掺杂氟化聚合物/硅溶胶超疏水复合涂层的制备及性能研究
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摘要
随着科学技术的不断发展，人们对材料性能的要求越来越高。近年来，一种具有超疏水性能的表面，因其诱人的特点引起了各国学者的极大关注。一般说来，超疏水性表面可以通过两种方法制备：一种是在低表面能材料的表面构建粗糙结构；另一种是在粗糙的表面上修饰低表面能的物质。目前，超疏水表面材料的制备由于工艺的限制，以及粗糙表面的构建通常会影响到材料的使用性能，使该材料尚未得到普遍应用。因此采用简单的工艺条件制备具有良好使用性能的超疏水材料是该领域的研究难点。
本文首先采用溶液聚合法，制备了含有疏水性基团-CF_3、-CH_3和-CH_2的低表面能氟化聚合物。该聚合物与高醚化度的三聚氰胺甲醛树脂交联成膜后，对水的接触角达到102(?)，为疏水性涂层。然后，以工艺简单的溶胶．凝胶法原理为基础，控制溶胶和凝胶的形成条件。在水量不足的酸性条件下，使有机／无机前驱体部分水解，控制了缩合过程，且延缓了疏水性有机树脂引入到体系中产生相分离，制备了均匀稳定的含溶胶体系的聚四氟乙烯掺杂氟化聚合物／硅溶胶杂化材料。该材料在基材表面涂敷后，采用表面凝胶化处理技术，将凝胶过程限定在涂层的表面进行。经空气中高温交联成膜，形成了具有微观表面结构和内部均匀密实的超疏水复合涂层。
分别采用FTIR、DSC和XRD等技术手段，对复合材料的特征和特性进行了表征，采用SEM、TEM和XPS等对表面凝胶化处理技术进行了分析讨论。采用JC2000A静滴接触角／界面张力测量仪分别测量了涂层对水的静态接触角和滚动角。采用SEM、AFM和BET等对涂层的表面结构进行了研究，并建立了相应涂层的疏水性模型。最后，对涂层的力学性能和对水的抗渗透性能进行了测量。结果表明，该复合涂层材料不仅具有良好的超疏水性能，而且具有优异的使用性能。其研究得出的主要结论如下：
1、表面凝胶化技术处理的聚四氟乙烯掺杂氟化聚合物／硅溶胶复合涂层，表面和内部化学元素的组成和组织结构具有明显的差异，表面凝胶化处理技术使涂层的凝胶化过程只在涂层表面发生，从而有效地避免了通常条件下凝胶材料干燥引起的开裂。
2、在复合涂层中，经表面凝胶化处理技术以后，使涂层表面生成了二氧化硅粒子，该粒子的直径随着凝胶化时间的增加，pH值的增大而减小。表面凝胶化生成的二氧化硅粒子和掺杂的聚四氟乙烯粒子形成聚集体。其形态为无定形的二氧化硅粒子和晶态的聚四氟乙烯粒子。
3、由于微米级聚四氟乙烯粒子的掺杂和纳米级二氧化硅粒子的生成，涂层表面具有与天然荷叶类似的微米结构和纳米结构相结合的阶层结构，微米结构的高度约为1μm，跨度大约为6.5μm左右。纳米结构的尺度为300nm左右。阶层结构仅在复合涂层表面5μm以内生成，涂层内部则均匀密实。复合涂层表面对水的最大接触角达到155(?)，滚动角最小为9(?)，为超疏水性涂层。
4、复合涂层具有与光滑氟化聚合物涂层相同的附着力、柔韧性和硬度。复合涂层的耐冲击强度虽略有下降，但该强度仍然符合船舶、桥梁及钢结构对表面涂层冲击强度的要求。经电化学交流阻抗测试，与光滑氟化聚合物涂层相比，复合涂层具有更强的抗腐蚀性介质渗透的能力。
5、建立了氟化聚合物涂层光滑表面的润湿行为，即基团等概率分布排列模型，该模型较好地解释了氟化聚合物涂层光滑表面的润湿行为。
6、对于复合涂层表面的润湿行为，在粗糙度较低时，基本接近Wenzel模型；而在粗糙度较高时，基本接近Cassie模型。假设复合涂层表面的微米结构与纳米结构相结合的阶层结构类似于Koch曲线所描述的分形结构，并以分形结构方程为基础建立了复合涂层的超疏水分形结构模型，该模型所得出的结果与复合涂层表面的润湿行为基本一致。
With the constant development of science and technology, the requirement for material properties becomes higher and higher. Scientists give more attention to super-hydrophobic surface during recent years, it is now playing a more and more importance role in surface science for it's attracted potential industry applications. Conventionally, super-hydrophobic surface has been produced mainly in two ways. One is to create a rough structure on a hydrophobic surface, and the other is to modify a rough surface by materials with low surface free energy. Unfortunately, it rather difficult to prepare this kind of material by applied process due to the limitation of their own characteristics. Simple process conditions for preparation super-hydrophobic materials with good mechanical properties are a difficulty in this field.
