fabrication of superoleophobic surfaces on al substrates

Journal ofMaterials Chemistry A

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Key Laboratory for Precision and Non-tradit

of Education, Dalian University of Technolo

China. E-mail: [email protected]; Fax: +8

† Electronic supplementary informa10.1039/c3ta13807k

Cite this: J. Mater. Chem. A, 2013, 1,14783

Received 22nd September 2013Accepted 30th September 2013

DOI: 10.1039/c3ta13807k

www.rsc.org/MaterialsA

This journal is ª The Royal Society of

Fabrication of superoleophobic surfaces on Alsubstrates†

Jinlong Song, Shuai Huang, Ke Hu, Yao Lu, Xin Liu and Wenji Xu*

An easy method of fabricating superoleophobic surfaces on Al substrates by constructing reentrant

structures is reported. The reentrant micro/nanometer-scale structures comprise micrometer-scale,

rectangular-shaped, and step-like Al structures obtained by electrochemical etching and nanometer-

scale Ag grains resulting from immersion in [Ag(NH3)2]+ solution. Surface energy is reduced by

perfluorooctanoic acid (PFOA) containing –CF3 and –CF2– groups. The PFOA-modified micro/nanometer-

scale rough structures enable the formation of a composite solid–liquid–air interface with peanut oil.

These structures show good superoleophobicity with a peanut oil contact angle of 160.0 � 2� and a

sliding angle of 8�. Nanometer-scale structures can effectively transform the micrometer-scale non-

reentrant structures into reentrant structures. With the aid of suitable low surface energy materials such

as PFOA, fabricating superoleophobic surfaces on Al substrates can be easier.

Introduction

Superhydrophobic surfaces with a water contact angle larger than150� and a sliding angle smaller than 10� can be found in manyanimals and plants in nature, e.g., water striders, cicadas,mosquitoes, lotus, rice leaves, and taro leaves.1–3 Over the past 15years, superhydrophobic surfaces have attracted much attentiondue to their potential applications in self-cleaning,4–6 anti-icing,7,8

oil/water separation,9–12 corrosion resistance,13–15 smart orresponsive surfaces,16–19 and microuidics.20 To date, thousandsof published research papers on superhydrophobic surfaces exist.Numerous methods and basic theories on the fabrication ofsuperhydrophobic surfaces on various substrates, includingmetals, polymer, wood, cotton, paper, glass, and carbon, havebeen presented by researchers.21–28 However, most commonsuperhydrophobic surfaces are easily degraded by water contain-ing oil, which limits the practical application of superhydrophobicsurfaces. Thus, the fabrication of superoleophobic surfaces withoil contact angles larger than 150� and sliding angles smaller than10� can be effective to prevent surface contamination by oil.

Compared with superhydrophobic surfaces, methods forfabricating superoleophobic surfaces are lacking. The pub-lished research papers on superoleophobic papers are very few.Oils possess much lower surface tension than water, and oilrepellency requires a surface with lower surface energy.29

The main processes involved in fabricating superoleophobic

ional Machining Technology for Ministry

gy, Dalian 116024, People's Republic of

6-411-84708422; Tel: +86-411-84708422

tion (ESI) available. See DOI:

Chemistry 2013

surfaces are the primary construction of rough structures andthe subsequent lowering of the surface energy by low surfaceenergy materials (these two steps are merged into one step bysome researchers), which are similar to the processes involvedin fabricating superhydrophobic surfaces.30–38 However, therough structures required by superoleophobic surfaces aremuch stricter than those required by superhydrophobicsurfaces. To illustrate the strictness of the rough structuresrequired by superoleophobic surfaces, several schematics ofliquids in contact with the rough structures are shown (Fig. 1).Angles Fstructure are the local geometric angles of the roughstructures that are formed between the side walls of the struc-tures and the horizontal line. Angles q are the intrinsic (equi-librium) contact angles of liquids on smooth surfaces with thesame chemical composition and surface energies as the roughstructures. For any liquid, if Fstructure < qliquid, the liquid–airinterface (meniscus) in the grooves of the rough structures isconvex and the net force F on the liquid–air interface is upward,thus preventing liquids from wetting the surfaces inside therough structures and forming an ideal composite solid–liquid–air interface in the Cassie–Baxter state. If Fstructure > qliquid, theliquid–air interface in the grooves of the rough structures isconcave and the net force F on the liquid–air interface isdownward, causing the complete wetting of the surfaces insidethe rough structures by the liquids.39–44 For most low surfaceenergy material modied smooth surfaces, the water contactangle qwater is larger than 90� but smaller than 120� whichmeans that many rough structures withFstructure of smaller than120� can be used to fabricate superhydrophobic surfaces in theCassie–Baxter state [Fig. 1(a)–(c)]. However, the contact angleqoil of oil (e.g., peanut oil with a surface tension of 37.5 mNm�1)on the low surface energy material modied smooth surfaces is

