heads. When working voltage increases,he current density increases, leading the deposition to speed upnd the grains to grow rapidly, eventually leading to the increasef porosity. As can be seen in Fig. 3, when the working voltages 10 V, the coating surface is flat and has low porosity; with thencrease of voltage, the grains become finer, the porosity increase,


he micro/nano scale roughness become obvious, and the surface isore similar to the lotus leaf surface, which prove once again that

he hydrophobic properties of the coating is relevant to the sizef the grains, the porosity and the roughness; the finer the grains,

Fig. 4. Optical images of water droplets on the surface of th

voltage (at 2000× magnifications). (a) 10 V, (b) 12.5 V, (c) 15 V.

the lower the porosity and the rougher the surface, the bigger thecontact angle.

It can be found from Fig. 4 that the bottom of water dropletsis very bright, it is because a very thin air layer exists betweenthe bottom of water droplets and coating surface. This appear-ance conforms to the Cassie-Baxter model which is supposed thatthe surface is comprised of solid and air pockets, and the contactof water droplets and rough surfaces is a liquid–solid/liquid–gascomposite contact. The Cassie–Baxter equation is

Cos�∗ = −1 + �S(1 + Cos�) (1)

�* is the contact angle of composite interface, � is the contact angleon a flat surface, �S is the percentage of liquid–solid interface.

As can be seen in Formula (1), when �S decreases, �* will


increases, that is to say when the percentage of Liquid-Solid inter-face decreases or the surface roughness increases, the contactangle will become larger. As shown in Figs. 2 and 3, the contactangle increases with the increase of coating porosity, which means

e superhydrophobic coating (at 1× magnifications).





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Fig. 7. Contact angles of coatings prepared at different Cu nanoparticles concentra-tions.

Fig. 5. Contact angles of coatings prepared at different brush speed.

hat when the percentage of liquid–solid interface decreases, theontact angle increases. The experiment results conform to thisquation.

.3. Influence of brush speed on hydrophobic properties

Fig. 5 shows the contact angle of coatings prepared at differ-nt brush speed. The deionized water used to measure the contact


ngles was 5 �L. The corresponding SEM images of coating arehown in Fig. 6. The working voltage was 15 V, brush plating timeas 1.5 min, concentration of Cu nanoparticles was 10 g/L. As can

e seen in Fig. 5, while brush speed varies between 4 m/min and

Fig. 6. Surface topography of coatings prepared at different brush speed (at 200

8 m/min, the contact angle of coating changes little, which is around152.8◦; while the brush speed exceeds 8 m/min, the contact angletends to decrease; when the brush speed increase to 12 m/min,16 m/min, the contact angle decrease to 150.6◦, 145.2◦. As theworkpiece will be heated seriously and side-effects will increaseif the brush speed is too low, leading to a serious decrease of themechanical properties of coatings, the best choice of brush speed


is 8–12 m/min.

0× magnifications). (a) 4 m/min, (b) 8 m/min, (c) 12 m/min, (d) 16 m/min.





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ig. 8. Surface topography of coatings prepared at different Cu nanoparticles conce0 g/L.

.4. Influence of Cu nanoparticles concentration on hydrophobicroperties

Fig. 7 shows the contact angles of coatings prepared at dif-erent concentrations of Cu nanoparticles. The deionized watersed to measure the contact angles was 5 �L. The correspondingEM images of coating are shown in Fig. 8 . The working voltageas 15 V, brush plating time was 1.5 min and brush speed was

m/min. As shown in Fig. 7, while the particle concentration variesetween 1 g/L and 5 g/L, the contact angle increases along with theoncentration of nanoparticles; while the particle concentrationncreases from 5 g/L to 20 g/L, the contact angle tends to decrease;

hile the particle concentration varies between 3 g/L and 10 g/L,


he contact angles of coatings are all above 150◦and at concen-ration of 5 g/L, the contact angel of coating is the largest, whichp to 155.5◦, the sliding angle is only 5◦. In the electrodepositionrocess, the adjunction of nano-particles increase the nucleation

ions (at 2000× magnifications). (a) 1 g/L, (b) 3 g/L, (c) 5 g/L, (d) 10 g/L, (e) 15 g/L, (f)

