不锈钢表面微、纳米薄膜的制备及光催化和抗菌性能研究
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摘要
不锈钢具有良好的耐蚀性、耐热性，以及优异的机械强度和延展性，并且表面光亮，已广泛用于建筑材料、卫浴洁具、厨房用品、家用电器和医疗器械等领域。在室外使用环境中，不锈钢制品的表面容易受到灰尘、油污的沾染；在室内等环境中使用，还常常会粘附水渍，从而滋生细菌，威胁人们的健康，在公众场所还将造成交叉传染。不锈钢制品在使用过程中需要进行定期清洗，尤其是在幕墙、屋顶及野外等场合使用的不锈钢制品，清洗难度大、人工耗费高，因此制备光催化和抗菌功能的不锈钢具有广阔的应用前景。本文采用电化学阳极化在不锈钢表面原位形成Fe_2O_3纳米孔阵列，首次研究了这种在不锈钢表面原位生成纳米孔结构的光催化性能，通过高能离子注入、化学水热等手段，在不锈钢表面形成TiO_2、WO_3半导体光催化剂掺杂的纳米复合结构，使不锈钢在光照条件下具有自清洁功能和良好的抑菌杀菌能力，同时保持不锈钢表面的硬度、机械强度、光洁度和耐蚀性能等性质基本不变。这种具有光催化性能的不锈钢可大量节省不锈钢制品的清洗、保洁费用，将产生良好的社会和经济效益。主要研究工作如下：
1）通过阳极氧化法在不锈钢表面原位生成纳米孔结构。系统研究了阳极氧化条件对不锈钢表面纳米孔结构的影响。分别在高氯酸乙二醇溶液、NH_4F溶液、NH_4Cl溶液、硫酸根溶液和磷酸二氢钠溶液中，以抛光的不锈钢片为阳极，在合适电压、温度和时间范围内进行阳极氧化。结果表明，在所选溶液体系下，均能在不锈钢表面获得纳米孔阵列结构，纳米孔主要由Fe_2O_3和Cr_2O_3组成，直径在30～300nm之间，深度范围为10～130nm，纳米孔的形貌和结构可以根据阳极氧化实验条件进行调控。本文制备的不锈钢表面纳米孔阵列，将进一步拓宽不锈钢的应用领域，为实现不锈钢功能化的研究奠定基础。
2）通过对高氯酸乙二醇溶液的浓度、电压和时间的控制，制备了具有规则均匀纳米孔结构表面的不锈钢。当温度为5℃、阳极氧化电压40V、高氯酸溶液浓度为5vol%、阳极氧化时间10分钟时，所制备的纳米孔直径约100nm，深度为26nm，纳米孔阵列主要由为Fe_2O_3和Cr_2O_3组成，此时不锈钢表面薄膜表现出最大的光催化活性。在高氯酸乙二醇溶液中阳极氧化制备的不锈钢纳米孔结构不会改变不锈钢光洁美观的表面，同时保持了不锈钢良好的耐蚀性能。
3）在不锈钢表面通过阳极氧化制备纳米孔阵列，通过离子注入对不锈钢纳米孔结构进行掺杂，经退火在不锈钢表面形成Fe_2O_3/TiO_2复合薄膜，以提升光催化性能。结果表明，加速电压为50kV下注入3×10~(15)atoms/cm~2剂量的钛离子，然后450℃退火2小时，所得Fe_2O_3/TiO_2复合薄膜比阳极氧化形成的纳米孔阵列的光催化性能提高4.6倍，并且耐蚀性能比不锈钢本体有所提高。
4）在不锈钢表面通过阳极氧化制备纳米孔阵列，利用化学水热法负载TiO_2/WO_3，以提升光催化性能。结果表明，以0.010mol/L (NH_4)_2TiF_6和0.0066mol/L Na_2WO_4混合溶液为前驱体，120℃水热3小时所制备的复合薄膜光催化性能，比阳极氧化形成的纳米孔阵列的光催化性能提高15.7倍。这种复合薄膜的光催化性能，比同样条件下单独负载TiO_2和WO_3分别提高了5倍和8倍，其良好的光催化性能应归功于TiO_2/WO_3异质结的形成，延迟了光生电子与空穴的复合，从而使光催化活性显著提高。
5）在不锈钢表面通过阳极氧化制备纳米孔阵列，利用化学水热法负载SnO_2，以提升光催化性能。结果表明，以0.030mol/L SnCl_4溶液为前驱体，220℃水热3小时所制备复合薄膜光催化性能，比阳极氧化形成的纳米孔阵列的光催化性能提高11.8倍。SnO_2是n型半导体，在阳极氧化的不锈钢表面形成Fe_2O_3/SnO_2异质结，从而使光催化性能明显提高。并且负载SnO_2的薄膜具有良好导电性能，表现出显著的光电流响应，在相同条件下，其光电流比阳极氧化的纳米孔阵列提高了14.8倍。
6）为弥补单一金属抗菌离子在抗菌广谱性方面的不足，开展了双元抗菌元素的不锈钢研制，以降低贵金属银的用量，改善不锈钢的耐蚀性能和使用安全性。首次采用利用双层辉光离子渗金属技术制备了含Ag/Cu、Cu/Zn的抗菌不锈钢，所得渗层在不锈钢表面分布均匀，耐腐蚀性能有所提高。抗菌不锈钢抗菌广谱性好，杀菌效率高，对革兰氏阴性菌大肠杆菌和革兰氏阳性菌金黄色葡萄球菌的杀菌率都达到100%。
Stainless steels are essential base materials with a host of commercial applications, such asbuilding materials, sanitary wares, kitchenwares, household appliances and medical apparatusdue to its advantages of resistance to corrosion and heating, good mechanical properties andductibility, and high polish surface. However, composite organic, inorganic and biologicalfouling occurs on stainless steel surface. The surface fouling will lower the corrosion resistanceand smear the high polish surface of stainless steels. Traditional heavy manual cleaning worksfor curtain walls and roof glazing systems are accompanied by great risk and high cost tocleaners and architectures. Protection of stainless