| 单分散掺硫碳微球的水热制备及其表征 | |
| Hydrothermal Synthesis and Characterization of Sulfur-Doped Carbon Microspheres | |
| 摘要: 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4 μm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。 | |
| 关键词: 碳微球 硫掺杂 水热碳化 表征 | |
| 基金项目: 国家自然科学基金(No.21201065,21031001,U0734005);广东省自然科学基金(No.s2012040007836);广东省高校科技创新计划(No.cxzd1014)和华南农业大学校长基金资助项目。 | |
| Abstract: Sulfur-doped carbon microspheres (SCMSs) with mean size of about 4 μm were prepared successfully by a simple one-step sulfur-assisted hydrothermal carbonization (ASHTC) method. Soluble starch was used as carbon precursor and sublime sulfur as sulfur source. The as-prepared SCMSs were characterized systematically by means of SEM, TEM, XRD, N2 absorption-desorption isotherms, FTIR, XPS, and solid NMR. The existing forms of sulfur in SCMSs were also discussed. It was found that monodispersed SCMSs with high output could be obtained under high starch concentration (1.0 g·mL-1) and sulfur atoms could be introduced into carbon networks easily, indicating that the ASHTC is a powerful method for SCMS synthesis. For comparison, carbon microspheres (CMSs) were synthesized by conventional hydrothermal carbonization of starch in the absence of sulfur under the same hydrothermal conditions. Experimental results show that the as-synthesized SCMSs exhibit much higher specific surface area than that of CMSs. The reason of the increase of surface area of SCMSs may be due to the structural and chemical defects resulted from the sulfur doping. The chemical defects come from the-S-S-,-S-,-SO2-and-SO-groups, while the structural defects result from the substitution of graphite hexatomic-rings by thiophene five-membered rings in SCMSs. | |
| Keywords: carbon microsphere sulfur doping hydrothermal carbonization characterization | |
| 投稿时间：2013-02-22 修订日期：2013-03-16 | |
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| 郑明涛,肖勇,张浩然,董汉武,龚学斌,徐汝淳,雷炳富,刘应亮,刘晓瑭.单分散掺硫碳微球的水热制备及其表征[J].无机化学学报,2013,29(7):1391-1399. | |
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