CAJ | 학술논문

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100．7 eV 处的拟合峰和红外光谱在波数1100 cm－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1650和1560 cm－1的两个酰胺特征峰，结合910 cm－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。
재열도자강판표면제비료규완범고복합둔화막。용 X 사선광전자능보（XPS）、사빈휘광방전발사광보（rf-GD-OES）화부리협변환쇠감전반사홍외광보（ATR-FTIR）표정료둔화막적조성결구，분석료규완범고복합둔화막적성막궤리。결과표명：규완지간호련구성료규완범고복합둔화막적주성막성분，무궤완식제균균분포재막층중。둔화막표면 Si2p 적 XPS 착폭소묘보100．7 eV 처적의합봉화홍외광보재파수1100 cm－1 Si—O흡수봉변관가강，표명규완이 Si—O—Zn 건적형식화학흡부재자적표면，규완분자지간통과Si—O—Si건상호교련；홍외광보중1650화1560 cm－1적량개선알특정봉，결합910 cm－1적배양특정봉적소실，표명γ-GPT적배양기단재안기활성경적유도하개배화γ-APT적안기지간발생취합반응형성교련적공간망상결구；rf-GD-OES분석발현둔화막0．3μm처존재일층부양층，둔화반응생성적ZrF4，ZrO2화범염등무궤물균균분포재둔화막중。분석막층조성결구화성막전후적ATR-FTIR광보，연구료성막과정중발생적물리과정화화학변화，제출료규완범고복합둔화막적성막궤리。
A composite silanes-V-Zr passive film was overlayed on hot-dip galvanized steel.Attenuated total reflection Fourier transformed infrared spectroscopy (ATR-FTIR),X-ray photoelectron spectrometer (XPS)and radio frequency glow discharge optical emission spectrometry (rf-GD-OES)were used to characterize the molecular structure of the silanes-V-Zr passive film. The mechanism of film formation was discussed.The results show that the silane molecules are crosslinked as the main film for-mer and inorganic inhibitor is even distributed in the film.The fitting peak of 100. 7 eV in XPS single Si2p energy range spectra of the composite silanes-V-Zr passive film and the widening and strengthening of the Si—O infrared absorption peak at 1 100 cm-1 indicate that the silanes were adsorbed on the surface of zinc with chemical bond of Si—O—Zn,and the silane molecules were connected with each other by bond of Si—O—Si.Two characteristic absorption peaks of amide at 1 650 and 1 560 cm-1 ap-pear in the infrared spectroscopy of the composite silanes-V-Zr passive film,and a characteristic absorption peak of epoxy groups at 910 cm-1 disappears in the infrared spectroscopy of the passive film.The results indicate thatγ-APT can be prepared through nucleophilic ring-opening of ethylene oxide inγ-GPT molecule to form C—N covalent bonds.The rf-GD-OES results indicate that there is a oxygen enriched layer in 0. 3 μm depth of the composite silanes-V-Zr passive film.Moreover,ZrF4 ,ZrO2 and some inorganic matter obtained by the reaction during the forming process of the composite silanes-V-Zr passive film are distribu-ted evenly throughout the film.According to the film composition,the physical processes and chemical reactions during the film forming process were studied by using ATR-FTIR.Based on this,the film forming mechanism was proposed.