In this paper, the fluorinater acrylate polymer with hydrophobic groups -CF_3, -CH_3 and -CH_2 has been synthesized by radical copolymerization, the hydrophobic coating with water contact angle 102~(?) was prepared by crosslinking with HMMM. The well-proportioned composite sols were prepared by using simple sol-gel technology with tetraethyl orthosilicate (TEOS) and methyl triethoxy silane (MTES) as the precursors in alcohol-soluble fluorinated polymer solution with PTFE doping under the hydrochloric acid and deficiency of water conditions. alkoxides were partly hydrolyzed, the condensation process was suppressed due to the deficient amount of water available in the system and in hydrochloric acid medium, this deficiency of water prevented phase segregation that has a tendency to occur due to the organic polymer introduced into the systems. After the surface of material was coated by composite sol, the composite coating was formed on substrate surface through the surface gelation treatment technology, the gelation occurred only on the composite coating surface, and condensation polymerizing - cross at high temperature. The close-grained coating with microstructure surface was prepared.
Physical techniques including FTIR, DSC, XRD, SEM, TEM, XPS and JC2000A were applied to investigate the characteristic of the hybrid materials, results of the surface gelation treatment and hydrophobicity of the composite coatings. The hydrophobic models in the surfaces of the coatings were discussed, the mechanical properties and water proof performance of the composite coatings were measured. The results are as bellow:
1. The PTFE doping fluoropolymer/silica sol composite coating is considerable different between the chemical compositions from surface to the interior of the coating, the gelation only on the surface of the composite coating, the collapse of the gel network is avoided during drying.
2. The silica dioxide particles were obtained after the composite coating was surface gelation treated in the surface of coating. The sizes of the silica dioxide particles were decreased with the increase of pH values and the rising of treatment times. The agglomerates were consisting of amorphous silica dioxide particles and crystalline PTFE particles.
3. The angles for the composite coating were 155°and 9°for water contact angle and water sliding angle repectively, the composite coating prepared by this means was super-hydrophobic. SEM and AFM results indicated that there existed micro- and nanoscale hierarchical structures on the surface of the coating, it is very similar to the structure of the surface of a lotus leaf. The drop height of agglomerates was estimated at 1μm, the interval between two agglomerates was estimated at 6.5μm, the size of silica dioxide particle was estimated at 300 nm. The microstructure could only formed to the place of 5μm under surface, and tightness and continuity inside the coating.
4. The results of the experiment reveal that adhesion, flexility and rigidity of the composite coating were as good as that of the fluorinated acrylate copolymer coating, although the impact intensity of composite coating was decreased consistent with the requirements of ship, bridge and steel structure and so on. The results of electrochemical impedance spectroscopy showed the composite coating has much stronger resistance ability to corrosive medium permeation of the coating, comparing with the fluorinated acrylate copolymer coating.
5. In order to reveal the hydrophobic nature of the cross-linked fluorinated acrylate copolymer smooth coating theoretically, the equal probabilistic distribution model was set up, The results were in good agreement with experiments.