steels from corrosion and keeping the surfaceclean are an area of study commanding considerable attention. Photocatalytic processes arewidely recognized as viable stategies to solve the surface fouling problems, because organicspecies can be completely mineralized to carbon dioxide or become nontoxic materials byphotocatalytic pathways. For the first time, several strategies were proposed to developphotocleanable and antibacterial stainless steels. Micro-and nanocomposites films composed ofFe_2O_3, TiO_2and WO_3were prepared on stainless steels by electrochemical anodization, ionimplantation and hydrothermal reactions. The as-prepared composite films on stainless steelswith favourable photocatalytic properties and excellent antibacterial performance demonstratecomparable hardness, mechanical properties, high polish surface and corrosion resistance tothose of original surface of stainless steels. The composite films on stainless steels withremarkable photocatalytic activities will exhibit potential applications particularly for outdoorpurpose and will considerably reduce the cleaning cost. Great social and economic benefits willbe expected. The main research works are as follows:
1) Nanopores arrays (NPAs) on stainless steels surface are prepared by electrochemicalanodization. The morphology, microsture and chemical composition of the NPAs areinvestigated. The anodization process was carried out with a polished stainless steel foil servedas the anode in several solutions, such as perchloric acid, NH_4F, NH_4Cl, SO42-and NaH2PO4.Uniform NPAs composed of Fe_2O_3and Cr_2O_3were prepared in these solutions, with diametersin the range of30~300nm, and depths in the range of10~130nm. The morphology andmicrosture of the NPAs can be controlled by anodization process. The controllable formation ofNPAs will expand the applications of stainless steels and provide a set of systematic methodsfor functionalization of stainless steels.
2) Formation of NPAs on the surface of stainless steel is demonstrated by anodization inethylene glycol (EG) solution containing perchloric acid. Perchloric acid concentration, appliedvoltage and anodization time of anodization process are investigated. The maximum depth of anodic overlayer is26nm composited by Fe_2O_3and Cr_2O_3after anodization in5vol%HClO4EG solution at40V for10min. The anodized stainless steel shows significant photocatalyticactivities, which should be attributed to the photocatalytic performance of Fe_2O_3and theFe_2O_3-Cr_2O_3heterojunction. Moreover, the formation of NPAs does not damage the polishappearance of stainless steels and remains good corrosion resistance.