rate by providing nucleus for the deposition of Ni metal, and hin-der the growth of grains; so, with the increase of Cu particles, the“tip effect” become more obvious, the porosity increase, and thegrain become finer. But when the Cu particles is excessive, thenucleus for deposition are too much, leading to an equivalent depo-sition velocity at different locations, which on the contrary reducesthe porosity and causes the micro/nano scale structure to be notobvious; besides, the ability of Ni to wrap up Cu nano-particles isdecreased, causing a reduction of coating’s mechanical property.As can be seen in Fig. 8, when the nanoparticle concentration is1 g/L, the grains is large and the porosity is relatively low; as thenanoparticle concentration increases, the grains become finer, theporosity increases, and the structure is more similar to that of lotus


leaf; when the nanoparticle concentration is excessive, at 15 g/Lor 20 g/L, the porosity decreases and the micro/nano scale struc-ture is not obvious. The experiment results conform to Formula(1).





leaf a

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Fig. 9. SEM images of lotus

.5. Comparison of the surface topography of as-prepared


uperhydrophobic coatings and lotus leaf

Fig. 9 is the SEM images of lotus leaf at different magnifications,nd Fig. 10 is that of as-prepared superhydrophobic coatings. As

Fig. 10. SEM images of superhydrophobic coa

t different magnifications.

can be seen in Fig. 9, lotus surface has lots of micro scale mastoids


which are about 10 �m in diameter and 12 �m away from eachother; the micro scale mastoids surface are covered by lots of nanoscale protuberances which are about 200 nm in diameter. A lot ofair exists in the space between these protuberances, which enables

ting surface at different magnifications.


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[21] H. Wang, D. Dai, X. Wu, Fabrication of superhydrophobic surfaces on aluminum,

ig. 11. Potentiodynamic polarization curve of superhydrophobic coating and355DD carbon steel substrate.

he lotus leaf surface to have the superhydrophobic properties. Asan be seen in Fig. 10, the as-prepared superhydrophobic coatingurface also has lots of micro scale protuberances which are about

�m in diameter; these protuberances are composed of many nanocale grains which are about 800 nm in diameter. With the compa-ation of these two figures, it can be found that the as-prepareduperhydrophobic coating surface is structural similar to lotus leafurface in a certain degree.

.6. Anti-corrosion ability of the as-prepared superhydrophobicoatings

Anti-corrosion abilities of the superhydrophobic coating andhe carbon steel substrate were evaluated by a potentiodynamicolarization curve measured in the 3.5 wt.% NaCl aqueous solu-ion by an Electrochemical workstation. Three-electrode systemas applied to test the performance. Pt (99.99%) was used as the

uxiliary electrode, Ag/AgCl as the reference electrode, superhy-rophobic coating and the carbon steel substrate as the workinglectrode. Polarization curves of three superhydrophobic samplesave been measured and the results have good repeatability. Theesults are shown in Fig. 11. The free corrosion potentials (Ecorr)f both coatings are determined by curve fitting over the Tafelegions where the current is nearly proportional to the exponentialf the potential. The Ecorr of as-prepared superhydrophobic coatings approximately −0.42163 V, higher than that of carbon steel sub-trate, which is −0.57843 V. Besides, as shown in Fig. 11, the anodicranch curve of polarization curve for carbon steel substrate shows

rapid dissolution, the anodic current density of superhydropho-ic coating is lower than that of carbon steel, and increases slowlyith the increase of potential. So the superhydrophobic coating has

etter anti-corrosion performance compared with substrate.

. Conclusions

In this paper, we study the method to fabricate superhy-rophobic surface on carbon steel substrate via nano-composite


lectro-brush plating. The conclusion is summarized as follows:he superhydrophobic structure can be successfully prepared bylating nano-C/Ni and nano-Cu/Ni two-layer coating on carbonteel substrate under appropriate technology; the micro/nano

[

PRESSience xxx (2013) xxx– xxx

scale roughness of superhydrophobic coating surface is similarto that of lotus leaf; when the working voltage is 15 V, brushspeed is 8 m/min, concentration of Cu nanoparticles is 5 g/L, thecontact angle of coating after modification with 1H,1H,2H,2H-Perfluorooctyltrimethoxysilane is the largest, up to 155.5◦, thesliding angle is 5◦; compared with carbon steel substrate, the super-hydrophobic coating has better anti-corrosion performance.

Acknowledgments

This work was supported by the National Nature ScienceFoundation of China (51075387) and the National 863 Project(2013AA06A411).

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fabrication of lotus-leaf-like superhydrophobic surfaces via ni-based nano-composite electro-brush...

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