超疏水铝合金表面的仿生构建
摘要
超疏水表面因其独特的性能和潜在的应用前景引起了广泛的研究兴趣,但对金属超疏水表面的制备和性能研究才刚刚起步。本文通过对制备铝合金超疏水材料的常规化学处理液、电解液的科学配方和工艺参数进行了系统研究,并采用普通有机材料对铝合金表面进行修饰改性,探索一种用化学、电化学方法生成微纳米表面与高分子材料覆膜改性相结合的制备方法,构建了具有微米或微纳米结构的铝合金超疏水表面。多层次有序地展开了对超疏水铝合金表面综合性能的研究,旨在开发具有产业化应用前景的制备方法,并获得具有稳定微纳米结构和超疏水性能的铝合金新材料,为实现进一步产业化生产和推广提供理论支持,论文的主要研究内容和创新点如下：
1.以铝镁合金和铝锰合金为基材,分别采用酸刻蚀法、原电池腐蚀法、硝酸盐法、磷酸-铬酸盐法、硫酸阳极氧化法制备了超疏水铝合金纹理粗糙表面,进行了表面微观结构和化学组分的分析。粗糙表面经硬脂酸(SA)乙醇溶液浸涂后,均实现了超疏水特性,接触角大于150。,滚动角小于10。。表面形成的不规则多孔结构与荷叶表面乳突结构的尺寸类似,孔深约5-25μm,孔径约5-20μm。以经酸刻蚀法、原电池腐蚀法、硫酸阳极氧化法和磷酸-铬酸盐法制备的表面较为光整。
2.对铝合金超疏水表面的润湿特性和稳定性进行了研究,分析了纹理刻蚀表面的粗糙度对疏水性能的影响,研究发现表面粗糙度的增加可以增强表面的疏水性。分析了覆膜材料和工艺对表面润湿性的影响,亲水性的铝合金刻蚀后具有超亲水性,分别经浸覆聚丙烯、聚苯乙烯、马来酸酐接枝聚丙烯和硅烷-聚丙烯膜,均实现了超疏水性,改性聚丙烯还可增加表面的疏水性能。对超疏水表面的润湿特性和稳定性进行了分析,实验发现超疏水表面在pH为5～11的溶液和浓度小于5%的有机溶剂中能保持良好的疏液特性和稳定性,在相对湿度为30%～70%,温度变化范围为10℃～40℃的环境中,仍能保持长期的疏水稳定性,聚丙烯覆膜表面在100℃下可保持良好的疏水稳定性。相比硬脂酸、聚乙烯、高密度聚乙烯、聚苯乙烯覆膜表面,硬脂酸膜表面具有室温长效稳定性,聚丙烯膜表面具有更好的超疏水性和力学性能。
3.探寻了不同的酸刻蚀剂组方的刻蚀效果及对表面疏水性能的影响,实验表明相同化学成分的物质因其表面结构不同,显示出不同的润湿特性。对不同的酸溶液浓度及浸泡时间对疏水性的影响进行了分析,得到了0.08mol/L草酸与1mol/L盐酸溶液混合刻蚀15h及1%硬脂酸乙醇溶液浸泡30min的最佳反应条件,并简略分析了这种微细结构的形成机理。通过盐酸,草酸混合刻蚀与低表面能物质硬脂酸修饰相结合的方法成功制备出了铝合金基体上的超疏水表面,并以此方法获得了适用于实际应用的短时间制备方法。
4.研究了硫酸阳极氧化工艺和覆膜工艺对构建铝合金超疏水表面的影响,获得了最大接触角可达162.0。,最小滚动角为2.0。的铝合金超疏水表面。铝合金经过硫酸阳极氧化后生成了无规多孔的微纳米二级结构,经覆膜处理后表面呈微米球和微米孔复合结构。对比了聚丙烯、聚苯乙烯、马来酸酐接枝聚丙烯和硅烷-聚丙烯膜四种不同覆膜表面对润湿性的影响,硅烷-聚丙烯膜的疏水性能最佳,并且有更好的耐久性。以此方法对某企业现有阳极氧化工艺进行了改进,得到了最佳工艺参数,即：1.803mol/L的硫酸、0.068mol/L的重铬酸钾、0.079mol/L的草酸、2.57mol/L的氯化钠和1.37mol/L的甘油；以铝片为阳极,石墨为阴极；控制电流密度为1.2A/dm2,反应时间均为30min。
5.通过原电池腐蚀法用廉价的氯化钠为电解质溶液成功构建了由铝表面不规则多孔结构构成的超疏水硬脂酸盐膜表面,接触角值达到154°。表面孔径约15-20μm,孔深约5-10μm,与荷叶表面微细结构尺寸类似。分析了氯化钠溶液中的C1-对表面形成多孔结构的原理以及其对构建铝合金超疏水表面的影响,研究发现微米级多孔结构的尺度大小是构建超疏水表面的关键因素之一,而纳米粒子的聚集有助于提高表面的疏水性。
6.对铝合金超疏水表面的自清洁性、防冻抑霜性、抑菌性、耐蚀性进行了研究,研究结果表明超疏水铝合金表面具有良好的自清洁性能。在结冰温度下超疏水铝合金表面具有延迟冻结与抑霜功能,从润湿性理论和热力学理论分析了产生这一现象的原因。通过奎因法、贴膜法、振荡烧瓶法测试了超疏水铝合金表面的抑菌性能,研究表明超疏水铝合金样片对大肠杆菌、金黄色葡萄球菌的抑菌率随着接触角的增大而明显提高,当接触角达到164°时抑菌率分别可达到89.7%和91.2%。通过极化曲线的测定及不同pH值溶液下的浸泡实验,发现超疏水铝合金较普通铝合金具有更好的耐盐腐蚀性能,弱酸和弱碱环境中的耐腐蚀性较好,但强酸和强碱环境中的耐腐蚀性能不佳。