6. The wetting behavior of the composite coating surface exhibited Wenzel model when the surface's roughness was lower enough, and Cassie model was available at higher enough. It was assumed that the hierarchical structures of the composite coating were agree with the fractal structures described by Koch curve. Based on the fractal structure equation, the super-hydrophobic fractal structure model of the composite coating was constructed, the model agrees with the experimental data well.
本文首先采用溶液聚合法，制备了含有疏水性基团-CF_3、-CH_3和-CH_2的低表面能氟化聚合物。该聚合物与高醚化度的三聚氰胺甲醛树脂交联成膜后，对水的接触角达到102(?)，为疏水性涂层。然后，以工艺简单的溶胶．凝胶法原理为基础，控制溶胶和凝胶的形成条件。在水量不足的酸性条件下，使有机／无机前驱体部分水解，控制了缩合过程，且延缓了疏水性有机树脂引入到体系中产生相分离，制备了均匀稳定的含溶胶体系的聚四氟乙烯掺杂氟化聚合物／硅溶胶杂化材料。该材料在基材表面涂敷后，采用表面凝胶化处理技术，将凝胶过程限定在涂层的表面进行。经空气中高温交联成膜，形成了具有微观表面结构和内部均匀密实的超疏水复合涂层。
分别采用FTIR、DSC和XRD等技术手段，对复合材料的特征和特性进行了表征，采用SEM、TEM和XPS等对表面凝胶化处理技术进行了分析讨论。采用JC2000A静滴接触角／界面张力测量仪分别测量了涂层对水的静态接触角和滚动角。采用SEM、AFM和BET等对涂层的表面结构进行了研究，并建立了相应涂层的疏水性模型。最后，对涂层的力学性能和对水的抗渗透性能进行了测量。结果表明，该复合涂层材料不仅具有良好的超疏水性能，而且具有优异的使用性能。其研究得出的主要结论如下：
1、表面凝胶化技术处理的聚四氟乙烯掺杂氟化聚合物／硅溶胶复合涂层，表面和内部化学元素的组成和组织结构具有明显的差异，表面凝胶化处理技术使涂层的凝胶化过程只在涂层表面发生，从而有效地避免了通常条件下凝胶材料干燥引起的开裂。
2、在复合涂层中，经表面凝胶化处理技术以后，使涂层表面生成了二氧化硅粒子，该粒子的直径随着凝胶化时间的增加，pH值的增大而减小。表面凝胶化生成的二氧化硅粒子和掺杂的聚四氟乙烯粒子形成聚集体。其形态为无定形的二氧化硅粒子和晶态的聚四氟乙烯粒子。
3、由于微米级聚四氟乙烯粒子的掺杂和纳米级二氧化硅粒子的生成，涂层表面具有与天然荷叶类似的微米结构和纳米结构相结合的阶层结构，微米结构的高度约为1μm，跨度大约为6.5μm左右。纳米结构的尺度为300nm左右。阶层结构仅在复合涂层表面5μm以内生成，涂层内部则均匀密实。复合涂层表面对水的最大接触角达到155(?)，滚动角最小为9(?)，为超疏水性涂层。
4、复合涂层具有与光滑氟化聚合物涂层相同的附着力、柔韧性和硬度。复合涂层的耐冲击强度虽略有下降，但该强度仍然符合船舶、桥梁及钢结构对表面涂层冲击强度的要求。经电化学交流阻抗测试，与光滑氟化聚合物涂层相比，复合涂层具有更强的抗腐蚀性介质渗透的能力。
5、建立了氟化聚合物涂层光滑表面的润湿行为，即基团等概率分布排列模型，该模型较好地解释了氟化聚合物涂层光滑表面的润湿行为。
6、对于复合涂层表面的润湿行为，在粗糙度较低时，基本接近Wenzel模型；而在粗糙度较高时，基本接近Cassie模型。假设复合涂层表面的微米结构与纳米结构相结合的阶层结构类似于Koch曲线所描述的分形结构，并以分形结构方程为基础建立了复合涂层的超疏水分形结构模型，该模型所得出的结果与复合涂层表面的润湿行为基本一致。
With the constant development of science and technology, the requirement for material properties becomes higher and higher. Scientists give more attention to super-hydrophobic surface during recent years, it is now playing a more and more importance role in surface science for it's attracted potential industry applications. Conventionally, super-hydrophobic surface has been produced mainly in two ways. One is to create a rough structure on a hydrophobic surface, and the other is to modify a rough surface by materials with low surface free energy. Unfortunately, it rather difficult to prepare this kind of material by applied process due to the limitation of their own characteristics. Simple process conditions for preparation super-hydrophobic materials with good mechanical properties are a difficulty in this field.
