类石墨氮化碳薄膜的电化学沉积

Electrodeposition of Graphite-like Carbon Nitride Thin Films

用 1:1.5的三聚氯氰和三聚氰胺的饱和乙腈溶液为沉积液 ,在Si(10 0 )衬底上室温常压下电化学沉积了CNx薄膜。用X射线光电子能谱 (XPS)、傅立叶转换红外光谱 (FTIR)、X射线衍射图谱 (XRD)对沉积的CNx 薄膜进行了测试和分析。XRD的衍射峰的结构数据与文献计算的类石墨相氮化碳的结构数据较为吻合。XPS结果表明沉积的薄膜中主要元素为C、N ,且N/C =0 .81,C1s和N1s的结合能谱中 2 87.84eV的碳和 4 0 0 .0 0eV的氮是样品中碳氮的主体 ,以C3 N3 杂环的形式存在。FTIR光谱中在 80 0cm-1、1310cm-1和 16 10cm-1的吸收峰也表明薄膜中存在C3 N3环 ,和XPS能谱的分析结果一致。Teter和Hemley预言的g C3 N4在结构形式上和三聚氰胺的完美脱胺缩聚物是一样的 ,红外光谱和X射线光电子能谱表明在样品中存在三嗪环 (C3 N3 ) ,支持XRD的实验结果。这说明CNx 薄膜中有类石墨相的C3 N4晶体存在。

The CN x thin film was deposited on Si(100)plate from a saturated acetonitrile solution of cyanuric trichloride and melamine( cyanuric trichloride/melamine=1:1.5) at room temperature.The film was characterized by X-ray photoelectron spectroscopy (XPS),Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD),respectively.XRD results showed that the d values,to which the diffraction peaks in the pattern correspond,are in good agreement with the structure data of graphite-like carbon nitride calculated in the literature.XPS measurements suggested the elements in the deposited films mostly consist of C and N(N/C=0.81),N(400.00eV) bonded with C( 287.84eV) in the form of six-member C 3N 3 ring.Peaks corresponding to 800cm -1,1310cm -1 and 1610cm -1 in the FTIR spectrum indicated triazine ring (six-member C 3N 3 ring) exists in the product.XPS and FTIR spectrum support the indexing result of XRD pattern because the melamine-based carbon nitride introduced by Teter and Hemley is formally depicted as a perfect deammonation polycondensate of melamine.The results demonstrated that crystalline g-C 3N 4 exists in the CN x film.