J. Mater. Chem. A, 2013, 1, 14783–14789 | 14783

http://dx.doi.org/10.1039/c3ta13807k

http://pubs.rsc.org/en/journals/journal/TA

http://pubs.rsc.org/en/journals/journal/TA?issueid=TA001046

Fig. 1 Schematics of water (a to c) and oil (d to h) in contact with the rough structures with different values of Fstructure.

Fig. 2 Schematics of the processes for fabricating superoleophobic surfaces onAl substrates.

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smaller than 90�, indicating that only rough structures with aFstructure of smaller than 90� can be used in the fabrication ofsuperoleophobic surfaces in the Cassie–Baxter state [Fig. 1(d)–(f)]. If there are ner structures on the side walls, the roughstructures shown in Fig. 1(d) and (e) may be transformed intoreentrant structures [Fig. 1(g) and (h)]. Therefore, the roughstructures required by superoleophobic surfaces are muchstricter compared with those required by superhydrophobicsurfaces, and only reentrant structures (Fstructure < qoil < 90�) aresuitable for fabricating superoleophobic surfaces.

Al and its alloys are widely used in automotive, aerospace,aviation, shipbuilding and construction industries because oftheir superior mechanical properties. The fabrication of super-oleophobic surfaces on Al substrates is signicant. Super-hydrophobic Al surfaces can be fabricated easily, but methods forfabricating superoleophobic Al surfaces are few. In this study, wedeveloped reentrant micro/nanometer-scale rough structures tofabricate superoleophobic surfaces on Al substrates. The reen-trant micro/nanometer-scale rough structures composed ofmicrometer-scale rectangular-shaped and step-like Al structuresand nanometer-scale Ag grains were created by electrochemicaletching and immersion in [Ag(NH3)2]

+ solution. These micro/nanometer-scale rough structures, combined with the lowsurface energy obtained by peruorooctanoic acid modication,lead to superoleophobicity for peanut oil. In addition, the suit-ability of low surface energy materials, which are oen used tofabricate superhydrophobic surfaces, in the fabrication ofsuperoleophobic surfaces is also reported. This study provides anew way to confer superoleophobicity to Al substrates.

ExperimentalMaterials

Commercially available Al plates (2 mm thick; purity >99%)were purchased from the Dalian Aluminum Material

14784 | J. Mater. Chem. A, 2013, 1, 14783–14789

Manufacturer (China). Stearic acid [STA, CH3(CH2)16COOH],ammonia, NaCl, and AgNO3 were purchased from TianjinKermel Chemical Reagent Co. (China). Fluoroalkylsilane [FAS,tridecauoroctyltriethoxysilane, CF3(CF2)5(CH2)2Si(OCH2CH3)3]was purchased from the Degussa Co. (Germany). Per-uorooctanoic acid [PFOA, CF3(CF2)6COOH] was purchasedfrom Sigma-Aldrich (USA). Peanut oil was purchased fromLuhua Co. (China). The rest of the chemicals used in theexperiment were of analytical grade and purchased from TianjinKermel Chemical Reagent Co. (China).

Fabrication of superoleophobic surfaces

Before processing, ammonia solution was added dropwise intoaqueous AgNO3 solution to form a transparent 0.1 mol L�1

[Ag(NH3)2]+solution. Al plates were cut into 30 mm � 40 mm

pieces, polished using #1200 and #1500 abrasive paper, and

This journal is ª The Royal Society of Chemistry 2013


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ultrasonically cleaned with alcohol and deionized water insequence to remove the surface oxide layer, other impurities,and grease [Fig. 2(a)]. The pre-cleaned Al plates were electro-chemically etched at 500 mA cm�2 processing current densityand 6 min processing time in a 0.1 mol L�1 aqueous NaClsolution to obtain micrometer-scale rough structures[Fig. 2(b)].45 Aer electrochemical etching, the Al plates wererinsed with deionized water and immersed in 0.1 mol L�1

[Ag(NH3)2]+ solution for 120 s at ambient temperature to obtain

nanometer-scale rough structures [Fig. 2(c)]. Subsequently, theAl plates were re-rinsed with deionized water and dried. Aerthe formation of surface structures, the Al plates were immersedin a 0.015 mol L�1 aqueous PFOA solution to reduce the surfaceenergy [Fig. 2(d)]. The obtained samples were le in air forseveral days until characterization. PFOA modication did notchange the surface morphology but lowered the surface energy.