3) Anodized stainless steel was implanted by Ti ions at an extracting voltage of50KVwith an implantation dose of3×10~(15)atoms/cm~2. The implanted stainless steel was then annealedin air at450℃for2h. The results showed that the Fe_2O_3-TiO_2composite film exhibited anenhanced photocatalytic activity that is4.6times to that of as-anodized stainless steel.Meanwhile, the implanted stainless steel showed a slightly better resistance to corrosion thanthat of mechanically polished stainless steel.
4) A one-step hydrothermal reaction was presented to prepare TiO_2/WO_3nanocompositefilms deposited on anodized stainless steel. The TiO_2/WO_3nanocomposite film prepared in0.01mol/L (NH_4)_2TiF_6and0.0066mol/L Na_2WO_4solution at120℃for3h exhibits the maximumphotocatalytic activity that is15.7times to that of as-anodized stainless steel. Thephotocatalytic activity of TiO_2/WO_3nanocomposite film is five times higher than that of pureTiO_2film and eight times higher than that of pure WO_3film. The excellent photocatalyticactivity of the nanocomposite film should be attributed to the formation of heterojunctionbetween TiO_2and WO_3nanoparticles that can facilitate the separation of photo-generatedelectron-hole pairs.
5) Hydrothermal reaction was presented to prepare Fe_2O_3/SnO_2nanocomposite filmdeposited on anodized stainless steels. The Fe_2O_3/SnO_2nanocomposite film prepared in0.030mol/L SnCl_4solution at220℃for3h exhibits the maximum photocatalytic activity that is11.8times to that of as-anodized stainless steel. SnO_2is an n-type semiconductor. The excellentphotocatalytic activity of the nanocomposite film should be attributed to the formation ofheterojunction between Fe_2O_3and SnO_2nanocrystals that can facilitate the separation ofphoto-generated electron-hole pairs. Moreover, the conductive nanocomposite film showsconsiderable photocurrent that is14.8times higher than that of as-anodized stainless steel.
6) Antibacterial activities of medical materials contained with only one antibacterial agentwill be compromised in many situations. Antibacterial stainless steel containing twoantibacterial agents will offset these deficiencies and will obtain high antibacterial efficiencytowards most microorganisms. Antibacterial stainless steels containing Ag/Cu or Cu/Zn wereprepared glow discharge plasma metallurgy. The corrosion resistance of stainless steel isslightly enhanced after glow discharge plasma treatment. Excellent antibacterial activities(100%) against both Gram-negative Escherichia coli and Gram-positive Staphylococcus aureusare obtained for Ag/Cu or Cu/Zn doped stainless steel.
1）通过阳极氧化法在不锈钢表面原位生成纳米孔结构。系统研究了阳极氧化条件对不锈钢表面纳米孔结构的影响。分别在高氯酸乙二醇溶液、NH_4F溶液、NH_4Cl溶液、硫酸根溶液和磷酸二氢钠溶液中，以抛光的不锈钢片为阳极，在合适电压、温度和时间范围内进行阳极氧化。结果表明，在所选溶液体系下，均能在不锈钢表面获得纳米孔阵列结构，纳米孔主要由Fe_2O_3和Cr_2O_3组成，直径在30～300nm之间，深度范围为10～130nm，纳米孔的形貌和结构可以根据阳极氧化实验条件进行调控。本文制备的不锈钢表面纳米孔阵列，将进一步拓宽不锈钢的应用领域，为实现不锈钢功能化的研究奠定基础。
2）通过对高氯酸乙二醇溶液的浓度、电压和时间的控制，制备了具有规则均匀纳米孔结构表面的不锈钢。当温度为5℃、阳极氧化电压40V、高氯酸溶液浓度为5vol%、阳极氧化时间10分钟时，所制备的纳米孔直径约100nm，深度为26nm，纳米孔阵列主要由为Fe_2O_3和Cr_2O_3组成，此时不锈钢表面薄膜表现出最大的光催化活性。在高氯酸乙二醇溶液中阳极氧化制备的不锈钢纳米孔结构不会改变不锈钢光洁美观的表面，同时保持了不锈钢良好的耐蚀性能。
3）在不锈钢表面通过阳极氧化制备纳米孔阵列，通过离子注入对不锈钢纳米孔结构进行掺杂，经退火在不锈钢表面形成Fe_2O_3/TiO_2复合薄膜，以提升光催化性能。结果表明，加速电压为50kV下注入3×10~(15)atoms/cm~2剂量的钛离子，然后450℃退火2小时，所得Fe_2O_3/TiO_2复合薄膜比阳极氧化形成的纳米孔阵列的光催化性能提高4.6倍，并且耐蚀性能比不锈钢本体有所提高。
