光谱学研究硅烷钒锆复合钝化膜的结构和成膜机理

发布时间：2019-04-24 06:48

【摘要】：在热镀锌钢板表面制备了硅烷钒锆复合钝化膜。用X射线光电子能谱(XPS)、射频辉光放电发射光谱(rf-GD-OES)和傅里叶变换衰减全反射红外光谱(ATR-FTIR)表征了钝化膜的组成结构,分析了硅烷钒锆复合钝化膜的成膜机理。结果表明:硅烷之间互联构成了硅烷钒锆复合钝化膜的主成膜成分,无机缓蚀剂均匀分布在膜层中。钝化膜表面Si2p的XPS窄幅扫描谱100.7eV处的拟合峰和红外光谱在波数1 100cm-1 Si—O吸收峰变宽加强,表明硅烷以Si—O—Zn键的形式化学吸附在锌的表面,硅烷分子之间通过Si—O—Si键相互交联;红外光谱中1 650和1 560cm-1的两个酰胺特征峰,结合910cm-1的环氧特征峰的消失,表明γ-GPT的环氧基团在氨基活性氢的诱导下开环和γ-APT的氨基之间发生聚合反应形成交联的空间网状结构;rf-GD-OES分析发现钝化膜0.3μm处存在一层富氧层,钝化反应生成的ZrF4,ZrO2和钒盐等无机物均匀分布在钝化膜中。分析膜层组成结构和成膜前后的ATR-FTIR光谱,研究了成膜过程中发生的物理过程和化学变化,提出了硅烷钒锆复合钝化膜的成膜机理。
[Abstract]:Silane-vanadium-zirconium composite passivation film was prepared on the surface of hot-dip galvanized steel plate. The composition and structure of the passive films were characterized by X-ray photoelectron spectroscopy (XPS),) RF glow discharge emission spectroscopy (rf-GD-OES) and Fourier transform attenuated total reflection infrared spectroscopy (ATR-FTIR). The formation mechanism of silane-vanadium-zirconium composite passivation film was analyzed. The results show that the main composition of silane vanadium zirconium composite passivation film is formed by the interconnection of silane and zirconium, and the inorganic corrosion inhibitor is uniformly distributed in the film. The fitting peak at the narrow XPS scanning spectrum of Si2p on the surface of the passive film and the infrared spectrum at the wavelength number of 1 100cm-1 Si-O broadened, indicating that silane was chemisorbed on the surface of zinc in the form of Si-O-Zn bond. Silane molecules are cross-linked by Si-O-Si bonds. The two characteristic peaks of amide of 1 650 and 1 560cm-1 in IR spectra, and the disappearance of epoxy characteristic peaks of 910cm-1. The results show that the ring opening of 纬-GPT and the polymerization of amino groups of 纬-APT take place under the inducement of amino active hydrogen to form a cross-linked spatial reticular structure. Rf-GD-OES analysis showed that there was an oxygen-rich layer at 0.3 渭 m in the passivation film, and the inorganic substances such as ZrF4,ZrO2 and vanadium salt were uniformly distributed in the passivation film. The composition and structure of the film and the ATR-FTIR spectra before and after the film formation were analyzed. The physical and chemical changes of the film formation process were studied. The film forming mechanism of the silane vanadium zirconium composite passivation film was put forward.
【作者单位】：沈阳理工大学环境与化学工程学院;东北大学材料各向异性与织构工程教育部重点实验室;
【基金】：国家高技术发展计划(863)项目(2009AA03Z529)资助
【分类号】：TG174.4

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