【作者】 王凯；

【导师】 彭汝芳；

【作者基本信息】 西南科技大学 ， 应用化学， 2010， 硕士

【摘要】 本文研究并获得了电弧放电法制备内嵌金属富勒烯Gd@C₈₂的最佳工艺条件:氦气压力0.08MPa,摩尔比Gd:C=1:15-1:20,活化电流200A,活化时间30min以上,反应电流90¹00A。详细研究并获得了制备烟灰中Gd@C₈₂分离纯化条件和方法:以DMF为溶剂,减压萃取至无色;再以Buckyprep-M柱为色谱柱,甲苯为流动相,流速为10mL/min,采用高效液相色谱分离,Gd@C₈₂保留时间为40⁵0min。研究了滴覆法及真空蒸镀法在富勒烯镀膜中的应用,并首次将旋涂法引入富勒烯镀膜,且取得了较好的结果,最终确定旋涂法及真空蒸镀法可以应用于富勒烯镀膜。研究了液-液界面微环境对富勒烯晶型的影响,并制备了常温下不易稳定存在的简单六方C60晶体,为以后Gd@C₈₂的镀膜研究提供了实验依据。最后使用Dmol3程序计算了C₈₂碳笼和Gd@C₈₂碳笼的一些性质,解释了Gd@C₈₂制备过程中遇到的一些现象,并预测了Gd@C₈₂的一些化学性质。更多还原

【Abstract】 In this paper, process conditions preparing endohedral metallofullerene Gd@C₈₂ by arc-discharge method are studied, and its best technological conditions are obtained: helium pressure 0.08 MPa, nGd: nC = 1:15-1:20, activation current 200A, activation time 30min, reaction current I = 90 100A; conditions of separation and extraction of Gd@C₈₂ from soot are studied: firstly, the soot is extracted in vacuum with DMF as the solvent; secondly, Gd@C₈₂ is separated by Buckyprep-M column and its retention time is about 40 50min when the mobile phase is toluene and flow rate is 10mL/min. Applications to fullerene film of drop-coating method and vacuum evaporation method are studied. Spin-coating is introduced into fullerene film in the first time, and achieves good results. Ultimately spin-coating method and vacuum evaporation coating method are determinted to can be applied to fullerene film. Effects of liquid - liquid interface micro-environment on of the fullerene crystal are studied, and simple cubic C60 crystal not easily prepared at room temperature are abtained. At last some properties of C₈₂ and Gd@C₈₂ carbon cage are calculated using the Dmol3, some phenomena encountered in the preparation of Gd@C₈₂ are explained, and some chemical properties of Gd@C₈₂ are predicted.更多还原