7.对聚丙烯超疏水铝合金表面的结合力与耐久性改进及其机理进行了研究,研究表明硅烷化处理有助于提高铝合金与聚丙烯或马来酸酐接枝聚丙烯涂层的结合力,在铝合金表面形成了一层高分子层聚硅氧烷,并形成了化学键Si-O-Al。马来酸酐接枝聚丙烯提高了涂层的极性,在一定程度上降低了涂层表面的超疏水性能,但加涂一层聚丙烯,表面的超疏水性会得到改善。其疏水性与涂覆溶液浓度有关,添加纳米颗粒,不仅促进了涂层结构的疏水性并使结构更加稳定。
Superhydrophobic surfaces were attracted much attention because of their unique properties and potential applications, but the preparation and performance study of metal superhydrophobic surfaces has just begun. In this dissertation, five kinds of methods were used to fabricate aluminum superhydrophobic surfaces. The structure and properties of the surface were studied systematically. At the same time, the process parameters were also optimized by experiments. In order to obtain a superior superhydrophobic surface, some chemical and electrochemical methods were explored to form micro-nano structures of aluminum superhydrophobic surfaces, and then some polymer materials were coated on the aluminum surface. The performance of superhydrophobic aluminum surfaces was studied sequentially for industrial applications. The main work and innovation of the dissertation are listed as following:
1. Al-Mg alloy and Al-Mn alloy substrates were etched by some methods such us acid etching method, galvanic corrosion method, nitrate method, phosphoric acid-dichromate method and sulfuric acid anodizing method to form rough texture of surface on aluminum alloy. And then the microstructure and chemical components of the surface were analyzed. When rough surfaces were immersed in stearic acid ethanol solution, a superhydrophobicity was obtained. As a result, the contact angles were larger than150°, and sliding angles were lower than10°. The size of irregular porous on surface was similar to the size of papilla on Lotus leaf surfaces. These holes were about between5to30μm in depth, and5to20μm in width. Surfaces were relative smooth and stable when it was prepared by acid etching, galvanic corrosion method, sulfuric acid anodizing method and phosphoric acid-dichromate method.
