含铁碳纳米纤维的制备与表征
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摘要
功能性碳纤维在能源、环保、航天等方面得到了广泛的应用,其中负载金属的碳纤维是材料科学研究的前沿,可控制备载铁碳纳米纤维具有重要意义。
本论文以DMF作为溶剂,将二茂铁(Fc)溶于质量分数为15%的聚丙烯腈(PAN)溶液,以N,N-二甲基甲酰胺和四氢呋喃作为混合溶剂,配制聚丙烯腈和聚二茂铁硅烷(PFS)的共混溶液。采用静电纺丝,分别得到PAN/Fc和PAN/PFS微纳前驱体纤维,对得到的纤维进行预氧化和炭化处理,最终得到了含Fe的碳纳米纤维膜。
初步研究了静电纺制备纳米纤维前驱体、纤维的预氧化和纤维炭化工艺,利用TGA分析了纳米纤维前驱体的热失重规律,SEM、TEM、XPS、FTIR和Raman分别对纳米纤维的形貌、尺寸、组成和结构演变进行了表征。结果表明:经热处理后纤维直径明显减小,含PFS的纤维中表面有元素Fe,并随热处理的深入Fe价态发生变化。
Functional carbon fibers are important and have a wide range of applications from energy to the aerospace industry, and the carbon nanofibers containing metal become foreland domain of materials science research, So controllable Preparation of carbon nanofibers containing iron is important.
In the present work, PAN/Fc nanofibers were prepared by electrospinning using a composite solution of Fc dispersed into 15 Wt.% polyacrylonitrile (PAN) solution in DMF, and a mixture of polyacrylonitrile and polyferrocenylsilanes in N, N-dimethylformamide and tetrahydrofuran were electronspun into submicrometer fibers. The fiber precursors were stabilized, and then carbonized, the carbon nanofibers containing iron were successfully prepared.
The electrospinning, stabilization, and carbonization processes were researched. The thermal decomposition of nanofiber precursors were charactered by TGA, and the morphology, size, structure evolution, and components of nanofibers were characterized by SEM, TEM, XPS, FTIR, and Raman. The results show that the diameters of the nanofibers were decreased during the pyrolysis process, Fe were contained in the surface of the PAN/PFMMS fibers and the valence state of Fe changed in the stabilization and carbonization processes.
本论文以DMF作为溶剂,将二茂铁(Fc)溶于质量分数为15%的聚丙烯腈(PAN)溶液,以N,N-二甲基甲酰胺和四氢呋喃作为混合溶剂,配制聚丙烯腈和聚二茂铁硅烷(PFS)的共混溶液。采用静电纺丝,分别得到PAN/Fc和PAN/PFS微纳前驱体纤维,对得到的纤维进行预氧化和炭化处理,最终得到了含Fe的碳纳米纤维膜。
初步研究了静电纺制备纳米纤维前驱体、纤维的预氧化和纤维炭化工艺,利用TGA分析了纳米纤维前驱体的热失重规律,SEM、TEM、XPS、FTIR和Raman分别对纳米纤维的形貌、尺寸、组成和结构演变进行了表征。结果表明:经热处理后纤维直径明显减小,含PFS的纤维中表面有元素Fe,并随热处理的深入Fe价态发生变化。
Functional carbon fibers are important and have a wide range of applications from energy to the aerospace industry, and the carbon nanofibers containing metal become foreland domain of materials science research, So controllable Preparation of carbon nanofibers containing iron is important.
In the present work, PAN/Fc nanofibers were prepared by electrospinning using a composite solution of Fc dispersed into 15 Wt.% polyacrylonitrile (PAN) solution in DMF, and a mixture of polyacrylonitrile and polyferrocenylsilanes in N, N-dimethylformamide and tetrahydrofuran were electronspun into submicrometer fibers. The fiber precursors were stabilized, and then carbonized, the carbon nanofibers containing iron were successfully prepared.
The electrospinning, stabilization, and carbonization processes were researched. The thermal decomposition of nanofiber precursors were charactered by TGA, and the morphology, size, structure evolution, and components of nanofibers were characterized by SEM, TEM, XPS, FTIR, and Raman. The results show that the diameters of the nanofibers were decreased during the pyrolysis process, Fe were contained in the surface of the PAN/PFMMS fibers and the valence state of Fe changed in the stabilization and carbonization processes.
引文
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[3]胡爱娟,崔玉双,孔令泉,鲁在君.含聚丙烯腈的嵌段共聚物及其纳米碳材料.中国科技论文在线. 2008, 3(6):395-403.
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[5]贺福.碳纤维及其应用技术.北京:化学工业出版, 2004, p64-69, 160-179.
[6]杨秀珍,李青山,卢东.聚丙烯腈基碳纤维研究进展.现代纺织技术. 2007, 1, 45-47.
[7]朱群玉,王庆瑞.聚丙烯腈基活性中空炭纤维的制备和性能的研究.博士论文. 2006.
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[13] Chen, J. T.; Shin, K.; Leiston-Belanger, J. M.; Zhang, M.; Russell, T. P. Amorphous carbon nanotubes with tunable properties via template wetting. Adv. Funct. Mater. 2006, 16(11):1476-1480.
[14] Wang, J.; Yang, Q.; Zhang, Z. Selective synthesis of magnetic Fe2P/C and FeP/CCore/Shell nanocables. J. Phys. Chem. Lett. 2010, 1(1):102-106.
[15] Ipaktschi, J.; Hosseinzadeh, R.; Schlaf, P. Self-assembly of quinodimethanesthrough covalent bonds: a novel principle for the synthesis of functionalmacrocycles. Angew. Chem. Int. Ed. 1999, 38(11):1658-1660.
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