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The Electrochemical Synthesis of the Graphite Intercalation Compounds Containing Tetra-n-alkylammonium Cations

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  • The electrochemical intercalation of tetra-n-alkylammonium (TAA) cations into graphite is investigated using galvanostatic reduction and cyclic voltammetry in TAABr/ dimethylsulfoxide (DMSO) electrolytes. Structural and compositional analyzes by X-ray diffraction, thermogravimetric and elemental analyzes show that stable graphite intercalation compounds (GICs) are formed with highly-flattened TAA cation bilayers for (C₅H₁₁)₄N⁺, (C₆H₁₃)₄N⁺, (C₇H₁₅)₄N⁺, (C₈H₁₇)₄N⁺, with gallery expansions of 0.81 nm. (C₄H₉)₄N⁺ forms a mixed-phase product including a stable GIC with monolayer TAA arrangement and a gallery expansion of 0.48 nm. The GICs with bilayer galleries incorporate 0.7–1.2 DMSO co-intercalate molecules per cation; the monolayer galleries contain relatively little DMSO. Although cyclic voltammetry shows that TAA cations smaller than (C₄H₉)₄N⁺ do intercalate into graphite, they do not form stable GICs. The GICs obtained by galvanostatic reduction are compared to those prepared using chemical ion-exchange reactions. A surface passivation model is introduced to explain the relative stabilities of GICs formed with larger TAA cation intercalates.
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  • Sirisaksoontorn, W., & Lerner, M. (2013). The electrochemical synthesis of the graphite intercalation compounds containing tetra-n-alkylammonium cations. Ecs Journal of Solid State Science and Technology, 2(9), M28-M32. doi:10.1149/2.042309jss
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  • 2
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  • 9
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  • The published article can be found at The Electrochemical Society.
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