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Fabrication of Stable Superhydrophobic Coatings with Bicomponent Polyurethane/Polytetrafluoroethylene Composites

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Fabrication of Stable Superhydrophobic Coatings with Bicomponent Polyurethane/Polytetrafluoroethylene Composites Asian Journal of Chemistry; Vol. 23, No. 7 (2011), 2866-2870 Fabrication of Stable Superhydrophobic Coatings with Bicomponent Polyurethane/Polytetrafluoroethylene Composites * HU LIU, QIANQIAN SHANG, GUOMIN XIAO and JIANHUA LV School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, P.R. China *Corresponding author: Tel/Fax: +86 25 52090612; E-mail: [email protected]; [email protected] (Received: 8 July 2010; Accepted: 4 March 2011) AJC-9688 A superhydrophobic coating was fabricated with bicomponent polyurethane/polytetrafluoroethylene (BPUR/PTFE) composites. Bicomponent polyurethane was obtained by cross-linking reaction between polyisocyanate and hydroxylic fluoroacrylate resin, which was synthesized via free radical polymerization. Superhydrophobic surface with water contact angle of 158º and sliding angle of 2º was obtained from bicomponent polyurethane and polytetrafluoroethylene at their weight ratio of 2/3 by a simple procedure. An irregular rough structure with dispersed grooves and protuberances observed by scanning electron microscope was considered to be responsible for the surface superhydrophobicity. The coating adhered strongly to the substrate and was stable to corrosive medium. The technique is facile, economical and can be expected for large-scale application in anticorrosion and related areas. Key Words: Superhydrophobic coating, BPUR/PTFE composites, Stability, Phase separation, Self-cleaning. INTRODUCTION Two component polyurethane coatings are widely used in automobile industry, naval vessel and building field due to Inspired by naturally water-repellent plant leaves and their high performance of adhesion stress, chemical resistance insects, such as lotus and water strider, superhydrophobic and so on. It is expected that the application range will be surfaces with water contact angle more than 150º have recently broadened after endowing polyurethane coatings with drawn much attention in both fundamental research and superhydrophobicity. Polytetrafluoroethylene (PTFE) is a practical applications due to their self-cleaning, antiicing and commercially available fluoropolymer with excellent chemical 1-3 anticontamination properties . Up to now, various methods properties and well-known low surface energy (18 mN/m)14,15. have been reported for the preparation of artificial super- Herein, PTFE attracted much attention in fabricating hydrophobic surfaces, including electrochemical reaction and superhydrophobic surface. Yang et al.16 reported a super- 4,5 6 7,8 deposition , chemical vapour deposition , etching method , hydrophobic coating based on furfural acetone resin and PTFE 9,10 11 electrospinning and lithography or sol-gel technique and composites after curing at 300 ºC. The combination of double- so on. These approaches adopted could be generally categorized scaled structure and surface enrichment of fluorine element as either creating a rough microstructure on a hydrophobic made the coating surface superhydrophobicity16. However, to substrate surface or modifying the rough surface with low our knowledge, there is little literature about preparing surface energy materials such as fluorinated or silicon comp- superhydrophobic coatings based on bicomponent poly- ounds. However, these methods generally present some short- urethane (BPUR) and polytetrafluoroethylene (PTFE) compo- comings such as step-complex, expensive and, especially, low sites. In this study, the superhydrophobic surfaces of BPUR/ 12 surface coverage. Though some researchers have reported PTFE composite coatings were prepared using conventional that the superhydrophobic surfaces can be prepared by a simple spray and curing processes on tin plates. Hydroxylic and cost-effective spray process, the preparation process fluoroacrylate resin was synthesized firstly and then cross- involved the use of aggressive solvent such as dimethyl linked with polyisocyanate to obtain BPUR. Surface roughness formamide, which can dissolve the bottom coating, or the was created by embedding hydrophobically PTFE particles in so-called lifting phenomenon. Additionally, from practical BPUR matrix. The composite coatings presented superhydro- view point, superhydrophobic surfaces with sufficient phobicity and showed irregular rough structure with dispersed adhesive force and long-term stability in corrosive solutions grooves and protuberances after curing at 120 ºC. It should be are another two significant issues for them to be used in noted that the superhydrophobic coatings present high practice13. Vol. 23, No. 7 (2011) Fabrication of Superhydrophobic Coatings with Polyurethane/Polytetrafluoroethylene