10-56-47-superhydrophobic-PET-Al2O3-SiO2

ORIGINAL PAPER

Preparation of superhydrophobic PET fabric from Al 2O 3–SiO 2hybrid:geometrical approach to create high contact angle surface from low contact angle materials

N.P.Damayanti

Received:8January 2010/Accepted:18June 2010/Published online:30June 2010óSpringer Science+Business Media,LLC 2010

Abstract In this work we prepare high contact Poly Ethylene Terephthalate (PET)fabric surface from low contact angle materials.Superhydrophobic PET fabric is prepared by coating the fabric with hybrid Al 2O 3–SiO 2sol.In this case,the high contact angle Al 2O 3–SiO 2hybrid is created from low contact angle Al 2O 3and SiO 2precursors.PET treated with hybrid Al 2O 3–SiO 2exhibit Water Contact Angle (WCA)as 150°,while PET treated with individual Al 2O 3sol or SiO 2sol exhibits lower WCA,(Al 2O 3WCA =137°;SiO 2WCA =141°).FESEM and AFM investigations show that the hybrid Al 2O 3–SiO 2sol and individual Al 2O 3or SiO 2sol imparted different roughness geometry on the PET fabric surface.We observe surface structure of ?sh ?n-like,particle-like and hybrid ?n-parti-cle for treated PET fabric with;Al 2O 3,SiO 2and hybrid Al 2O 3–SiO 2sol,under FESEM and AFM observa-tions.AFM observations show the evolution of roughness (Ra)dimension of different surface structures with the order of:SiO 2\Al 2O 3\Al 2O 3–SiO 2(Ra =31,63and 273nm).We believe that the disparity of the surface geometries lead into different surface WCA.FTIR spectra of Hybrid Al 2O 3–SiO 2shows additional peak at 902,850,557,and 408cm -1which can be ascribed to the hybrid-ization structure.

Keywords Superhydrophobic áHybrid áSiO 2–Al 2O 3áHierarchical roughness

1Introduction

Superhydrophobic fabrics recently are of high interests [1]because of their wide range of applications such as protec-tive clothing [2],automobile [3],building architecture [4]and so forth.To date,superhydrophobicity on textile fabrics have been achieved by alteration of ?ber materials [5,6]or modi?cation of surface properties [7–18].Modi?cation of surface properties includes modi?cation process of surface chemistry [7–12]and or surface structures [13–18].

Given that surface structure is proven to enhance anti wetting character [19–27],numerous works creating dif-ferent surface architectures on fabrics have been reported [8,10,21,28,29].Different surface architectures have been commonly obtained by introducing particles onto the surfaces.There are several kinds of inorganic particles such as ZnO [9],SiO 2[10–15,17,19,30,31],Al 2O 3[21,33–35],Co 2O 3[36],and TiO 2[37],have been reportedly synthesized in micrometer to nanometer range to impart roughness on the surfaces.

As far as the geometry of surface is the concern,super-hydrophobic state resulted from surface treatment involving SiO 2or Al 2O 3are known to be achieved by different surface architectures [19,20,28,29,33,36].However,those architectures are derived from sophisticated techniques [19,28,29,33,36]which impede the industrial scale-up.In this work we create unique surface structure on PET fabric that render surface superhydrophobic by incorporating facile sol gel method which allows industrial scale up.

It is noteworthy that superhydrophobic state in the pre-vious studies employing SiO 2[10,15,16]and Al 2O 3[32,33,37]could be achieved by surface post-treatment with high contact angle materials such as ?uorine [10,11,16,37]or long chain silane precursor [15,37,38].Therefore,no clear information can be acquired,whether the roles of

N.P.Damayanti (&)

Polymer Materials Section,Department of Raw Materials and Yarns,Taiwan Textile Research Institute,No 6,Chengtian Rd,Tucheng City,Taipei County,Taiwan,ROC e-mail:pradanidamayanti@https://www.360docs.net/doc/3114969017.html,

J Sol-Gel Sci Technol (2010)56:47–52DOI 10.1007/s10971-010-2271-0

SiO2and Al2O3are solely to impart roughness to the sur-face or they can render surface superhydrophobic without the presence of problematic[30,39]high contact angle materials[30,31].