4）在不锈钢表面通过阳极氧化制备纳米孔阵列，利用化学水热法负载TiO_2/WO_3，以提升光催化性能。结果表明，以0.010mol/L (NH_4)_2TiF_6和0.0066mol/L Na_2WO_4混合溶液为前驱体，120℃水热3小时所制备的复合薄膜光催化性能，比阳极氧化形成的纳米孔阵列的光催化性能提高15.7倍。这种复合薄膜的光催化性能，比同样条件下单独负载TiO_2和WO_3分别提高了5倍和8倍，其良好的光催化性能应归功于TiO_2/WO_3异质结的形成，延迟了光生电子与空穴的复合，从而使光催化活性显著提高。
5）在不锈钢表面通过阳极氧化制备纳米孔阵列，利用化学水热法负载SnO_2，以提升光催化性能。结果表明，以0.030mol/L SnCl_4溶液为前驱体，220℃水热3小时所制备复合薄膜光催化性能，比阳极氧化形成的纳米孔阵列的光催化性能提高11.8倍。SnO_2是n型半导体，在阳极氧化的不锈钢表面形成Fe_2O_3/SnO_2异质结，从而使光催化性能明显提高。并且负载SnO_2的薄膜具有良好导电性能，表现出显著的光电流响应，在相同条件下，其光电流比阳极氧化的纳米孔阵列提高了14.8倍。
6）为弥补单一金属抗菌离子在抗菌广谱性方面的不足，开展了双元抗菌元素的不锈钢研制，以降低贵金属银的用量，改善不锈钢的耐蚀性能和使用安全性。首次采用利用双层辉光离子渗金属技术制备了含Ag/Cu、Cu/Zn的抗菌不锈钢，所得渗层在不锈钢表面分布均匀，耐腐蚀性能有所提高。抗菌不锈钢抗菌广谱性好，杀菌效率高，对革兰氏阴性菌大肠杆菌和革兰氏阳性菌金黄色葡萄球菌的杀菌率都达到100%。
Stainless steels are essential base materials with a host of commercial applications, such asbuilding materials, sanitary wares, kitchenwares, household appliances and medical apparatusdue to its advantages of resistance to corrosion and heating, good mechanical properties andductibility, and high polish surface. However, composite organic, inorganic and biologicalfouling occurs on stainless steel surface. The surface fouling will lower the corrosion resistanceand smear the high polish surface of stainless steels. Traditional heavy manual cleaning worksfor curtain walls and roof glazing systems are accompanied by great risk and high cost tocleaners and architectures. Protection of stainless steels from corrosion and keeping the surfaceclean are an area of study commanding considerable attention. Photocatalytic processes arewidely recognized as viable stategies to solve the surface fouling problems, because organicspecies can be completely mineralized to carbon dioxide or become nontoxic materials byphotocatalytic pathways. For the first time, several strategies were proposed to developphotocleanable and antibacterial stainless steels. Micro-and nanocomposites films composed ofFe_2O_3, TiO_2and WO_3were prepared on stainless steels by electrochemical anodization, ionimplantation and hydrothermal reactions. The as-prepared composite films on stainless steelswith favourable photocatalytic properties and excellent antibacterial performance demonstratecomparable hardness, mechanical properties, high polish surface and corrosion resistance tothose of original surface of stainless steels. The composite films on stainless steels withremarkable photocatalytic activities will exhibit potential applications particularly for outdoorpurpose and will considerably reduce the cleaning cost. Great social and economic benefits willbe expected. The main research works are as follows:
1) Nanopores arrays (NPAs) on stainless steels surface are prepared by electrochemicalanodization. The morphology, microsture and chemical composition of the NPAs areinvestigated. The anodization process was carried out with a polished stainless steel foil servedas the anode in several solutions, such as perchloric acid, NH_4F, NH_4Cl, SO42-and NaH2PO4.Uniform NPAs composed of Fe_2O_3and Cr_2O_3were prepared in these solutions, with diametersin the range of30~300nm, and depths in the range of10~130nm. The morphology andmicrosture of the NPAs can be controlled by anodization process. The controllable formation ofNPAs will expand the applications of stainless steels and provide a set of systematic methodsfor functionalization of stainless steels.