Characterization

The surface morphologies of the samples were characterizedusing a scanning electron microscope (SEM, JSM-6360LV,Japan). The chemical compositions of the electrochemicallyetched and Ag-coated Al plates were characterized by using anXRD-6000 X-ray diffractometer system (Japan) and Empyrean X-ray diffractometer system (Holland), respectively. The wetta-bility of the samples was measured using an optical contactangle meter (DSA100, Kruss, Germany).

Fig. 3 Images of water droplet (5 mL) and peanut oil droplet (5 mL) on the PFOA-moAl surfaces (c and d).

Fig. 4 SEM images and XRD pattern of electrochemically etched Al surfaces: (a to


Results and discussionEffect of surface morphology on oleophobicity

Common polished Al surfaces exhibit hydrophilicity and oleo-philicity because of high surface free energy. Lowering surfaceenergy with low surface energy materials can reduce wettabilityof Al surfaces, but achieving superhydrophobicity and super-oleophobicity by relying only on lowered surface energy isalmost impossible. Changing the wettability by constructingsuitable rough structures and lowering the surface energy iseffective. The contact angles of water and peanut oil on PFOA-modied common polished Al surfaces are only 117.2� (zqwater)and 87.7� (zqoil), respectively, which are far from the valuesrequired for superhydrophobicity and superoleophobicity[Fig. 3(a) and (b)]. Aer electrochemical etching, the PFOA-modied electrochemically etched Al surfaces show extremewettability [Fig. 3(c) and (d)]. The contact and sliding angles ofwater are 167.1 � 2.3� and 2.5�, respectively. The contact angleof peanut oil is 145.2 � 1.6�. Peanut oil remains on thesurface when the sample surface is turned upside down.Micromorphology was detected by SEM to explain the changesof wettability. Fig. 4(a)–(e) show the SEM images of the elec-trochemically etched Al surfaces obtained at the 500 mA cm�2

processing current density and 6 min processing time in a0.1 mol L�1 aqueous NaCl solution. The electrochemicallyetched Al surfaces are rough and covered with a large number ofpits and protrusions [Fig. 4(a)–(c)]. These protrusions can be

dified common Al surfaces (a and b) and PFOA-modified electrochemically etched

c) top-view SEM images; (d and e) tilt-view SEM images; and (f) XRD pattern.

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considered as rectangular-shaped plateaus [Fig. 4(d)]. Somestep-like structures exist on the rectangular-shaped plateaus[Fig. 4(e)]. Thus, the electrochemically etched Al surfaces showtypical micrometer-scale rectangular-shaped plateaus and step-like structures with sizes in the range of 1 mm to 5 mm.According to the XRD pattern of the electrochemically etched Alsurfaces [Fig. 4(f)], the main component of the rough structuresis Al (JCPDS Card no. 04-0787). The formation mechanism ofthe micrometer-scale rectangular-shaped and step-like Alstructures has been discussed in our previous papers.46,47 Largeamounts of grain boundaries and dislocations exist in commonpolycrystalline Al. These grain boundaries and dislocations areprone to destruction during processing at relatively high ener-gies. The rough Al structures result from the preferentialdissolution of grain boundaries and dislocations by an appliedelectric eld. Fig. 5(a) shows the cross-sectional-view SEMimages of electrochemically etched Al surfaces mounted inepoxy, which reveal the local geometric angle Fstructure of eachrough structure. Schematics of water and oil in contact with therough structures are shown in Fig. 5(b) and (c). Almost allFstructure of PFOA modied electrochemically etched Al surfacesare smaller than qwater (z117.2�), indicating that the roughstructures can support a water droplet in contact with them inthe Cassie–Baxter state based on our earlier consideration ofrough structures shown in Fig. 1. However, not many reentrantstructures exist. Most Fstructure is larger than qoil (z87.7�).

Fig. 5 (a) Cross-sectional-view SEM images of electrochemically etched Al surfaces,indicate that the grooves of rough structures are not wetted by water but are wett

Fig. 6 SEM images and XRD pattern of electrochemically etched and Ag-coatedsectional-view SEM images (samples were mounted in epoxy).