In this work we investigate the possibility of creating high contact angle surface from low contact angle materials by imparting certain geometry on the surface.We intro-duce superhydrophobicity on PET fabric by coating the fabric with hybrid Al2O3–SiO2sol without surface post-treatment with high contact angle materials.We disclose details preparation of three different sols;Al2O3sol,SiO2 sol,and the hybrid Al2O3–SiO2,via facile sol gel method. We provide insight on how each oxide imparts different hydrophobic character on the PET surfaces based on the surface structures investigation.

2Experiments

2.1Materials

Aluminum-tri-sec-butoxide(Al(O-sec-Bu)3),isopropyl alcohol(i-PrOH),ethanol(EtOH),Ethyl acetoacetate (EAcAc),Hydrochloric acid(HCl),Methyltrimethoxysi-lane(MTMS),c-aminopropyltriethoxysilane(APTS),are obtained from Acros,Tedia,Merck,Showa,Showa, Degussa,and Degussa,respectively.All chemical are used as received without further puri?cation.The water(H2O) used in the sol gel process is puri?ed by both ion exchange and distillation.The PET fabric used in this work is pre-treated with acetone extraction(80%w/w)at60°C for1h to remove surface impurities.

2.2Synthesis of Al2O3sol

Al2O3sol is prepared by simple sol gel process at the room temperature.The initial procedure is similar with Tadana-ga’s procedure[35]to create Al2O3sol.However,in this work we employ two different solvents and two steps of hydrolysis.Firstly,Al(O-sec-Bu)3and i-PrOH are stirred for1h.The EAcAc is further added and the mixture is stirred for3h.The mixture of water H2O and i-PrOH is added and stirred30min[35].EtOH is added to the solution and stirred for15min.The mixture of H2O and HCl is slowly added and stirred for20h.The molar ratio of HCl,EtOH, i-PrOH,H2O,and EAcAc to Al(O-sec-Bu)3are0.5,71,20, 95,and1M respectively.The sol is transparent yellow in color and remains in this state for the rest of20h reaction time.

2.3Synthesis of SiO2sol

SiO2sol is prepared by mixing MTMS and EtOH,under mild stirring condition for15min,APTS is further added and stirred for15min.The mixture of H2O and HCl is slowly added and stirred for20h.The molar ratio of MTMS:ETOH:HCL:H2O toward APTS are2:5:6:12 respectively.

2.4Synthesis of Hybrid SiO2–Al2O3

Hybrid sol between Al2O3and SiO2is prepared by?rstly mixing MTMS and EtOH under mild stirring condition for 15min.Al2O3sol produced in Sects.2.2is added,and the mixture is stirred for15min.APTS is further added and stirred for15min.The mixture of H2O and HCl is slowly added and stirred for20h.The weight ratio from total solution of Al2O3:MTMS:APTS:EtOH:H2O:HCl are 12:24:4:48:12:0.1respectively.

2.5Treatment of PET fabrics

PET fabrics(plain-wave,138g/m2)are pretreated by simple process of acetone extraction,in which PET fabrics has been soaked in15%acetone solution(1h,60°C) before dip-coated with as prepared sols.Fabrics are dipped into sol solution for1h,coated fabrics is further dried at the room temperature and cured at160°C.

2.6Characterization

Surface structures are observed by Thermomicroscope APL-020atomic force microscopy(AFM)and JEOL JSM6510 Field Emission Scanning Electron Microscope(FESEM). Energy Dispersive Spectroscopy(EDS)INCA51-ADD076 is used for element analysis.The surface chemistry of the fabric is examined by Nicolet Magna560Fourier Transform Infra Red(FTIR)spectrometer.Static water contact angles (WCA)are measured with Kyowa CA-D type simple goni-ometer.Sliding angle is performed with employing micro-scope slide and simple protractor.