Composites 2867 cohesional strength with the substrates and are stable under 1.1 followed by intensive stirring. Polytetrafluoroethylene was corrosive conditions. It is expected that this technique will be added into the as-prepared solution with a certain percentage important for potential applications in future. by mechanical stirring and ultrasonic treatment for 0.5 h. The overall NCO/OH molar ratio was maintained at about 1.1 to EXPERIMENTAL ensure full reaction of OH groups. Methyl methacrylate (MMA) and butyl acrylate (BA), Tin plates with a thickness of 0.28 mm were polished purchased from LingFeng Chemical Regent Co. Ltd. (China), with metallographic abrasive papers repeatedly and then rinsed were washed by 10 wt % aqueous solution of sodium hydroxide with alcohol thoroughly. The coatings on the tin plates were to remove inhibitor and then by distilled water thoroughly, prepared by spraying the coating precursors with 0.2 MPa until pH value of the washings became neutral. The washing- nitrogen gas and then cured at the temperature of 120 ºC for 2 h. treated monomers were dried over anhydrous magnesium By the same procedure, the pure BPUR coating without PTFE sulfate for 48 h followed by distillation under reduced pressure (denoted as sample E) was also prepared as a comparison. and then the distillates were stored in fridge. β-Hydroxyethyl The thickness of all cured coatings was about 50-100 µm. methacrylate (HEMA), purchased from JingChun Regent Co. Surface characterization of prepared coatings: The Ltd. (China) and dodecafluoroheptyl methacrylate (DFHMA, static water contact angles (WCA) were measured based on sessile drop method using a contact angle meter (JC2000C1 C11H8O2F12) purchased from XueJia Fluorine-Silicon Chemical Co. Ltd. (China) were used as received. Polytetrafluoroethylene of ZhongChen Digital Technical Apparatus Co. Ltd., China). (PTFE) powders were kindly supplied by XinYing Industrial In a typical process, a deionized water droplet (ca. 5 µL) was Development Co. Ltd. (China). Hexamethylene diisocyanate dropped carefully onto the surface at ambient temperature and trimer curing agent, with trademark of Desmodur N3600, was the images were captured using the accessory digital camera. provided by Bayer Corp. (Germany). All the other regents used All the water contact angle values reported herein were obtained were analytical grade. as averages of five measurements performed on different points Synthesis of hydroxylic fluoroacrylate resin (HFAR): of the sample surface so as to improve the accuracy. The water Hydroxylic fluoroacrylate resin was synthesized by free radical sliding angle (WSA) was defined as the titled angle at which a solution polymerization using benzoyl peroxide (BPO) as water droplet of a certain amount begins to roll off gradually initiator in solvent under the protection of nitrogen gas. The inclined surface. Morphology characterization of the samples synthesis process was employed as follows: In a 250 mL four- surface was conducted by using scanning electron microscopy necked round-bottomed flask equipped with mechanical stirrer, (SEM, Hitachi S-3000N). reflux condenser, dropping funnel and inlet for nitrogen gas, RESULTS AND DISCUSSION 12 g MMA, 24 g butyl acrylate, 6 g HEMA, 8 g DFHMA and 100 mL butyl acetate were mixed and heated. After the solution We made a series of composite coatings based on BPUR was heated to 85 ºC, a solution of 0.8 g BPO in 15 mL ethyl and PTFE at different weight ratios and the wettability of the acetate was added dropwise into the flask. The reaction mixture as-prepared coatings was determined by water contact angle was stirred isothermally at this temperature for 3 h. Afterward, and water sliding angle with the results shown in Table-1. It another amount of 0.2 g BPO in 5 mL ethyl acetate was added can be seen that water contact angle increased and WSA into the flask followed by reaction at 85 ºC for another 3 h. decreased with the increase of PTFE content in coatings. Upon cooling at room temperature, the resulting product was Sample E presented a smooth and transparent surface. The precipitated in n-hexane, filtered, collected and then dried coating adhered strongly to the substrates and had a water under vacuum at 25 ºC for 24 h. The final monomer conversion contact angle (WCA) of 91º, indicating a hydrophobic surface. (C) was 99.2 %, which was calculated by gravimetric analysis To our knowledge, water contact angle on fluoroacrylate was as follows: higher than that on ordinary polyacrylate18. This phenomenon might be attributed to the low surface energy of the coating (Wp − Wi ) C = (1) surface derived from the migration of fluorine-containing units Wm to surface layer during the curing process19. It was found that where Wm is the weight of total monomers, Wp is the weight water contact angle increased sharply from 102º to 144º and of polymer synthesized
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