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
1. [1]
  [1] CHENG Li-Qiang(程立强), LIU Ying-Liang(刘应亮), ZHANG Jing-Xian(张静娴), et al. Prog. Chem.(Huaxue Jinzhan), 2006,18(10):1298-1304
2. [2]
  [2] Xu C W, Cheng L Q, Shen P K, et al. Electrochem. Commun., 2007,9:997-1001
3. [3]
  [3] WANG Xiu-Li(王秀丽), LIN Hong-Yan(林宏艳), LU Hai-Yan(卢海燕), et al. Chin. J. Appl. Chem.(Yingyong Huaxue), 2006,23(11):1223-1227
4. [4]
  [4] PING Li-Na(平丽娜), ZHENG Jia-Ming(郑嘉明), SHI Zhi-Qiang(时志强), et al. Acta Phys.-Chim. Sin.(Wuli Huaxue Xuebao), 2012,28(7):1733-1738
5. [5]
  [5] Pan L L, Bi J Q, Bai Y J, et al. J. Phys. Chem. C, 2008,112: 12134-12137
6. [6]
  [6] Deshmukh A A, Mhlanga S D, Coville N J. Mater. Sci. Eng. R, 2010,70:1-28
7. [7]
  [7] WU Yong-Jian(武拥建), ZHENG Ming-Tao(郑明涛), XIE Chun-Lin(谢春林), et al. Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 2011,27(12):2447-2452
8. [8]
  [8] CHEN Feng(陈丰), CHEN Zhi-Gang(陈志刚), LI Xia-Zhang (李霞章), et al. J. Chin. Ceram. Soc.(Guisuanyan Xuebao), 2011,39(3):397-402
9. [9]
  [9] CI Ying(慈颖), GE Jun(葛军), Wang Xiao-Feng(王小峰), et al. Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 2007, 23(2):365-368
10. [10]
  [10] Cui J, Hu C, Yang, et al. J. Mater. Chem., 2012,22:8121-8126
11. [11]
  [11] Serp P, Feurer R, Kalck P, et al. Carbon, 2001,39:621-626
12. [12]
  [12] Zhao S, Wang C Y, Chen M M, et al. Mater. Lett., 2008,62: 3322-3324
13. [13]
  [13] Wang Z L, Kang Z C. J. Phys. Chem., 1996,100:17725-17731
14. [14]
  [14] Lou Z S, Chen Q W, Gao J, et al. Carbon, 2004,42:229-232
15. [15]
  [15] Wang Q, Li H, Chen L Q, et al. Carbon, 2001,39:2211-2214
16. [16]
  [16] YIN Cai-Liu(尹彩流), HUANG Qi-Zhong(黄启忠), WANG Xiu-Fei(王秀飞), et al. Carbon Techn.(Tansu Jishu), 2009, 28(3):19-22
17. [17]
  [17] Sun X M, Li Y D. Angew. Chem. Int. Ed., 2004,43:3827-3831
18. [18]
  [18] Sun X M, Li Y D. Angew. Chem. Int. Ed., 2004,43:597-601
19. [19]
  [19] Cui X J, Antonietti M, Yu S H. Small, 2006,2:756-759
20. [20]
  [20] Sevilla M, Fuertes A B. Carbon, 2009,47:228-229
21. [21]
  [21] Sevilla M, Fuertes A B. Chem. Eur. J., 2009,15:4195-4203
22. [22]
  [22] Baccile N, Laurent G, Babonneau F, et al. J. Phys. Chem. C, 2009,113:9644-9654
23. [23]
  [23] Mi Y Z, Hu W B, Dan Y M, et al. Mater. Lett., 2008,62: 1194-1196
24. [24]
  [24] Zheng M, Liu Y, Xiao Y, et al. J. Phys. Chem. C, 2009,113: 8455-8459
25. [25]
  [25] Zheng M, Liu Y, Jiang K, et al. Carbon, 2010,48:1224-1233
26. [26]
  [26] Tuinatra F, Koenig J L. J. Chem. Phys., 1970,53:1126-1130
27. [27]
  [27] Ferrari A C, Robertson J. Phys. Rev. B, 2000,61:14095-14107
28. [28]
  [28] Ferrari A C. Solid State Commun., 2007,143:47-57
29. [29]
  [29] Compagnini G, Puglisi O, Foti G. Carbon, 1997,35:1793-1797
30. [30]
  [30] Tan P, Dimovski S, Gogotsi Y. Phys. Eng. Sci., 2004,362: 2289-2310
31. [31]
  [31] Chadli H, Rahmani A, Sbai K, et al. Phys. A, 2005,358: 226-236
32. [32]
  [32] Lu X, Sun C, Li F, et al. Chem. Phys. Lett., 2008,454:305-309
33. [33]
  [33] Tapasztó L, Kertész K, Vértesy Z, et al. Carbon, 2005,43: 970-977
34. [34]
  [34] Yue Z R, Jiang W, Wang L, et al. Carbon, 1999,37:1785-1796
35. [35]
  [35] Puziy A M, Poddubnaya O I, Socha R P, et al. Carbon, 2008,46:2113-2123
36. [36]
  [36] Cai W, Piner R D, Stadermann F J, et al. Science, 2008, 321:1815-1817
37. [37]
  [37] Hayashia S, Hoshib F, Ishikurab T, et al. Carbon, 2003,41: 3047-3056
38. [38]
  [38] Rafalskii R P, Medvedeva L S, Prisyagina N I, et al. Geokhimiya, 1983,5:665-676
39. [39]
  [39] Bondarenko G V, Gorbaty Y E. Geochimica et Cosmochimica Acta, 1997,61:1413-1420
40. [40]
  [40] Tsuchiya N, Suto Y, Kabuta T, et al. J. Mater. Sci., 2008, 43:2115-2122
41. [41]
  [41] Gorbaty Y E, Gupta R B. Ind. Eng. Chem. Res., 1998,37: 3026-3035
42. [42]
  [42] Gorbaty Y E, Kalinichev A G. J. Phys. Chem., 1995,99: 5336-5340
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1.
沈阳化工大学材料科学与工程学院沈阳 110142