物理强化和稀土改性阳极氧化工艺及性能研究
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摘要
本文介绍了铝阳极氧化工艺、种类及应用，铝阳极氧化膜的结构、形成机理及研究进展，尤其介绍了当前国内外关于稀土添加剂对铝合金强化效果方面的研究情况，分析了各种工艺所存在的不足。论文通过对国内外文献的研究分析，确定采用稀土和超声波作用于铝阳极氧化的工艺方法作为强化的手段，以求在不需要苛刻的条件下获得高性能的氧化膜。
实验采用工业纯铝L3和硬铝LY12在含有稀土盐(结晶硫酸高铈Ce(SO_4)_2.4H_2O和稀土盐硫酸镧La_2(SO_4)_3.9H_2O)的硫酸电解液中进行阳极氧化，所得到氧化膜的性能和无稀土盐时所得到的进行比较，发现：前者性能要优于后者，硬度和厚度分别高出95HV和5.4μm左右(对工业纯铝L3)，硬铝LY12提高30HV和3.8μm左右；其稀土最佳含量为0.4～0.5g/L左右；在含复合稀土盐介质中所获得的试样其耐蚀性最好，而没有添加稀土时最差，单一稀土介于两者之间。
适当频率的超声波可以对阳极氧化膜的性能起到一定的作用，其频率应不超过20KHz。在添加稀土盐结晶硫酸高铈Ce(SO_4)_2.4H_2O(其浓度为0.5g/L)的电解液中，进行超声波作用(频率小于20KHz左右)可以改善氧化膜的性能，但是频率升高又会降低其性能。通过采用电子探针和能谱组合仪对膜成分进行测定，结果发现：氧化膜中没有发现稀土元素的存在，其只起类似于催化剂的作用。文章还用SEM分析了氧化膜结构的形貌。
The paper introduces the technologies, types and applications of aluminum anodizing, the structure of anodic aluminum oxide film, as well as forming mechanism and current studying situation; particularly, advances about effects of rare-earth additives on strengthening aluminum and its alloys, and analyzes the shortcomings of these technologies. After analyzing and studying literatures at home and abroad, rare-earth and ultrasonic are determined to be used in the process of anodic oxidation as a measure for strengthening aluminum so that high quality oxide films can be obtained under not harsh terms.
Pieces of industrial pure aluminum L3 and hard aluminum alloy LY12 with their size 2cm×2cm are anodized in H2SO4 electrolyte containing rare salts, at a result, it shows that the properties of their products are better than those of the one obtained in free rare salt H2SO4 electrolyte; And their optimum percents are 0.5% or so. In addition, composite rare earth salts are better than single salt for improving their properties.
Ultrasonic with proper frequency which is not more than 20KHz can serves to improve the properties of anodic oxide film. Less than 20 KHz ultrasonic which acts in the anodizing process of H2SO4 electrolyte containing rare salt Ce(SO4)2.4H2O(its concentration is 0.5g/L) can significantly improve the properties of anodic aluminum oxide film; but over high frequency may degrade the quality. There is not found any rare-earth elements in the oxide films with the use of XPS, which only acts as a catalyst.
实验采用工业纯铝L3和硬铝LY12在含有稀土盐(结晶硫酸高铈Ce(SO_4)_2.4H_2O和稀土盐硫酸镧La_2(SO_4)_3.9H_2O)的硫酸电解液中进行阳极氧化，所得到氧化膜的性能和无稀土盐时所得到的进行比较，发现：前者性能要优于后者，硬度和厚度分别高出95HV和5.4μm左右(对工业纯铝L3)，硬铝LY12提高30HV和3.8μm左右；其稀土最佳含量为0.4～0.5g/L左右；在含复合稀土盐介质中所获得的试样其耐蚀性最好，而没有添加稀土时最差，单一稀土介于两者之间。
适当频率的超声波可以对阳极氧化膜的性能起到一定的作用，其频率应不超过20KHz。在添加稀土盐结晶硫酸高铈Ce(SO_4)_2.4H_2O(其浓度为0.5g/L)的电解液中，进行超声波作用(频率小于20KHz左右)可以改善氧化膜的性能，但是频率升高又会降低其性能。通过采用电子探针和能谱组合仪对膜成分进行测定，结果发现：氧化膜中没有发现稀土元素的存在，其只起类似于催化剂的作用。文章还用SEM分析了氧化膜结构的形貌。
The paper introduces the technologies, types and applications of aluminum anodizing, the structure of anodic aluminum oxide film, as well as forming mechanism and current studying situation; particularly, advances about effects of rare-earth additives on strengthening aluminum and its alloys, and analyzes the shortcomings of these technologies. After analyzing and studying literatures at home and abroad, rare-earth and ultrasonic are determined to be used in the process of anodic oxidation as a measure for strengthening aluminum so that high quality oxide films can be obtained under not harsh terms.
Pieces of industrial pure aluminum L3 and hard aluminum alloy LY12 with their size 2cm×2cm are anodized in H2SO4 electrolyte containing rare salts, at a result, it shows that the properties of their products are better than those of the one obtained in free rare salt H2SO4 electrolyte; And their optimum percents are 0.5% or so. In addition, composite rare earth salts are better than single salt for improving their properties.