3Results and discussion

Figure1shows typical SEM images of untreated PET fabric,which will be treated with as prepared sols in this work.SEM image of PET fabric upon acetone extraction shows smooth?bers surface in the micrometer range,with minimum bonding between adjacent?bers.Smooth?ber in the micrometer range indicates no impurities on the?ber surface,in which such impurities will impede strong pen-etration of coating agent onto the surface[41].The mini-mum bonding ensures smooth hand feeling of the fabric [42].AFM image(Fig.1b)shows nanometer roughness on the?ber surface with average roughness(Ra)of2.43nm. We identify the observed nanometer roughness as inherent

roughness of the untreated PET ?ber [43].The pristine PET fabric exhibits hydrophilic character with WCA as 0°.The correlation of surface structure on the treated fabric and the WCA is depicted in Fig.2a–c,in which we can observe typical SEM images of PET fabrics treated with three different sols;Al 2O 3sol (2a),SiO 2sol (2b)and the hybrid Al 2O 3–SiO 2sol (2c).The insets of Fig.2a–c show corresponding WCA for each surface structure.Figure 2a–c indicate denser and rougher structure of the hybrid produce higher WCA value than the less dense structure of indi-vidual Al 2O 3or SiO 2.

We verify that surface structures on the PET surfaces are formed by as prepared sols by performing EDS charac-terization (Fig.2c–e).We observed Ti,Pt,C and O peak in all of the treated PET fabrics.We believe that Pt peak comes from the sputtering process,while Ti,C and O can be ascribed to the intrinsic element of PET fabric.Further observation on the EDS spectra reveals that there are dif-ferent elements on the different treated PET fabrics.We observed Al peaks in the EDS spectra of PET treated with Al 2O 3(Fig.2d),Si peaks on SiO 2treated PET (Fig.2e),and Al–Si peaks in the EDS spectra of PET treated with hybrid Al 2O 3–SiO 2(Fig.2f).These results demonstrate that Al 2O 3,SiO 2and Al 2O 3–SiO 2sols are successfully coated on the PET fabrics.

Figure 2a shows that PET surface treated with Al 2O 3sol exhibits dense protrusion in the micrometer range on its surface.Dense and bumpy protrusion surface structure of Al 2O 3treated PET is believed as the main factor in ren-dering PET fabric hydrophobic.Previous studies employ-ing Al 2O 3sol to create superhydrophobic ?owerlike structure [21,22,34]applied ?uorine post-treatment pro-cedure to hydrophobicized Al 2O 3structure.It was observed in the previous study [22,43]that coating with Al 2O 3alone could not render the surface hydrophobic.In this work,Al 2O 3sol rendered PET surface hydrophobic with WCA as 131°[Fig.2a (inset)].This value of WCA is achieved without post treating PET with high contact angle materials.

PET treated with SiO 2sol consist of rounded protuber-ances on its surface under SEM observation (Fig.2b It exhibits WCA as 143°[Fig.2b (bottom)].This value of WCA for SiO 2coated fabrics in the previous studies [13,31,36]is measured about 120–141°.Unlike in the prece-dent studies working with silane precursors [13,15,31,36,46],we do not employ long carbon chain silane precursors which are high contact angle materials.The high WCA for SiO 2treated PET in this work is ascribed to geometry effect of the surface.

Figure 2c shows SEM image of PET treated with the hybrid of Al 2O 3–SiO 2.Under the SEM observations,PET fabric treated with hybrid Al 2O 3–SiO 3consists of compact robust structure which is different from the structure of PET treated with individual Al 2O 3or SiO 2sol.This compact robust structure exhibits excellent repellency to water droplets,that is,WCA as 150°.

We predict that the unique roughened structure of Al 2O 3–SiO 2(Fig.2c)will trap air in its valleys that allow water droplet to sit on its protuberances and the air.This condition maximize the interaction among droplet,surface material and air [43,44]that lead into superhydrophobic state.Therefore,it can be suggested that Al 2O 3–SiO 2hybrid can form certain degree of roughness [25,27,45]on the PET surface that enough for rendering surface super-hydrophobic,regardless the absence of high contact angle materials.