2. The wettability and stability of aluminum alloy superhydrophobic surfaces were studied. On the basis of Wenzel and Cassie models, the relationship between the roughness of the etched surface and superhydrophobicity was also investigated. The results indicated that the roughness on surface greatly enhanced the hydrophobicity of aluminum alloy surfaces. To analyze the relationship between wettability of the surface and coating process, the aluminum alloys were etched before its wettability transformed from hydrophilicity to superhydrophilicity. When they were coated with organic materials such as polypropylene (PP), polystyrene (PS) or maleic anhydride grafted polypropylene (PP-g-MAH), these surfaces were obtained superhydrophobicity. Among these materials, modified PP enhanced the hydrophobicity mostly. The wetting investigation showed that the superhydrophobicity could maintain in a wide pH range, and keep stable when it were immersed in organic solvent (concentration:<5%), and viarous influence factors such us relative humidity (30-70%), temperature range (10-40℃) and environment. In particular, PP film's surface could maintain a good hydrophobicity stability at100℃. Compared with the surfaces such as stearic acid (SA), polyethylene (PE), high-density polyethylene (HDPE), and PS film, and the SA film had long-term stability at room temperature. Obviously, PP film's surface had better superhydrophobicity and mechanical properties than others had.
3. The influence factors of the different acid etchant were studied in the preparation of superhydrophobic aluminum alloy surface, and the relationship between it and superhydrophobicity was also researched. The results showed that the different surface structures had the different wetting characteristics on the same chemical composition substances. Process were analyzed such as the concentration of acid solution and the immersion time, the best reaction conditions was expressed as follows:0.08mol/L oxalic acid and1mol/L hydrochloric acid solution at etching15hours and1%stearic acid ethanol solution at immersing30minutes. At the same time, the formation mechanism of this microstructure was analyzed.
4. The anodizing process by using sulfuric acid method and film-covered was studied. The water contact angle and sliding angle of superhydrophobic aluminum alloy surface were162°and2°, respectively. The composite structure surface was formed by coating with organic materials on micro-nano alloy substrates which were prepared by anodic oxidation method. Micro spheres and micropores presented these composite surfaces. Among of PP, PS, PP-g-MAH and the silane-PP films, the hydrophobic properties of the PP films pretreated by silane angent was the best one with a superior durability. Finally, the optimal process parmeter is:1.803mol/L sulfuric acid,0.068mol/L potassium dichromate,0.079mol/L oxalic acid,0.257mol/L sodium chloride and1.37mol/L glycerin; aluminum plate was designed as a anode and graphite was a cathode; current density was controlled as1.2A/dm2, and reaction time was30min.
5. Galvanic corrosion method was successfully used to prepare irregular porous structures on aluminum surfaces, sodium chloride solution was electrolyte solution and surfaces were coated stearic acid, the contact angle was154°. These holes were about between5to20μm in depth, and15to20μm in width, the size of the holes was similar to the size of the Lotus leaf surfaces'. The chloride ion played an important role in sodium chloride solution, the composition principle of surface porous structure. The relationship between the concentration of chloride ion in solution cell and superhydrophobicity were studied, the studies indicated that the size of the micron porous structure was a key factor which formed a superhydrophobic surface, and the accumulation of the nanoparticles could help to improve the hydrophobicity of the surfaces.
6. The properties of aluminum alloy superhydrophobic surfaces were studied, such as self-cleaning, anti-freezing, bacteriostasis and anti-corrosion. The research results showed that the superhydrophobic aluminum surface had good self-cleaning properties, and it can anti-freezing and anti-frosting under the freezing point. This phenomenon was analyzed with wettability theory and thermodynamics theory. The bacteriostasis properties of superhydrophobic aluminum surface were tested by quine method, sticking membrane method and shake flask test. The studies showed that the bacteriostasis properties of superhydrophobic aluminum samples was enhanced with the increase of the contact angle, the bacteriostasis rate was89.7%and91.2%when the contact angle was164°. The results indicated that superhydrophobic aluminum alloys had better anti-corrosion to salt than that of ordinary aluminums by polarization curve measurement and corrosion weight loss tests of different PH solutions. The studies were also showed that anti-corrosion of superhydrophobic aluminum alloys is well in weak acid and weak alkali environments, while it deteriorated in strong acid and strong alkali environments.
