徐亚洲,何瑾馨,朱卫彪,董霞,赵强强.基于含氟改性笼状倍半硅氧烷一步法制备透明超疏水涂层[J].表面技术,2022,51(10):336-343.
XU Ya-zhou,HE Jin-xin,ZHU Wei-biao,DONG Xia,ZHAO Qiang-qiang.Transparent Superhydrophobic Coating Prepared by One-step Method Based on Fluorinated Cage-like Sesimiloxane[J].Surface Technology,2022,51(10):336-343
基于含氟改性笼状倍半硅氧烷一步法制备透明超疏水涂层
Transparent Superhydrophobic Coating Prepared by One-step Method Based on Fluorinated Cage-like Sesimiloxane
  
DOI:10.16490/j.cnki.issn.1001-3660.2022.10.036
中文关键词:  POSS  超疏水涂层  透明  耐用  喷涂  相分离  紫外光固化
英文关键词:superhydrophobic coating  transparent  durable  spraying  phase separation  UV curing
基金项目:国家重点研发计划项目(2017YFB0309100)
作者单位
徐亚洲 东华大学 化学化工与生物工程学院,上海 201620 
何瑾馨 东华大学 化学化工与生物工程学院,上海 201620 ;纺织面料技术教育部重点实验室,上海 201620 
朱卫彪 东华大学 化学化工与生物工程学院,上海 201620 
董霞 东华大学 化学化工与生物工程学院,上海 201620 ;国家染整工程技术研究中心,上海 201620 
赵强强 东华大学 化学化工与生物工程学院,上海 201620 ;纺织面料技术教育部重点实验室,上海 201620 
AuthorInstitution
XU Ya-zhou School of Chemistry, Chemical Engineering and Biotechnology, Shanghai 201620, China 
HE Jin-xin School of Chemistry, Chemical Engineering and Biotechnology, Shanghai 201620, China;Key Lab of Textile Science & Technology, Ministry of Education,Shanghai 201620, China 
ZHU Wei-biao School of Chemistry, Chemical Engineering and Biotechnology, Shanghai 201620, China 
DONG Xia School of Chemistry, Chemical Engineering and Biotechnology, Shanghai 201620, China;National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, Shanghai 201620, China 
ZHAO Qiang-qiang School of Chemistry, Chemical Engineering and Biotechnology, Shanghai 201620, China;Key Lab of Textile Science & Technology, Ministry of Education,Shanghai 201620, China 
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中文摘要:
      目的 为了研究出一种在光滑镜面基材上大面积制备透明耐用的超疏水涂层,需要克服当前超疏水涂层存在的理化稳定性差、光学透明度不高以及制备繁琐、难以大面积实施等问题。方法 通过向聚氨酯丙烯酸酯疏水性光固化树脂体系中引入含氟低表面能改性的笼状倍半硅氧烷(POSS),结合喷涂法和相分离法在聚碳酸酯(PC)表面制备了一种超疏水光固化涂层。探究了低表面能改性POSS的掺杂量和乙醇添加量对构筑超疏水涂层的影响。结果 当POSS-SH-DFMA7的掺杂量为树脂含量的40%、乙醇的添加量为溶剂THF的25%时,涂层表现出优异的超疏水特性,静态水接触角和滑动角分别可达到156.92°和3.24°;良好的光学透明性,光线透过率为85.63%;可靠的机械稳定性,承受6 h的水滴冲击后依然保持超疏水特性;稳定的耐候和耐化学性,经历户外环境和不同pH值化学试剂的侵蚀后仍可保持涂层原有的润湿性能。结论 在光固化树脂体系中引入一定量的含氟单体改性POSS结合乙醇的作用可以一步法制备出透明、理化性能稳定的超疏水涂层。
英文摘要:
      The coating film-forming method has good application prospects in the preparation of transparent superhydrophobic coatings due to its simple process, good repeatability and low equipment requirements. However, the nanofillers in the existing coating film-forming methods generally have defects such as easy aggregation and poor durability. POSS is an organic- inorganic hybrid with a special cage-like structure. Compared with ordinary nanofillers, POSS has the characteristics of monodispersity and flexible functional modification. At present, most of the researches on POSS in the field of superhydrophobic coatings are based on rough substrate surfaces, but few researches have been done in the field of mirror-transparent optics. Therefore, the purpose of this study is to select POSS as a nanofiller and use a one-step coating film-forming method to construct a large-area transparent and durable superhydrophobic coating on a mirror substrate.In this study, an intermediate POSS-SH8 was synthesized from octavinyl POSS and ethanedithiol based on a two-step thiol-ene click chemistry reaction. Then, POSS-SH8 and dodecafluoroheptyl methacrylate monomer were used as reactants to obtain low surface energy modified product POSS-SH-DFMA7 through photoreaction. The effects of the doping mass fraction of F-POSS and the volume fraction of ethanol addition on the construction of superhydrophobic