Citation: ZHENG Ming-Tao, XIAO Yong, ZHANG Hao-Ran, DONG Han-Wu, GONG Xue-Bin, XU Ru-Chun, LEI Bing-Fu, LIU Ying-Liang, LIU Xiao-Tang. Hydrothermal Synthesis and Characterization of Sulfur-Doped Carbon Microspheres[J]. Chinese Journal of Inorganic Chemistry, ;2013, 29(7): 1391-1399. doi: 10.3969/j.issn.1001-4861.2013.00.244 shu

Hydrothermal Synthesis and Characterization of Sulfur-Doped Carbon Microspheres

1.
Department of Applied Chemistry, College of Science, South China Agricultural University, Guangzhou 510642, China

Received Date: 22 February 2013
Available Online: 16 March 2013
Fund Project: 国家自然科学基金(No.21201065,21031001,U0734005) (No.21201065,21031001,U0734005)广东省自然科学基金(No.s2012040007836) (No.s2012040007836)广东省高校科技创新计划(No.cxzd1014) (No.cxzd1014)

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.
- carbon microsphere;sulfur doping;hydrothermal carbonization;characterization
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沈阳化工大学材料科学与工程学院沈阳 110142