7. The binding force and the mechanism of durability of PP superhydrophobic aluminum alloy surface were studied. The studies showed that the binding force of aluminum alloy and PP (or PP-g-MAH coating) could be improved by silanization. A polysiloxane layer was formed in aluminum alloy surface with the Si-O-Al chemical bond. However, the superhydrophobic properties of the surface coating were decreased to some extent because the polarity of the coated film could be improved with PP-g-MAH. The superhydrophobic properties of the surface could be improved when PP was coated. The concentration of the PP solution has an important effect on the hydrophobicity. Furthermore, the addition of nanoparticles can not only improve the hydrophobicity of the coating structure, but also increase the stability of the structure.
1.以铝镁合金和铝锰合金为基材,分别采用酸刻蚀法、原电池腐蚀法、硝酸盐法、磷酸-铬酸盐法、硫酸阳极氧化法制备了超疏水铝合金纹理粗糙表面,进行了表面微观结构和化学组分的分析。粗糙表面经硬脂酸(SA)乙醇溶液浸涂后,均实现了超疏水特性,接触角大于150。,滚动角小于10。。表面形成的不规则多孔结构与荷叶表面乳突结构的尺寸类似,孔深约5-25μm,孔径约5-20μm。以经酸刻蚀法、原电池腐蚀法、硫酸阳极氧化法和磷酸-铬酸盐法制备的表面较为光整。
2.对铝合金超疏水表面的润湿特性和稳定性进行了研究,分析了纹理刻蚀表面的粗糙度对疏水性能的影响,研究发现表面粗糙度的增加可以增强表面的疏水性。分析了覆膜材料和工艺对表面润湿性的影响,亲水性的铝合金刻蚀后具有超亲水性,分别经浸覆聚丙烯、聚苯乙烯、马来酸酐接枝聚丙烯和硅烷-聚丙烯膜,均实现了超疏水性,改性聚丙烯还可增加表面的疏水性能。对超疏水表面的润湿特性和稳定性进行了分析,实验发现超疏水表面在pH为5～11的溶液和浓度小于5%的有机溶剂中能保持良好的疏液特性和稳定性,在相对湿度为30%～70%,温度变化范围为10℃～40℃的环境中,仍能保持长期的疏水稳定性,聚丙烯覆膜表面在100℃下可保持良好的疏水稳定性。相比硬脂酸、聚乙烯、高密度聚乙烯、聚苯乙烯覆膜表面,硬脂酸膜表面具有室温长效稳定性,聚丙烯膜表面具有更好的超疏水性和力学性能。
3.探寻了不同的酸刻蚀剂组方的刻蚀效果及对表面疏水性能的影响,实验表明相同化学成分的物质因其表面结构不同,显示出不同的润湿特性。对不同的酸溶液浓度及浸泡时间对疏水性的影响进行了分析,得到了0.08mol/L草酸与1mol/L盐酸溶液混合刻蚀15h及1%硬脂酸乙醇溶液浸泡30min的最佳反应条件,并简略分析了这种微细结构的形成机理。通过盐酸,草酸混合刻蚀与低表面能物质硬脂酸修饰相结合的方法成功制备出了铝合金基体上的超疏水表面,并以此方法获得了适用于实际应用的短时间制备方法。
4.研究了硫酸阳极氧化工艺和覆膜工艺对构建铝合金超疏水表面的影响,获得了最大接触角可达162.0。,最小滚动角为2.0。的铝合金超疏水表面。铝合金经过硫酸阳极氧化后生成了无规多孔的微纳米二级结构,经覆膜处理后表面呈微米球和微米孔复合结构。对比了聚丙烯、聚苯乙烯、马来酸酐接枝聚丙烯和硅烷-聚丙烯膜四种不同覆膜表面对润湿性的影响,硅烷-聚丙烯膜的疏水性能最佳,并且有更好的耐久性。以此方法对某企业现有阳极氧化工艺进行了改进,得到了最佳工艺参数,即：1.803mol/L的硫酸、0.068mol/L的重铬酸钾、0.079mol/L的草酸、2.57mol/L的氯化钠和1.37mol/L的甘油；以铝片为阳极,石墨为阴极；控制电流密度为1.2A/dm2,反应时间均为30min。
5.通过原电池腐蚀法用廉价的氯化钠为电解质溶液成功构建了由铝表面不规则多孔结构构成的超疏水硬脂酸盐膜表面,接触角值达到154°。表面孔径约15-20μm,孔深约5-10μm,与荷叶表面微细结构尺寸类似。分析了氯化钠溶液中的C1-对表面形成多孔结构的原理以及其对构建铝合金超疏水表面的影响,研究发现微米级多孔结构的尺度大小是构建超疏水表面的关键因素之一,而纳米粒子的聚集有助于提高表面的疏水性。
6.对铝合金超疏水表面的自清洁性、防冻抑霜性、抑菌性、耐蚀性进行了研究,研究结果表明超疏水铝合金表面具有良好的自清洁性能。在结冰温度下超疏水铝合金表面具有延迟冻结与抑霜功能,从润湿性理论和热力学理论分析了产生这一现象的原因。通过奎因法、贴膜法、振荡烧瓶法测试了超疏水铝合金表面的抑菌性能,研究表明超疏水铝合金样片对大肠杆菌、金黄色葡萄球菌的抑菌率随着接触角的增大而明显提高,当接触角达到164°时抑菌率分别可达到89.7%和91.2%。通过极化曲线的测定及不同pH值溶液下的浸泡实验,发现超疏水铝合金较普通铝合金具有更好的耐盐腐蚀性能,弱酸和弱碱环境中的耐腐蚀性较好,但强酸和强碱环境中的耐腐蚀性能不佳。
7.对聚丙烯超疏水铝合金表面的结合力与耐久性改进及其机理进行了研究,研究表明硅烷化处理有助于提高铝合金与聚丙烯或马来酸酐接枝聚丙烯涂层的结合力,在铝合金表面形成了一层高分子层聚硅氧烷,并形成了化学键Si-O-Al。马来酸酐接枝聚丙烯提高了涂层的极性,在一定程度上降低了涂层表面的超疏水性能,但加涂一层聚丙烯,表面的超疏水性会得到改善。其疏水性与涂覆溶液浓度有关,添加纳米颗粒,不仅促进了涂层结构的疏水性并使结构更加稳定。