Ultrasonic with proper frequency which is not more than 20KHz can serves to improve the properties of anodic oxide film. Less than 20 KHz ultrasonic which acts in the anodizing process of H2SO4 electrolyte containing rare salt Ce(SO4)2.4H2O(its concentration is 0.5g/L) can significantly improve the properties of anodic aluminum oxide film; but over high frequency may degrade the quality. There is not found any rare-earth elements in the oxide films with the use of XPS, which only acts as a catalyst.
引文
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[2] J.A.Treveton, N.C.Daries. Metals Teches.. 1977(4):480
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[5] Vijh A K. Sparking voltages and side reactions during anodization of valve metals in terms of electron tunneling [J]. Corros. Sci.. 1971,11:411
[6] Ikonopisov S. Theory of electrical breakdown dung formation of barrier anodic films[J]. J. Electrochem Acta, 1977, 22: 1077
[7] Albella J M, Montern I., Mqrtine-Duart J M. Electron injection and avalanche during the anodic oxidation of tantalum[J]. J. Electrochem. Sci.. 1984,131:1101
[8] Krymann W, Kurze P, Dittrich K H. Process characteristics and parameters of anodic oxidation by spark discharge (ANOF)[J]. Crystal Research and Technology, 1984, 19: 973
[9] Kurze P, Krymann W. Structure and properties of ANOF layers and composites [J]. Schreckenbach. Ibid, 1986,21:1603
[10] Kurze P, Krymann W. Application fields of ANOF layers and composites [J]. Schreckenbach. Ibid, 1987,22:53
[11] 新野重夫．阳极酸化分离膜方法特性[A]．表面技术协会第89回讲演大会要旨集[C]．[s．l．]：[s．n．]，1994
[12] Quarto F D, Gentile C, Piazza s et al. Photo Electrochemical Study on Anodic Aluminum Oxide Film [J].J Electrochem Soc,1991,138(6)
[13] 孙伯勤．铝阳极氧化膜的多功能应用[J]．轻金属，1995，(6)：34-36
[14] 中村庆久．高密度磁气记录[J]．应用物理，1994，63(3)
[15] Arai K I, Shiyama K I. Megnetie Properties of Co-Fe Electrodeposited Aluminum Films[J].IEEE Tras Magn, 1991 (27)
[16] Preston C K, Moskovits M. Optical characterization of Anodic Aluminum Oxide Film Containing Electrochemically Deposited Metal Particles 1. Gold in Phosphoric Acid Anodic Aluminum Oxide Film[J].J Phys Chem,1993(97)
[17] Anderson A et al. Nickel Pigmented Anodic Aluminum Oxide for Selective Absorption of Solar Energy [J].J Appl Phys, 1980(51)
[18] 龟山秀雄．村田究．寺井聪．阳极酸化皮膜连续触媒体开发[J]．表面技术，1995，46(5)：32-35
[19] G.E.Thompson, G.C.Wood, R.Hutchings,Trans.IMF, 1980(58):21—25
[20] D.Eyre, D.R.Gabe. Trans. IMF,1979(57):38—42
[21] K. Yokoyama, H. Kommo et al. Plating and Surface Finishing [J]. 1982, 69(7):62
[22] 高桥，长野，近藤．实务表面技术[M]．1976(2)：60
[23] I.Mita, M.Yamada. Proc. Interfinish, 1985,80:254
[24] F.Keller, M.S.Hunter, J.Electrochm.Soc., 1953(100):411-419
[25] J.E.Murphy, C.E.Michelson. Int. Symp. Anod. Nottingham,1961
[26] Wood.GC et al. J.Electrochem.Soc, 1969,116(10): 1351
[27] G.E.Thompson,G.C.Wood etal, Trans.Inst.Met.Fin, 1978(56): 159
[28] Wade.K et al. Fournal of Materials Science, 1986,21(11):3810
[29] 黎樵焱等．表面技术[J]．1992，21(4)：159
[30] 徐洮等．电子显微学报[J]．1994，(4)：276
[31] Shimizu.K, et al. Thin Solid Films, 1982,88:256
[32] Hoar T. P, Yahalan. J.J. Electrochm. Soc., 1963, 110: 614
[33] Takahashi. H, Nagayama. N., Electrochem. Acta., 1978, 23(2):279
[34] 野口骏雄，吉村长藏．表面技术(日)，1994，45(3)：313
[35] Xu．Y，Thompson．G．C．，中国腐蚀与防护学报，1988，8(1)：1
[36] 高桥俊郎，齐藤让一等．表面技术(日)，1976．27：511
[37] Pringle.J.P.S.,J.Electrochem. Soc.. 1972,119:482
[38] Brown.F., Mackingtosh.W.D., J.Electrochem.Soc., 1973,120:1096
[39] 徐源，G．E．Thompson等．中国腐蚀与防护学报[J]．1987，7(3)：161-170
[40] 徐源，G．E．Thompson等．中国腐蚀与防护学报[J]．1988，8(4)：1-14
[41] Thompson.G.E.et al.Trans. Met. Finish. 1977,(5): 177
[42] Franklin. R.F. Nature, 1957,180:1470
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