The characterization of fluorinated graphite
The characterization of solid fossil fuels by chemical and spectroscopic methods requires extensive modelling in less complex systems for chemical proof of principle and technique development. In previous work coal was fluorinated with dilute, elemental fluorine under conditions that were expected to lead to materials that contain only fluoromethine moieties. The solid state, cross polarization/magic angle spinning (CP/MAS) {sup 13}C NMR spectra of the fluorinated coal are complex, indicating more chemical modification than originally anticipated. Our goal in the coal derivatization was to sequentially increase the severity of the fluorination and observe by {sup 19}F and {sup 13}C NMR the type and concentration of fluorine functional groups created in the coal milieu. This requires the ability to discriminate between C, CF, CF{sub 2}, and CF, moieties in the coal matrix. The task can be accomplished by implementing the spectral editing technique of Wu and Zilm which distinguishes different kinds of carbon resonances, especially CH and CH{sub 2} resonances. These experiments utilize cross polarization (CP) and polarization inversion (PI) to effect the discrimination. Our version of this experiment is a triple resonance experiment that incorporates {sup 19}F-{sup 13}C CP, PI, and simultaneous {sup 1}H and {sup 19}F dipolar decoupling. In order to evaluate the elemental fluorine chemistry in a matrix simpler than coal, fluorinated graphite was prepared. X-ray photoelectron spectroscopy (XPS) was used to characterize the surface species, i.e., count CF, CF{sub 2} and CF{sub 3} species. These well-characterized samples are the models we will use to test the NIVIR editing experiments. The XPS and atomic force microscopy (AFM) data on the first fluorinated graphites we have prepared are reported in this paper.
- Research Organization:
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
- Sponsoring Organization:
- USDOE Office of Energy Research, Washington, DC (United States)
- DOE Contract Number:
- AC05-96OR22464
- OSTI ID:
- 486033
- Report Number(s):
- CONF-950801-28; ON: DE97006326; TRN: 97:003954
- Resource Relation:
- Conference: 210. national meeting of the American Chemical Society (ACS), Chicago, IL (United States), 20-25 Aug 1995; Other Information: PBD: 1995
- Country of Publication:
- United States
- Language:
- English
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