14786 | J. Mater. Chem. A, 2013, 1, 14783–14789

When an oil droplet comes in contact with these rough struc-tures, the oil will wet all the grooves of the rough structures witha Fstructure larger than 87.7� and only the grooves of the reen-trant structures will not be wetted by oil, resulting in a large areafraction of the solid and oil on the surface. The peanut oil on thePFOA-modied electrochemically etched Al surfaces is in the“Gecko state” (high contact angle and adhesion).48 Therefore,the PFOA-modied electrochemically etched Al surfaces withonly micrometer-scale rough structures are superhydrophobicbut far from superoleophobic.

To construct a large number of reentrant structures on theelectrochemically etched Al surfaces, we coated nanometer-scale Ag grains on the micrometer-scale Al structures. Fig. 6(a)–(c) show the top-view SEM images of the electrochemicallyetched and Ag-coated Al surfaces obtained at the 500 mA cm�2

processing current density and 6 min processing time in a0.1 mol L�1 aqueous NaCl solution and following immersion inthe 0.1 mol L�1 [Ag(NH3)2]

+ solution for 120 s. Comparedwith the electrochemically etched Al surfaces, the wholesurfaces of the micrometer-scale rectangular-shaped and step-like structures are uniformly covered with nanometer-scale Aggrains aer immersion in [Ag(NH3)2]

+ solution. Fig. 6(d) showsthe XRD pattern of electrochemically etched and Ag-coated Alsurfaces. Three diffraction peaks at 38.18�, 40.77�, and 77.43�

are detected along with other additional diffraction peaksattributed to Al. The peaks at 38.18� and 77.43� are the

and schematics of water (b) and oil (c) in contact with the rough structures (arrowsed by peanut oil).

Al surfaces: (a to c) top-view SEM images; (d) XRD pattern; and (e and f) cross-



Fig. 7 Images of water and peanut oil droplets on the PFOA-modified electrochemically etched and Ag-coated Al surfaces.


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characteristic peaks of Ag(111) and Ag(311), respectively (JCPDSCard no. 04-0783). The peak at 40.77� is the characteristic peakof Al(OH)3 (JCPDS Card no. 20-0011). When the electrochemi-cally etched Al plates are immersed in the 0.1 mol L�1

[Ag(NH3)2]+ solution, Al reacts with [Ag(NH3)2]

+ and OH� ions toform a large number of Ag molecules [eqn (1)]. The reduced Agdeposits on the Al surfaces form the nanometer-scale struc-tures. A spot of Al(OH)3 is formed during the chemical reaction.

Fig. 8 Effects of processing parameters on oleophobicity: (a) to (b) changes in thcoated Al surfaces as a function of the immersion time in 0.1 mol L�1 [Ag(NH3)2]

+ solimmersed in 0.1 mol L�1 [Ag(NH3)2]

+ solution for 300 s; and (e) to (g) SEM imagessolution for 120 s.


Thus, the characteristic peak of Al(OH)3 is also detected on theXRD pattern. Fig. 6(e) and (f) show the cross-sectional-view SEMimages of the electrochemically etched and Ag-coated Alsurfaces mounted in epoxy. The existence of the nanometer-scale Ag grains in the side walls of the convex structurestransforms the non-reentrant structures into reentrant struc-tures that can form a composite interface where numerouspockets of air are trapped underneath the oil. Therefore, the

e contact and sliding angles of PFOA-modified electrochemically etched and Ag-ution; (c) to (d) SEM images of electrochemically etched and Ag-coated Al surfacesof Ag-coated Al surfaces obtained only by immersion in 0.1 mol L�1 [Ag(NH3)2]

+

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hierarchical micro and nanometer-scale rough structurespossess the reentrant structures which can support oil in theCassie–Baxter state. The PFOA-modied electrochemicallyetched and Ag-coated Al surfaces achieve superoleophobicity[Fig. 7]. The contact and sliding angles of peanut oil droplet onthe samples are 160.0 � 2� and 8�, respectively. In addition,the resulting samples also show good superhydrophobicity. Thecontact and sliding angles of water droplet (5 mL) on thesurfaces are 165.7 � 1� and 3.5�, respectively.