In order to further examine the surface roughness geometries,we examine SEM images of three different thin ?lms;Al 2O 3,SiO 2and Al 2O 3–SiO 2(Fig.3a–c).AFM observation is also adopted to further investigate the sur-face structure of different treated PET fabrics (Fig.3d–f).SEM image of Al 2O 3(Fig.3a)conformed to AFM image of Al 2O 3treated PET (Fig.3d),showing robust surface which resemble layer by layer ?sh ?n-like struc-ture.We believe that hydrophobic character of Al 2O 3in the absence of high contact angle materials [21,22,34,43]can be ascribed to this compact unique structure.

Figure 3b shows SEM images of particle-like structure of SiO 2?lm.This result is supported with the corre-sponding AFM image (Fig.3e)that shows spherical shape on the PET treated with SiO 2.In this work we did not employ high contact angle silane precursors [13,15,31,36

,

Fig.1Untreated PET fabric:a SEM micrographs shows clean and smooth ?ber surface b AFM image shows untreated fabric has irregular roughness in nano scale

46].The high contact angle of 141°can be ascribed to the combination effect of the particle like structure and hydrophobic nature of silane precursor [27].

The failure of SiO 2sol alone to render PET fabric su-perhydrophobic is probably due to its sparsely distributed structure that it formed on the PET surface.Sparsely dis-tributed roughness does not promote droplet to sit on the protuberance and prevent air trapping between the cavities [24,25,39].It is also possible that such structure will allow droplet to shift easily from Cassie regime into Wenzel regime [24,26,27,47].

SEM image of hybrid Al 2O 3–SiO 2?lm (Fig.3c)shows bigger,denser and higher protuberances compare to those for individual oxide.This result is supported by AFM ima-ges (Fig.3e)which shows hierarchical alternate structure of two different geometries (a–b–a–b–…).This geometry represents orderly hierarchical structures that favor the for-mation of superhydrophobic state [26,39,40].

AFM images of the treated PET fabric corroborate SEM images of PET fabric and the ?lms.AFM image of treated PET with;Al 2O 3shows a ?sh-?n like geometry,SiO 2shows sphere like surface structure and the hybrid Al 2O 3–SiO 2shows alternating hierarchical structure.We believe those surface represent the major structure of the ?ber surface.

In this work we obtain sliding angle less than 3°for all treated PET.These results suggest that the roughness structures allow water droplets to fall into Cassie regime [25,46]instead of being trapped in Wenzel cavities [23,24,46].We believe that the geometry created in this work will allow droplet to sit on the protuberances and trap the air between the cavities.In this manner,the geometries will

(b)

143o

(c)

150o o

(a)

131o

(d)

(e)

(f)

1μ 1μ 1μ

Fig.2SEM micrographs of treated PET fabric (a ,b ,c )with its corresponding WCA (inset )and corresponding EDS spectra (d ,e ,f );a PET treated with Al 2O 3sol shows sub-micrometer roughness and con?rmed Al element by EDS (d ),b PET treated with SiO 2sol shows sparsely particle like roughness and con?rmed Si element by EDS (e ),c PET treated with hybrid Al 2O 3–SiO 2shows condensed roughness structure and con?rmed Si and Al elements by EDS (f )

(d) (a)1μ

(b)5μ

(e) (c)

b a a

b (f)

be able to render surface hydrophobic with high contact angle with the absence of high contact angle materials.

The comparison of SEM images for PET treated with

Al2O3(Fig.2a),SiO2(Fig.2b)and Al2O3–SiO2(Fig.2c) reveals the evolution of roughness from small and sparse roughness into bigger and robust roughness with the order; SiO2\Al2O3\Al2O3–SiO2.

To examine the in?uence of hybridization on the structural evolution,AFM analysis is adopted to?gure out the surface topography of the treated PET fabrics.Different roughness structure in the size and geometry can be observed in the AFM images of three different treated PET fabrics(Fig.3a–c).The data of the pro?le measurements allow the calculation for the values of:mean peak height from valley(Rz),average roughness(Ra)and average height from peak height above mean line(Rp),which are presented in Table1.