In this paper, the fluorinater acrylate polymer with hydrophobic groups -CF_3, -CH_3 and -CH_2 has been synthesized by radical copolymerization, the hydrophobic coating with water contact angle 102~(?) was prepared by crosslinking with HMMM. The well-proportioned composite sols were prepared by using simple sol-gel technology with tetraethyl orthosilicate (TEOS) and methyl triethoxy silane (MTES) as the precursors in alcohol-soluble fluorinated polymer solution with PTFE doping under the hydrochloric acid and deficiency of water conditions. alkoxides were partly hydrolyzed, the condensation process was suppressed due to the deficient amount of water available in the system and in hydrochloric acid medium, this deficiency of water prevented phase segregation that has a tendency to occur due to the organic polymer introduced into the systems. After the surface of material was coated by composite sol, the composite coating was formed on substrate surface through the surface gelation treatment technology, the gelation occurred only on the composite coating surface, and condensation polymerizing - cross at high temperature. The close-grained coating with microstructure surface was prepared.
Physical techniques including FTIR, DSC, XRD, SEM, TEM, XPS and JC2000A were applied to investigate the characteristic of the hybrid materials, results of the surface gelation treatment and hydrophobicity of the composite coatings. The hydrophobic models in the surfaces of the coatings were discussed, the mechanical properties and water proof performance of the composite coatings were measured. The results are as bellow:
1. The PTFE doping fluoropolymer/silica sol composite coating is considerable different between the chemical compositions from surface to the interior of the coating, the gelation only on the surface of the composite coating, the collapse of the gel network is avoided during drying.
2. The silica dioxide particles were obtained after the composite coating was surface gelation treated in the surface of coating. The sizes of the silica dioxide particles were decreased with the increase of pH values and the rising of treatment times. The agglomerates were consisting of amorphous silica dioxide particles and crystalline PTFE particles.
3. The angles for the composite coating were 155°and 9°for water contact angle and water sliding angle repectively, the composite coating prepared by this means was super-hydrophobic. SEM and AFM results indicated that there existed micro- and nanoscale hierarchical structures on the surface of the coating, it is very similar to the structure of the surface of a lotus leaf. The drop height of agglomerates was estimated at 1μm, the interval between two agglomerates was estimated at 6.5μm, the size of silica dioxide particle was estimated at 300 nm. The microstructure could only formed to the place of 5μm under surface, and tightness and continuity inside the coating.
4. The results of the experiment reveal that adhesion, flexility and rigidity of the composite coating were as good as that of the fluorinated acrylate copolymer coating, although the impact intensity of composite coating was decreased consistent with the requirements of ship, bridge and steel structure and so on. The results of electrochemical impedance spectroscopy showed the composite coating has much stronger resistance ability to corrosive medium permeation of the coating, comparing with the fluorinated acrylate copolymer coating.
5. In order to reveal the hydrophobic nature of the cross-linked fluorinated acrylate copolymer smooth coating theoretically, the equal probabilistic distribution model was set up, The results were in good agreement with experiments.
6. The wetting behavior of the composite coating surface exhibited Wenzel model when the surface's roughness was lower enough, and Cassie model was available at higher enough. It was assumed that the hierarchical structures of the composite coating were agree with the fractal structures described by Koch curve. Based on the fractal structure equation, the super-hydrophobic fractal structure model of the composite coating was constructed, the model agrees with the experimental data well.
引文
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