镀锌板钝化膜组成及性能的研究
摘要
钢板在镀锌后表面要进行钝化处理,但有时会出现钝化剂的性能不稳定、钝化效果不理想的现象,致使生产不能顺利进行。钝化膜的组成及结构决定它的性能,因此本文对镀锌板钝化膜的组成及耐蚀性进行了探讨。
本试验利用SEM和TEM方法观察了钝化剂原液的形貌,用SEM观察了镀锌板钝化后的形貌,钝化后锌板表面变得平整,缺陷减少;并用EDS检测了钝化膜的化学组成,膜中含有Zn,O,Cr,C;应用AES表面分析方法检测了各种元素随膜层厚度的变化情况,除Zn外的元素随膜厚度的增加,含量降低至零;采用XPS技术检测了钝化膜中含有Cr,O,C,Zn,P,N,F,Si等并测定了各元素的相对含量,它们主要以CrPO_4,Cr(OH)_3,CrOOH,Cr_2O_3,CrO_3,ZnO,Zn(OH)_2,Zn_3(PO_4)_2,H_2O,NH_3,有机分子以及硅溶胶的形式存在于钝化膜中。测试了两种钝化膜的附着力,S1优于T1;测试了镀锌板以及两种钝化膜的阳极极化曲线,S1膜的抗腐蚀性高于T1膜;盐雾试验结果表明,S1膜的耐蚀性更好。本文根据测试结果,大胆推测钝化过程可能发生的化学反应,并且认为钝化膜的生成支持成相膜理论。本试验通过检测与分析发现了NO_3~-用量上的差别影响钝化膜的耐蚀性。
Steel plate must have a passivating treatment after hot galvanizing, the manufacture was delayed by undesirable passivating results, which were caused by unreliable performance of passivator. The performance was determined by the composition and structure of the passive films, so the composition and properties of films were studied.Patterns of original passivator were observed by SEM and TEM, patterns of galvanizing sheet were observed by SEM, the surface of galvanizing sheet was smoothed with less defects. EDS analysis showed that Znic,Oxygen,Chromium,Carbon were contained in the surface films. AES analysis showed elements' distribution in depth, the content of all elements but zinc decreased while thickness of films increased. There were Cr,O,C,Zn,P,N,F,Si in films ,which were detected by XPS technique, they existed in films as CrPO_4,Cr(OH)_3,CrOOH,Cr_2O_3,CrO_3,ZnO,Zn(OH)_2,Zn3(PO_4)_2,H_2O,NH_3,organic molecule and silica sol. Adhesive power test showed S1 is better than T1. S1 showed good corrosion resistance during anodic polarization. NSS results showed S1 was best than others. According to all the results, chemical reactions which might happen in passivating treatment were inferred. It was deemed the films' formation supported phase-forming theory. It was found that corrosion resistance of passive films were influenced by the use level of
本试验利用SEM和TEM方法观察了钝化剂原液的形貌,用SEM观察了镀锌板钝化后的形貌,钝化后锌板表面变得平整,缺陷减少;并用EDS检测了钝化膜的化学组成,膜中含有Zn,O,Cr,C;应用AES表面分析方法检测了各种元素随膜层厚度的变化情况,除Zn外的元素随膜厚度的增加,含量降低至零;采用XPS技术检测了钝化膜中含有Cr,O,C,Zn,P,N,F,Si等并测定了各元素的相对含量,它们主要以CrPO_4,Cr(OH)_3,CrOOH,Cr_2O_3,CrO_3,ZnO,Zn(OH)_2,Zn_3(PO_4)_2,H_2O,NH_3,有机分子以及硅溶胶的形式存在于钝化膜中。测试了两种钝化膜的附着力,S1优于T1;测试了镀锌板以及两种钝化膜的阳极极化曲线,S1膜的抗腐蚀性高于T1膜;盐雾试验结果表明,S1膜的耐蚀性更好。本文根据测试结果,大胆推测钝化过程可能发生的化学反应,并且认为钝化膜的生成支持成相膜理论。本试验通过检测与分析发现了NO_3~-用量上的差别影响钝化膜的耐蚀性。
Steel plate must have a passivating treatment after hot galvanizing, the manufacture was delayed by undesirable passivating results, which were caused by unreliable performance of passivator. The performance was determined by the composition and structure of the passive films, so the composition and properties of films were studied.Patterns of original passivator were observed by SEM and TEM, patterns of galvanizing sheet were observed by SEM, the surface of galvanizing sheet was smoothed with less defects. EDS analysis showed that Znic,Oxygen,Chromium,Carbon were contained in the surface films. AES analysis showed elements' distribution in depth, the content of all elements but zinc decreased while thickness of films increased. There were Cr,O,C,Zn,P,N,F,Si in films ,which were detected by XPS technique, they existed in films as CrPO_4,Cr(OH)_3,CrOOH,Cr_2O_3,CrO_3,ZnO,Zn(OH)_2,Zn3(PO_4)_2,H_2O,NH_3,organic molecule and silica sol. Adhesive power test showed S1 is better than T1. S1 showed good corrosion resistance during anodic polarization. NSS results showed S1 was best than others. According to all the results, chemical reactions which might happen in passivating treatment were inferred. It was deemed the films' formation supported phase-forming theory. It was found that corrosion resistance of passive films were influenced by the use level of
引文
