A series of alkylammonium-containing graphite intercalation compounds (GICs) are prepared via cation exchange reactions. Powder X-ray diffraction, thermogravimetric analyses (TGA), capillary zone electrophoresis, and elemental analyses provided structural and compositional details.  Both symmetric (R4N+) and asymmetric (RR'3N+, R2R'2N+) cations form single-phase, well-ordered GICs by exchange into C15Na(en)1.0.  The resulting GICs have lower cation contents and are dull black in color, as compared to the bright blue reactant, and most are prepared as stage-1 products.  C41[(C4H9)4N] comprises a flattened monolayer arrangement, with a gallery expansion of 0.47 nm. For the larger intercalate cations, (C6H13)4N+, (C7H15)4N+, and (C8H17)4N+,a flattened bilayer arrangement is obtained with gallery expansions close to 0.80 nm. The asymmetric alkylammonium GICs prepared with (C12H25)(CH3)3N+, (C18H37)(CH3)3N+, and (C18H37)2(CH3)2N+ all adopt a flattened bilayer arrangement.  For the bilayer structures, significant co-intercalation of the DMSO solvent occurs, as demonstrated by TGA-mass spectrometry and compositional data.

Synthesis of graphite intercalation compounds containing alkylammonium cations

245th National Meeting (2013)

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