Graphite intercalation compounds with BF3/F2: preparation and characterization

Electrochemical Synthesis of Graphite-Tetrafluoroaluminate Intercalation Compounds

“…compound without co-intercalation). 9 Similar phenomena were observed for GICs of other anions prepared in organic solutions. 24,25 The thermogravimetric curve of the stage-3 AlF4-GIC is shown in Figure 6 with that of PVdF for comparison.…”

“…Al-F bond of 0.165 nm for the tetrahedral AlF4 - [13]) 17 . This gallery height is slightly larger than that of BF4-GIC (0.749 nm) with the same orientation in the graphite layers, 9 as is expected from the sizes and geometry of AlF4and BF4 -. Although potentiostatic electrolysis at higher potentials was attempted, an AlF4-GIC at lower stage (stage-1 or stage-2 GICs) was not obtained.…”

Highly fluorinated graphite prepared from graphite fluoride formed using BF3 catalyst

“…Their signals dominate the spectra; however, the broad line is present whatever T T . It has been shown by 19 F NMR experiment on BF 3 -GIC [20,23] that the chemical shift of BF 4 À is equal to -148.5 ppm; the value is shifted slightly in comparison with pure BF 4 À (À149.5 ppm) [24]. For T T above 350 8C, the line located at -149.5 ppm is the more intense whereas for CF x -raw and for CF x (T T > 300 8C), the line at À154.5 ppm, corresponding to HF n species as discussed before, is predominant.…”

“…When the sample is exposed to air, the moisture could react with labile fluorine of the fluorocarbon matrix, certainly to form HF or HF 2 À (noted HF n ). A typical 19 F spectrum of fluorine-intercalated graphite at room temperature consists of two types of line: a narrow line assigned to mobile fluorine species and a broad line assigned to fluorine in stronger interaction with carbon atoms which constitute the ''rigid lattice'' [10][11][12][13][20][21][22]. Narrow lines at À154.5 and À149.5 ppm are observed on the spectra of CF x -raw and of CF x (T T 450 8C) (Fig.…”

A lifetime of fluorine chemistry

“…This was made possible by the complete separation of the reaction chamber from the weighing mechanism by magnets coupled via a sapphire window with a feedback mechanism for keeping the distance between the magnets constant. For example, I show the intercalation of HOPG with mixtures of BF 3 and fluorine [26] (Fig. 3).…”