coatings were explored. The preparation of spraying prefabricated liquid was as follows: F-POSS with different mass fractions was blended in resin prepolymer. Resin prepolymer was composed of a mixture of hydrophobic photocurable resin (Changxing 6145-100) and diluent HDDA at 4∶1. After the prepolymer was evenly mixed, the dilution solvent THF was added to the system at a dilution ratio of 1∶20. It was dispersed uniformly in a stirrer and an ultrasonic shaker successively. In order to obtain the rough micro-nano composite structure on the smooth substrate surface, the method of spraying combined with non-solvent induced phase separation was adopted in this study. Different volume fractions of non-solvent ethanol were added to the above system to obtain a series of spraying prefabricated liquids. Next, the prefabricated solution was transferred to the surface of the smooth substrate by spraying and the coating was air-dried at room temperature. Finally, the air-dried coatings were cured in a UV curing apparatus under N2 atmosphere for 5 minutes. The chemical composition of the main substances in the obtained samples was analyzed by infrared spectrum curve. The static water contact angle and dynamic rolling angle of the coatings were recorded by contact angle analysis and self-made rolling angle measuring instrument to characterize the hydrophobicity of the coatings. The surface topography and roughness of the composite coatings with different rough structures were investigated by scanning electron microscopy and three-dimensional ultra-depth-of-field microscopy. The transmittance of the coatings was measured by a UV spectrophotometer to characterize the transmittance of the coating. A self-made device was used to set water droplets to be released at a uniform rate of 2 drops per second at a height of 30 cm. The hydrophobic property retention curve of the coatings at different times were obtained to characterize the mechanical stability of the coating. The three superhydrophobic coatings were placed in an outdoor open-air environment, and their contact angle changes were recorded every 3 days to evaluate their weatherability. In addition, the above three coatings were soaked in HCl and NaOH solutions with pH values ​​of 1 to 14 for 24 hours. And the contact angle curves of each coating at different pH values ​​were recorded to compare their resistance to reagents.The research results show that the coating exhibits excellent superhydrophobic properties when the doping mass fraction of POSS-SH-DFMA7 is 40% of the resin content and the addition volume fraction of ethanol is 25%. The static water contact angle and sliding angle can reach 156.92° and 3.24°, respectively. In addition, the superhydrophobic coating prepared under the optimal process conditions also has good optical transparency and its light transmittance is 85.63%. The coating still maintains superhydrophobic property after being impacted by water droplets for 6 hours, indicating its mechanical stability. Not only that, the original wetting property of the coating can still be maintained after experiencing various outdoor environments and the erosion of chemical agents with different pH values. Therefore, the introduction of a certain amount of fluorine-containing monomer to modify the POSS combined with the phase separation of ethanol into the photocurable resin system can prepare a large-area transparent and superhydrophobic coating with stable physical and chemical properties in one step.
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