Superhydrophobic surfaces were attracted much attention because of their unique properties and potential applications, but the preparation and performance study of metal superhydrophobic surfaces has just begun. In this dissertation, five kinds of methods were used to fabricate aluminum superhydrophobic surfaces. The structure and properties of the surface were studied systematically. At the same time, the process parameters were also optimized by experiments. In order to obtain a superior superhydrophobic surface, some chemical and electrochemical methods were explored to form micro-nano structures of aluminum superhydrophobic surfaces, and then some polymer materials were coated on the aluminum surface. The performance of superhydrophobic aluminum surfaces was studied sequentially for industrial applications. The main work and innovation of the dissertation are listed as following:
1. Al-Mg alloy and Al-Mn alloy substrates were etched by some methods such us acid etching method, galvanic corrosion method, nitrate method, phosphoric acid-dichromate method and sulfuric acid anodizing method to form rough texture of surface on aluminum alloy. And then the microstructure and chemical components of the surface were analyzed. When rough surfaces were immersed in stearic acid ethanol solution, a superhydrophobicity was obtained. As a result, the contact angles were larger than150°, and sliding angles were lower than10°. The size of irregular porous on surface was similar to the size of papilla on Lotus leaf surfaces. These holes were about between5to30μm in depth, and5to20μm in width. Surfaces were relative smooth and stable when it was prepared by acid etching, galvanic corrosion method, sulfuric acid anodizing method and phosphoric acid-dichromate method.
2. The wettability and stability of aluminum alloy superhydrophobic surfaces were studied. On the basis of Wenzel and Cassie models, the relationship between the roughness of the etched surface and superhydrophobicity was also investigated. The results indicated that the roughness on surface greatly enhanced the hydrophobicity of aluminum alloy surfaces. To analyze the relationship between wettability of the surface and coating process, the aluminum alloys were etched before its wettability transformed from hydrophilicity to superhydrophilicity. When they were coated with organic materials such as polypropylene (PP), polystyrene (PS) or maleic anhydride grafted polypropylene (PP-g-MAH), these surfaces were obtained superhydrophobicity. Among these materials, modified PP enhanced the hydrophobicity mostly. The wetting investigation showed that the superhydrophobicity could maintain in a wide pH range, and keep stable when it were immersed in organic solvent (concentration:<5%), and viarous influence factors such us relative humidity (30-70%), temperature range (10-40℃) and environment. In particular, PP film's surface could maintain a good hydrophobicity stability at100℃. Compared with the surfaces such as stearic acid (SA), polyethylene (PE), high-density polyethylene (HDPE), and PS film, and the SA film had long-term stability at room temperature. Obviously, PP film's surface had better superhydrophobicity and mechanical properties than others had.
