物理化学学报 >> 2017, Vol. 33 >> Issue (9): 1915-1922.doi: 10.3866/PKU.WHXB201705083

论文 上一篇    

微波辅助裂解离子液体制备硫氮共掺杂多孔碳材料

蒙延双1,3,王琛1,王磊1,王功瑞1,夏军1,朱福良1,3,*(),ZHANG Yue2,*()   

  1. 1 兰州理工大学材料科学与工程学院,兰州730050
    2 Department of Mechanical and Industrial Engineering, Texas A & M University-Kingsville, Kingsville, Texas 78363, USA
    3 省部共建有色金属先进加工与再利用国家重点实验室,兰州730050
  • 收稿日期:2017-03-22 发布日期:2017-07-05
  • 通讯作者: 朱福良,ZHANG Yue E-mail:chzfl@126.com;yue.zhang@tamuk.edu
  • 基金资助:
    国家自然科学基金(51364024);国家自然科学基金(51404124);甘肃省自然科学基金(1506RJZA100);甘肃省基础研究创新群体计划项目(1606RJIA322)

Efficient Synthesis of Sulfur and Nitrogen Co-Doped Porous Carbon by Microwave-Assisted Pyrolysis of Ionic Liquid

Yan-Shuang MENG1,3,Chen WANG1,Lei WANG1,Gong-Rui WANG1,Jun XIA1,Fu-Liang ZHU1,3,*(),Yue ZHANG2,*()   

  1. 1 School of Materials Science and Engineering, Lanzhou University of Technology, Lanzhou 730050, P. R. China
    2 Department of Mechanical and Industrial Engineering, Texas A & M University-Kingsville, Kingsville, Texas 78363, USA
    3 State Key Laboratory of Advanced Processing and Recycling of Non-ferrous Metals, Lanzhou 730050, P. R. China
  • Received:2017-03-22 Published:2017-07-05
  • Contact: Fu-Liang ZHU,Yue ZHANG E-mail:chzfl@126.com;yue.zhang@tamuk.edu
  • Supported by:
    the National Natural Science Foundation of China(51364024);the National Natural Science Foundation of China(51404124);Natural Science Foundation of Gansu Province, China(1506RJZA100);the Foundation for Innovation Groups of Basic Research in Gansu Province, China(1606RJIA322)

摘要:

采用一步微波辅助裂解离子液体法制备了硫氮共掺杂多孔碳材料。用傅里叶变换红外(FT-IR)光谱,拉曼光谱,X射线衍射(XRD),电子显微镜和X射线光电子能谱(XPS)等检测手段对裂解产物的结构和形貌进行了表征。对微波辐照下离子液体1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐(EMImNTf2)的裂解机理进行了分析。结果表明,微波辐照能够促进EMImNTf2的裂解,使其在320 ℃下裂解得到硫氮共掺杂的多孔碳材料。离子液体EMImNTf2的阳离子作为多孔碳材料骨架的前驱体,而阴离子作为硫源和造孔剂。制备的硫氮共掺杂多孔碳材料具有含缺陷的石墨结构。石墨碳基体中氮和硫的原子百分含量分别为12.84%和1.07%,其中N原子主要取代C成为活性点,而S原子主要存在于边界和缺陷处。

关键词: 硫氮共掺杂, 多孔碳, 微波, 裂解, 离子液体

Abstract:

Sulfur and nitrogen co-doped porous carbon (SNDPC) was successfully synthesized using one-step microwave-assisted pyrolysis of ionic liquid. The structure and morphology of the pyrolysis products were characterized by Fourier-transform infrared (FT-IR) spectroscopy, Raman spectroscopy, X-ray diffraction (XRD), electron microscopy, and X-ray photoelectron spectroscopy (XPS). The pyrolysis mechanism of the ionic liquid 1-ethyl-3-methylimidazolium bis((trifluoromethyl)sulfonyl)imide (EMImNTf2) under microwave irradiation was discussed. Microwave irradiation was found to accelerate the pyrolysis of EMImNTf2. The cation of EMImNTf2 works as the precursor of the carbon backbone of the porous carbon, while the anion acts as sulfur source and porosity-directing regulator. The SNDPC was obtained at 320 ℃ and exhibited graphitic structure with numerous surface defects. The atomic percentages of N and S in SNDPC were 12.84% and 1.07%, respectively. The N atoms mainly substitute the C sites in the graphitic carbon matrix, whereas the S atoms mainly bond to the ledges and defects of the carbon matrix.

Key words: Sulfur and nitrogen co-doped, Porous carbon, Microwave, Pyrolysis, Ionic liquid

MSC2000: 

  • O646