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[6] T Bellezze, G Roventi, R Fratesi. Electrochemical study on the corrosion resistance of Cr Ⅲ-based conversion layers on zinc coatings. Surface and coatings Technology, 2002, 155(2-3):221～222
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[8] A M Rocco, Tania M C, Renata A, et al. Evaluation of chromate passivation and chromate conversion coating on 55%Al-Zn coated steel. Surface and Coatings Technology, 2004, 179(23): 135～144
[9] I M Baghni, S B Lyon, Baofeng Ding. The effect of strontium and ions on the inhibition of zinc. Surface and Coatings Technology, 2004, 185(2-3): 194～198
[10] Kunitsugu Aramaki. Self-healing mechanism of an organosiloxane polymer film containing sodium silicate and cerium(Ⅲ) nitrate for corrosion of scratched zinc surface in 0.5M NaCl. Corrosion Science, 2002, 44(7): 1621～1632
[11] A B Velichenko, M Sarret, C Muller. Nature of the passive film formed at a zinc anode in zinc-nichel containing solutions. Journal of Electroanalytical Chemistry, 1998, 448(1): 1～3
[12] G Raichevsky, V Ivanova, St Vitkova, et al. Composition of passive chromate films on a Zn-Sn alloy. Surface and Coatings Technology, 1996, 82(3):239～246
[13] Hanxi Yang, Yuliang Cao, Xinping Ai, et al. Improved discharge capacity and suppressed surface passivation of zinc anode in diluter alkaline solution using surfactant additives. Power Sources, 2004, 128(1):97～101
[14] E Frackowiak, J M Skowronski. Passivation of zinc in alkaline solution effected by chromated and CrO_3-graphite system. Journal of Power Source, 1998, 73(2): 175～181
[15] J Peultier, E Rocca, J Steinmetz. Zinc carboxylating:a new conversion treatment of zinc. Corrosion Science, 2003, 45(8): 1703～1716
[16] L. J. Oblonsky, T. M. Devine. A study enhanced raman spectroscopic study of the passive films formed in borate buffer on iron, nickel, chromium and stainless steel. Corrosion Science, 1995, 37(1): 17～41
[17] Tim H Muster, Ivan S Cole. The protective nature of passivation films on zinc:surface charge. Corrosion Science, 2004, 46(9):2319～2335
[18] Mohammed A Amin. Passivity and passivity breakdown of a zinc electrode in aerated neutral sodium nitrate solutions. Electrochimica Acta, 2005, 50(6): 1265～1274
[19] Kh M S Youssef, C C Koch, P S Fedkiw. Improved corrosion behavior of nanocrystalline zinc produced by pulse-current electrodeposition. Corrosion Science, 2004, 46(1):51～46
[20] 屈定荣.Ti32Mo合金在盐酸溶液中钝化膜结构及性能研究[硕士学位论文].北京:北京化工大学,2002,3
[21] Z W Chen, N F Kennon, J B See, et al. Technigalva and Other Developments in Batch Hot-Dip Galvanizing. Journal of Materials Processing Technology, 1992, 44(1):22～26
[22] Wippermann K, Schultze J W, Kessel Retal. The Inhibition of Zinc Corrosion by Bisaminotriazole and Other Triazole Derivatives. Corrosion Science, 1991, 32(2):205
[23] 陈旭俊等.乙酸胺钼酸盐的缓蚀作用与机理.中国腐蚀与防护学报,1995,15(4):279～284
[24] Kurosawa K, Fukushima T. Effects of pH of a Na_2MoO_4-H_3PO_4 Type Aqueous Solution on the Formation of Chemical Conversion Coatings on Steels. Corrosion Science, 1989, 19(9): 1103～1107
[25] 方景礼,刘琴等.不锈钢上蓝色钼酸盐转化膜的研究.材料保护,1995,28(5):3～5
[26] 周金宝.镀锌层无铬钝化工艺的新进展.电镀与环保,1991,11(5):7
[27] 韩克平,叶向荣,方景礼.镀锌层表面硅酸盐防腐膜的研究.腐蚀科学与防护技术,1997,9(2):167
[28] 梁启民,张丽娜.镀锌层单宁酸钝化.电镀与精饰,1986,6(1):20
[29] 张安富.镀锌系钢板表面处理新工艺.表面技术,1991,20(5):29～33
[30] Motoaki Hara, Ryoichi Ichino, Masazumi Okido, et al. Corrosion protection property of colloidal silicate film on galvanized steel. Surface and Coatings Technology, 2003, 169-170:679～681
[31] Bijimi D, Gabe D R. Passivation Studies Using Group VIA Anions, Part 1:Aniodic Treatment of Tin. British Corrosion Journal, 1983, 18(2):88～91
[32] Bijimi D, Gabe D R. Passivation Studies Using Group VIA Anions, Part 2:Cathodic Treatment of Tin. British Corrosion Journal, 1983, 18(2):93～95
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