2) Formation of NPAs on the surface of stainless steel is demonstrated by anodization inethylene glycol (EG) solution containing perchloric acid. Perchloric acid concentration, appliedvoltage and anodization time of anodization process are investigated. The maximum depth of anodic overlayer is26nm composited by Fe_2O_3and Cr_2O_3after anodization in5vol%HClO4EG solution at40V for10min. The anodized stainless steel shows significant photocatalyticactivities, which should be attributed to the photocatalytic performance of Fe_2O_3and theFe_2O_3-Cr_2O_3heterojunction. Moreover, the formation of NPAs does not damage the polishappearance of stainless steels and remains good corrosion resistance.
3) Anodized stainless steel was implanted by Ti ions at an extracting voltage of50KVwith an implantation dose of3×10~(15)atoms/cm~2. The implanted stainless steel was then annealedin air at450℃for2h. The results showed that the Fe_2O_3-TiO_2composite film exhibited anenhanced photocatalytic activity that is4.6times to that of as-anodized stainless steel.Meanwhile, the implanted stainless steel showed a slightly better resistance to corrosion thanthat of mechanically polished stainless steel.
4) A one-step hydrothermal reaction was presented to prepare TiO_2/WO_3nanocompositefilms deposited on anodized stainless steel. The TiO_2/WO_3nanocomposite film prepared in0.01mol/L (NH_4)_2TiF_6and0.0066mol/L Na_2WO_4solution at120℃for3h exhibits the maximumphotocatalytic activity that is15.7times to that of as-anodized stainless steel. Thephotocatalytic activity of TiO_2/WO_3nanocomposite film is five times higher than that of pureTiO_2film and eight times higher than that of pure WO_3film. The excellent photocatalyticactivity of the nanocomposite film should be attributed to the formation of heterojunctionbetween TiO_2and WO_3nanoparticles that can facilitate the separation of photo-generatedelectron-hole pairs.
5) Hydrothermal reaction was presented to prepare Fe_2O_3/SnO_2nanocomposite filmdeposited on anodized stainless steels. The Fe_2O_3/SnO_2nanocomposite film prepared in0.030mol/L SnCl_4solution at220℃for3h exhibits the maximum photocatalytic activity that is11.8times to that of as-anodized stainless steel. SnO_2is an n-type semiconductor. The excellentphotocatalytic activity of the nanocomposite film should be attributed to the formation ofheterojunction between Fe_2O_3and SnO_2nanocrystals that can facilitate the separation ofphoto-generated electron-hole pairs. Moreover, the conductive nanocomposite film showsconsiderable photocurrent that is14.8times higher than that of as-anodized stainless steel.
6) Antibacterial activities of medical materials contained with only one antibacterial agentwill be compromised in many situations. Antibacterial stainless steel containing twoantibacterial agents will offset these deficiencies and will obtain high antibacterial efficiencytowards most microorganisms. Antibacterial stainless steels containing Ag/Cu or Cu/Zn wereprepared glow discharge plasma metallurgy. The corrosion resistance of stainless steel isslightly enhanced after glow discharge plasma treatment. Excellent antibacterial activities(100%) against both Gram-negative Escherichia coli and Gram-positive Staphylococcus aureusare obtained for Ag/Cu or Cu/Zn doped stainless steel.
引文
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