Operando X-ray diffraction during battery cycling at elevated temperatures: A quantitative analysis of lithium-graphite intercalation compounds

AbstractIntercalation compounds of graphite with Sn(CH3)3Cl have been prepared by UV irradiation, in the presence of graphite, of solutions of Sn(CH3)3Cl, Sn(CH3)4, or of Sn(CH3)4 + SnCl4 in CCl4. Mixtures of stage 1, stage 2, and stage 3 compounds have been obtained. They were characterized by X-ray diffraction, 119Sn Mossbauer spectroscopy, and by chemical analysis. Apparently an oligomeric, anionic species is intercalated together with some solvent.

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X-Ray Diffraction from Graphite Intercalation Compounds Under Hydrostatic Pressure

Springer Series in Solid-State Sciences - Physics of Intercalation Compounds ◽

10.1007/978-3-642-81774-8_29 ◽

1981 ◽

pp. 214-222 ◽

Cited By ~ 3

Author(s):

S. A. Solin

Keyword(s):

Hydrostatic Pressure ◽

Intercalation Compounds ◽

X Ray Diffraction ◽

Graphite Intercalation Compounds ◽

X Ray ◽

Graphite Intercalation

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Preparation of FeCl3–IBr–H2SO4–graphite multi-intercalation compounds

Journal of Materials Research ◽

10.1557/jmr.1994.0377 ◽

1994 ◽

Vol 9 (2) ◽

pp. 377-382 ◽

Cited By ~ 5

Author(s):

Takeshi Abe ◽

Yasuo Mizutani ◽

Eiji Ihara ◽

Mitsuru Asano ◽

Toshio Harada

Keyword(s):

Saturated Vapor ◽

Intercalation Compound ◽

Intercalation Compounds ◽

Stacking Sequence ◽

X Ray Diffraction ◽

Graphite Intercalation Compounds ◽

X Ray ◽

Graphite Intercalation ◽

Diffraction Patterns

Stages 4-6 FeCl3-graphite intercalation compounds (GIC's) have been prepared by an ordinary two-bulb method, and FeCl3-IBr-graphite bi-intercalation compounds (GBC's) are synthesized by holding the FeCl3-GIC's in the saturated vapor of IBr. The x-ray diffraction patterns of the FeCl3-IBr-GBC's obtained from stages 4, 5, and 6 FeCl3-GIC's give the stacking sequences as G(FeCl3)GG(IBr)GG(FeCl3)G, G(FeCl3)GG(IBr)GGG(FeCl3)G, and G(FeCl3)GG(IBr)GG(IBr)GG(FeCl3)G, respectively, where G, (FeCl3), and (IBr) refer to the graphite, FeCl3, and IBr layers, respectively. The multi-intercalation of H2SO4 into the FeCl3-IBr-GBC's synthesized from stages 4 and 6 FeCl3-GIC's occurs at all the vacant galleries of the GBC's at the same time. In contrast, the multi-intercalation of H2SO4 into the FeCl3-IBr-GBC obtained from the stage 5 FeCl3-GIC takes place in two processes. The first multi-intercalation occurs at the gallery adjacent to the bi-intercalated IBr layer, and the stacking sequence of the resulting graphite multi-intercalation compound is determined to be G(FeCl3)GG(IBr)G(H2SO4)GG(FeCl3)G, where (H2SO4) refers to the H2SO4 layer. The second multi-intercalation occurs at all the rest of the vacant galleries.

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Preparation of stages 2–4 ternary AlCl3–FeCl3-graphite intercalation compounds

Journal of Materials Research ◽

10.1557/jmr.1995.1196 ◽

1995 ◽

Vol 10 (5) ◽

pp. 1196-1199 ◽

Cited By ~ 1

Author(s):

Takeshi Abe ◽

Yasuo Mizutani ◽

Mitsuru Asano ◽

Toshio Harada

Keyword(s):

Vapor Pressure ◽

Gas Phase ◽

Intercalation Compound ◽

Intercalation Compounds ◽

Graphite Intercalation Compound ◽

X Ray Diffraction ◽

Vapor Species ◽

Graphite Intercalation Compounds ◽

X Ray ◽

Graphite Intercalation

Intercalation of AlCl3 into stage 2 FeCl3-graphite intercalation compound (GIC) using an ordinary two-bulb method has been studied by x-ray diffraction. Stages 2, 3, and 4 ternary AlCl3-FeCl3-GlC's are obtained when the temperatures of the stage 2 FeCl3-GIC were set at T (GIC) = 503, 523, and 553 K, respectively, for the AlCl3 intercalate material at T (AlCl3) = 473 K, that is, the vapor pressure of (AlCl3)2 (g) of the main vapor species to be held at p {(AlCl3)2} = 2.4 × 105 Pa. However, for the temperature of the stage 2 FeCl3-GIC at T (GIC) = 573 K, the (AlCl3)2 (g) vapor is found to promote the decomposition of the stage 2 FeCl3-GIC, resulting in the formation of graphite. The decomposition of the stage 2 FeCl3-GIC is considered to take place because the complex AlFeCl6 (g) in the gas phase, which is formed from both (AlCl3)2 (g) and FeCl3 existing at the edge of the FeCl3-GIC, is thermodynamically more stable than the FeCl3 and AlCl3 intercalates in their GIC at p {(AlCl3)2} = 2.4 × 105 Pa and T (GIC) = 573 K.

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