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以可溶性淀粉为碳源,采用硫辅助水热碳化法一步制备了平均粒径约为4μm的单分散掺硫碳微球。利用扫描电镜、透射电镜、X射线衍射、氮气吸脱附、傅里叶变换红外光谱、X射线光电子能谱、固体核磁共振等手段对掺硫碳微球的结构和性质进行了表征。硫辅助水热碳化法可以在高浓度条件下高产量地制备分散性良好的掺硫碳微球,更重要的是硫原子可以同步进入碳的网络结构中。与传统水热碳化法相比,采用硫辅助水热碳化法制备的掺硫碳微球具有更高的比表面积,其可能的原因是硫原子的引入产生了大量的化学与结构缺陷:-S-S-、-S-、-SO2-和-SO-等基团构成化学缺陷,而噻吩等五元环取代石墨六元环形成结构缺陷。
Using soluble starch as carbon source, monodispersed carbon-doped carbon microspheres with an average diameter of about 4μm were prepared in one step by sulfur-assisted hydrothermal carbonization. The structure and properties of carbon-doped carbon microspheres were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, nitrogen adsorption and desorption, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and solid state nuclear magnetic resonance. The sulfur-assisted hydrothermal carbonization method can prepare good dispersible sulfur-doped carbon microspheres with high yield under the condition of high concentration, and more importantly, the sulfur atoms can be simultaneously introduced into the carbon network structure. Compared with the traditional hydrothermal carbonization method, the sulfur-doped carbon microspheres prepared by sulfur-assisted hydrothermal carbonization have higher specific surface area. The possible reason is that the introduction of sulfur atoms has a lot of chemical and structural defects: -S- , -S-, -SO2- and -SO- groups constitute a chemical defect, while the five-membered rings such as thiophene replace the graphite six-membered rings to form structural defects.