Al + 3[Ag(NH3)2]+ + 3OH� / Al(OH)3 + 3Ag + 6NH3 (1)

Effect of low surface energy materials on oleophobicity

Low surface energy materials, such as PFOA, FAS, and STA, areoen successfully used to reduce the surface energy in thefabrication of superhydrophobic surfaces. However, oils havemuch lower surface tension than water and oil repellencyrequires surfaces with even lower surface energy. Thus, somelow surface energy materials cannot be used or are difficult touse for the fabrication of superoleophobic surfaces. Based onthe same micro/nanometer-scale rough structures, FAS-modi-ed electrochemically etched and Ag-coated Al surfaces showoleophobicity with a contact angle of 137.9 � 3� and without asliding angle. STA-modied electrochemically etched and Ag-coated Al surfaces show oleophilicity with a contact angle of69.3 � 1.4� and without a sliding angle. Both FAS-modied andSTA-modied samples show very good superhydrophobicity.Thus, choosing suitable low surface energy materials is veryimportant in the fabrication of superoleophobic surfaces.Differences in oil wettability are observed among groups withdifferent surface energies (see ESI 1†).

Effect of processing parameters on oleophobicity

Fig. 8(a) and (b) show the changes in the contact angles andsliding angles of the PFOA-modied electrochemically etchedand Ag-coated Al surfaces as a function of the immersion timein the 0.1 mol L�1 [Ag(NH3)2]

+ solution. The water contact andsliding angles remain almost unchanged during the 120 simmersion time in [Ag(NH3)2]

+ solution. However, the oilcontact angles increase and the sliding angles decrease withincreasing immersion time up to 120 s. At 120 s immersiontime, good superoleophobicity with 160.0 � 2� contact angleand 8� sliding angle and superhydrophobicity with 165.7 � 1�

contact angle and 3.5� sliding angle are obtained. The change inwettability is due to the formation of nanometer-scale Agstructures (Fig. 5 and 6). When the immersion time goes beyond120 s, both hydrophobicity and oleophobicity decrease with theimmersion time. When the immersion time extends to 300 s,superhydrophobicity and superoleophobicity disappear. Thecontact angles of water and peanut oil are reduced to 152.9 �3.5� and 129.8 � 0.6�, respectively. No sliding angle is observedfor both water and peanut oil. Water and peanut oil remain onthe surfaces when the sample surfaces are turned upside down.Fig. 8(c) and (d) show the SEM images of the electrochemicallyetched and Ag-coated Al surfaces immersed in [Ag(NH3)2]

+

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solution for 300 s. Al surfaces are covered with lump-like Agstructures. The surfaces of the lump-like Ag structures are verydense without grooves and voids to store air, and to supportwater and oil droplets. In addition, superoleophobicity cannotbe obtained on Al substrates only by immersion in [Ag(NH3)2]

+

solution and without electrochemical etching. Fig. 8(e) to (g)show the SEM images of the Ag-coated Al surfaces obtained onlyby immersion in 0.1 mol L�1 [Ag(NH3)2]

+ solution for 120 swithout any electrochemical etching. No micrometer-scalerectangular-shaped and step-like structures are observed, onlylump-like Ag structures and grains. Aer PFOA modication,the Ag-coated Al surfaces do not achieve superhydrophobicityand superoleophobicity. The contact angles of water and peanutoil are 135.6 � 4.6� and 115.1 � 5.7�, respectively (see ESI 2†).

Therefore, the important factors for fabricating super-oleophobic Al surfaces are PFOA modication and obtainingreentrant micro/nanometer-scale rough structures composed ofmicrometer-scale rectangular-shaped and step-like structuresand nanometer-scale Ag grains.

Conclusions

Low-adhesive superoleophobic surfaces on Al substrates havebeen fabricated by constructing reentrantmicro/nanometer-scalerough structures and lowering the surface energy. The reentrantmicro/nanometer-scale rough structures comprise micrometer-scale rectangular-shaped and step-like Al structures obtained byelectrochemical etching and nanometer-scale Ag grains obtainedby immersion in [Ag(NH3)2]

+ solution. The existence of nano-meter-scale Ag grains can effectively transform micrometer-scalenon-reentrant structures into reentrant structures. These reen-trant structures can support low surface tension liquid dropletsin the Cassie–Baxter state. PFOA is more useful for conferringsuperoleophobicity compared with other low surface energymaterials, such as FAS and STA which are oen used to fabricatesuperhydrophobic surfaces. The contact and sliding angles of apeanut oil droplet on the resulting superoleophobic surfaces onAl substrates are 160.0 � 2� and 8�, respectively.

Acknowledgements

This work was nancially supported by National NaturalScience Foundation of China (NSFC, Grant no. 90923022),Scholarship Award for Excellent Doctoral Student Granted byMinistry of Education, and China Scholarship Council.

Notes and references

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fabrication of superoleophobic surfaces on al substrates

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