3. The influence factors of the different acid etchant were studied in the preparation of superhydrophobic aluminum alloy surface, and the relationship between it and superhydrophobicity was also researched. The results showed that the different surface structures had the different wetting characteristics on the same chemical composition substances. Process were analyzed such as the concentration of acid solution and the immersion time, the best reaction conditions was expressed as follows:0.08mol/L oxalic acid and1mol/L hydrochloric acid solution at etching15hours and1%stearic acid ethanol solution at immersing30minutes. At the same time, the formation mechanism of this microstructure was analyzed.
4. The anodizing process by using sulfuric acid method and film-covered was studied. The water contact angle and sliding angle of superhydrophobic aluminum alloy surface were162°and2°, respectively. The composite structure surface was formed by coating with organic materials on micro-nano alloy substrates which were prepared by anodic oxidation method. Micro spheres and micropores presented these composite surfaces. Among of PP, PS, PP-g-MAH and the silane-PP films, the hydrophobic properties of the PP films pretreated by silane angent was the best one with a superior durability. Finally, the optimal process parmeter is:1.803mol/L sulfuric acid,0.068mol/L potassium dichromate,0.079mol/L oxalic acid,0.257mol/L sodium chloride and1.37mol/L glycerin; aluminum plate was designed as a anode and graphite was a cathode; current density was controlled as1.2A/dm2, and reaction time was30min.
5. Galvanic corrosion method was successfully used to prepare irregular porous structures on aluminum surfaces, sodium chloride solution was electrolyte solution and surfaces were coated stearic acid, the contact angle was154°. These holes were about between5to20μm in depth, and15to20μm in width, the size of the holes was similar to the size of the Lotus leaf surfaces'. The chloride ion played an important role in sodium chloride solution, the composition principle of surface porous structure. The relationship between the concentration of chloride ion in solution cell and superhydrophobicity were studied, the studies indicated that the size of the micron porous structure was a key factor which formed a superhydrophobic surface, and the accumulation of the nanoparticles could help to improve the hydrophobicity of the surfaces.
6. The properties of aluminum alloy superhydrophobic surfaces were studied, such as self-cleaning, anti-freezing, bacteriostasis and anti-corrosion. The research results showed that the superhydrophobic aluminum surface had good self-cleaning properties, and it can anti-freezing and anti-frosting under the freezing point. This phenomenon was analyzed with wettability theory and thermodynamics theory. The bacteriostasis properties of superhydrophobic aluminum surface were tested by quine method, sticking membrane method and shake flask test. The studies showed that the bacteriostasis properties of superhydrophobic aluminum samples was enhanced with the increase of the contact angle, the bacteriostasis rate was89.7%and91.2%when the contact angle was164°. The results indicated that superhydrophobic aluminum alloys had better anti-corrosion to salt than that of ordinary aluminums by polarization curve measurement and corrosion weight loss tests of different PH solutions. The studies were also showed that anti-corrosion of superhydrophobic aluminum alloys is well in weak acid and weak alkali environments, while it deteriorated in strong acid and strong alkali environments.
7. The binding force and the mechanism of durability of PP superhydrophobic aluminum alloy surface were studied. The studies showed that the binding force of aluminum alloy and PP (or PP-g-MAH coating) could be improved by silanization. A polysiloxane layer was formed in aluminum alloy surface with the Si-O-Al chemical bond. However, the superhydrophobic properties of the surface coating were decreased to some extent because the polarity of the coated film could be improved with PP-g-MAH. The superhydrophobic properties of the surface could be improved when PP was coated. The concentration of the PP solution has an important effect on the hydrophobicity. Furthermore, the addition of nanoparticles can not only improve the hydrophobicity of the coating structure, but also increase the stability of the structure.
引文
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