Precipitation of solvent-free C60(CO2)0.95 from Conventional solvents: A new antisolvent approach to controlled crystal growth using supercritical carbon dioxide

Christian N. Field, Paul A. Hamley, Jeremy M. Webster, Duncan H. Gregory, Jeremy J. Titman, Martyn Poliakoff

研究成果: ジャーナルへの寄稿学術誌査読

38 被引用数 (Scopus)

抄録

C60(CO2)x, where x = 0.2 or 0.95, has been synthesized from solutions of C60 in conventional organic solvents using antisolvent precipitation with supercritical CO2. The technique requires much lower pressures and temperatures than current routes to C60(CO2)x and, for small quantities, is quicker. Products were characterized by SEM, IR, 13C solid-state NMR, and powder XRD. Reitveld refinement of the powder XRD shows CO2 to be located in the octahedral interstitial sites of the C60 lattice. The cell lattice parameter is observed to increase for higher occupancies of CO2. Experimental conditions can be varied to generate radically different morphologies of C60(CO2)x. Using rapid antisolvent precipitation, irregular aggregates of ca. 200 nm particles are formed, where x = 0.2. With slower, diffusion-controlled precipitation, regular, highly crystalline; octahedral-shaped particles (1-70 μm) can be formed, where x = 0.95. All products were precipitated completely free from the original organic solvent, and we conclude that CO2 has entered the lattice during crystallization.

本文言語英語
ページ(範囲)2480-2488
ページ数9
ジャーナルJournal of the American Chemical Society
122
11
DOI
出版ステータス出版済み - 3月 22 2000
外部発表はい

!!!All Science Journal Classification (ASJC) codes

  • 触媒
  • 化学一般
  • 生化学
  • コロイド化学および表面化学

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