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. 2010 Jan 1;157(2):A148-A154.
doi: 10.1149/1.3267042.

Solid-State NMR Studies of Chemically Lithiated CF

N D Leifer  1 , V S Johnson, R Ben-Ari, H Gan, J M Lehnes, R Guo, W Lu, B C Muffoletto, T Reddy, P E Stallworth, S G Greenbaum
Affiliations

Solid-State NMR Studies of Chemically Lithiated CF

N D Leifer et al. J Electrochem Soc. .

Abstract

Three types of fluorinated carbon, all in their original form and upon sequential chemical lithiations via n-butyllithium, were investigated by (13)C and (19)F solid-state NMR methods. The three starting CF(x) materials [where x = 1 (nominally)] were fiber based, graphite based, and petroleum coke based. The aim of the current study was to identify, at the atomic/molecular structural level, factors that might account for differences in electrochemical performance among the different kinds of CF(x). Differences were noted in the covalent F character among the starting compounds and in the details of LiF production among the lithiated samples.

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Figures

Figure 1
Figure 1
(Color online) 19F NMR of starting materials CFx C, F, and G on a 300 MHz spectrometer at 26–32 kHz spinning speeds.
Figure 2
Figure 2
(Color online) 19F NMR of lithiated CFx C series at 23 kHz spinning speed.
Figure 3
Figure 3
(Color online) 19F NMR (300 MHz) comparative quantitative line deconvolutions of lithiated (a) CFx C, (b) CFxF, and (c) CFxG. The numbers next to the species identifications refer to the chemical shift in parts per million, and the percentages on the horizontal axis describe the equivalent DOD.
Figure 4
Figure 4
(Color online) 13C NMR spectra of the lithiated CFx C series, shown as a representative example of the 13C NMR of the materials. The critical information is in the spectral deconvolutions, which are shown for all three samples.
Figure 5
Figure 5
(Color online) 13C NMR (500 MHz) comparison of quantitative spectral deconvolutions of (a) CFx C, (b) CFx F, and (c) CFx G. The numbers next to the species identifications refer to the chemical shift in parts per million, and the percentages on the horizontal axis describe the equivalent DOD.
Figure 6
Figure 6
(Color online) XRD of chemically lithiated CFx C.
Figure 7
Figure 7
(Color online) F/C ratio throughout lithiation of C and F series. The percentages on the horizontal axis describe the equivalent DOD.
Figure 8
Figure 8
(Color online) FTIR spectra of chemical lithiated CFx C at 0, 50, and 90% DOD. The doublets at ~2350 cm−1 are the CO2 background.
Figure 9
Figure 9
(Color online) 13C NMR (300 MHz) of solvent derivative species in (a) CFx C, (b) CFx F, and (c) CFx G.
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