We observed an increase in Rz value in the order of: SiO2\Al2O3\Al2O3–SiO2,with the value as;188,273, and955nm,respectively.The same trend can be seen in the value of Ra and Rp.The results demonstrate Al2O3 creates a bigger roughness structure than SiO2on the PET surface,and the hybridization between Al2O3and SiO2 induces a rougher and bigger roughness structure than the individual sol.

Superhydrophobicity of hybrid structure in this work is in accordance with nature’s superhydrophobic surface, Lotus leaf.Superhydrophobic state of Lotus is ultimately governed by its structure.The wax on the lotus leaf is believed to be intrinsically hydrophilic[42,45].However, the hierarchical structure of crystalloid of the wax play signi?cant role of its superhydrophobicity[43,45,47].

In this study we obtain WCA ranging from hydrophobic (134°)to superhydrophobic(150°).Such of those WCA values are obtained on the modi?ed PET surface with the ratio(h of peak to valley[48]within the range of1Table1. Previous study[47]employing silane precursor maintained that roughness structure should have minimum h=2to allow air trapping and to prevent water penetration(WCA 123°).The higher WCA of this study compare to those surfaces with h C2[48]suggest that h C1is suf?cient to prevent water penetration.Furthermore,the sliding angle of \3°in this study indicates that water droplet fall on Cassie regime[25,27,48].These results further suggest that h=1in this work will not only prevent water penetration but also allow droplet to fall into Cassie regime.When droplet falls into Cassie regime,it will be easily rolled off, since it is not trapped in the Wenzel cavities[25,27].

Figure4shows the FTIR spectra of three sols to treat the PET fabrics.In all three spectra;SiO2–Al2O(a),Al2O3(b), and SiO2(c),we identify major peaks in the range of 400–1,800cm-1.The typical absorption peaks of Si–O–Si bonds[49–52]appearing at1,200–1,000cm-1in both(a) and(c)spectra.

We observe a red shift of the Si–O–Si peak in(a) (1,196cm-1)from those corresponding peak in(c).We predict that the shift is attributed to the formation of Si–O–Al–O–Si bond[48]and an indication of Al perturbation to Si–O–Si network[52].

We detect Al2O3structure in the(b)spectra.The peak at 769cm-1can be ascribed as stretching vibration of Al–O4 octahedral[53],while typical Al-O-Al bending vibration can be identi?ed at1,116cm-1[53].

We identify typical absorption peaks of Si–O–Al bonds [51,52,54]at:850and557cm-1.We attribute a strong peak within400–500cm-1to Si–O–Al ring[55],and an addi-tional broad peak in902cm-1in(a)is also ascribed as Si–O–Al bond.FTIR results(Fig.4)suggest that Al2O3and SiO2were hybridized by the formation of Si–O–Al bond. The bonding between Al2O3and SiO2result in the unique structure which render PET surface superhydrophobic.

4Conclusion

We successfully prepare superhydrophobic PET from low contact angle materials with the absence of;?uorine materials,long carbon chain silane precursors or strong solvents.The hybridization of Al2O3and SiO2employ facile sol gel method under room temperature which raises the potential for industrial application.Hybrid Al2O3–SiO2

Table1The value of Rz=mean peak height from valley; Rp=Peak height above mean line;Ra=average roughness, h=peak to valley ratio for PET fabric treated with different sols Treated PET Rz(nm)Rp(nm)Ra(nm)h

Blank PET1272 1.00 SiO2–Al2O3(a)955493273 1.07 SiO2–Al2O3(b)566293147 1.07 Al2O327313563 1.00 SiO21889831

1.08

Fig.4The FTIR spectra of a Al2O3?lm,b Hybrid SiO2–Al2O3?lm

and c SiO2?lm

introduces unique geometry via formation of Si–O–Al bond on the PET fabric surface by simple coating method under low curing temperature.Therefore geometrical approach employing sol gel process to render PET fabric superhydrophobic is potential candidate for water repellent treatment in industrial application,especially for fabric water repellent.

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