LiCl-KCl熔盐中纯氧氧化提纯单壁碳纳米管PurificationofSingle.PDF

2010 年第68 卷 化 学 学 报 Vol. 68, 2010 第5 期, 413～417 ACTA CHIMICA SINICA No. 5, 413～417 ·研究论文· LiCl-KCl 熔盐中纯氧氧化提纯单壁碳纳米管 瞿美臻a,b 林浩强a 于作龙*,a (a 中国科学院成都有机化学研究所 成都 610041) (b 中国科学院研究生院 北京 100039) 摘要 以LiCl-KCl (wLiCl ∶wKCl ＝55 ∶45)熔盐为反应介质, 对在熔盐中纯氧氧化提纯单壁碳纳米管(SWCNT)进行了研 究. 发现可以通过控制熔盐温度和氧气流量来控制氧化反应温和地进行. 将5 g SWCNT 粗产品分散在200 g 熔盐中, 在470 ℃下用300 mL•min－1 氧气氧化2 h 可获得3.8% SWCNT 收率. 采用TEM, SEM, TGA 和Raman 谱对提纯前后 SWCNT 的形貌和组成进行了分析, 发现提纯后SWCNT 产品中无定形碳被有效去除, 而SWCNT 结构未发现明显变化. 关键词 碳纳米管; 熔盐; 无定形碳; 氧气氧化 Purification of Single-walled Carbon Nanotubes by Oxygen Oxidation in LiCl-KCl Molten Salt Qu, Meizhena,b Lin, Haoqianga Yu, Zuolong*,a a ( Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041) (bGraduate University of Chinese Academy of Sciences, Beijing 100039) Abstract The purification of SWCNT by oxygen oxidation in LiCl-KCl molten salt was investigated. 5 g of as-prepared SWCNT was suspended in 200 g of molten salt (wLiCl ∶wKCl ＝55 ∶45) at 470 ℃ by agita- －1 tion. After 2 h oxidation in 300 mL•min oxygen flow, 3.8% of purified SWCNT was obtained. The oxida- tion degree could be controlled by adjusting the reaction temperature and oxygen flow rate. Scanning elec- tron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and Raman spectra were employed to characterize the as-prepared and purified SWCNT. The results indicated