Published online by Cambridge University Press: 15 February 2011
The pH of the reaction media is a critical factor in the formation of new vanadium oxides with the tetramethylammonium (TMA) ion via the conventional hydrothermal method. New vanadium oxides; TMAV3O7, Li0.6V2−δO4−δ·H2O and Li0.6V2−δO4−δ, TMAV4O10, and two more new vanadium phases with d spacings of 11.5Å and 19.1Å are formed as the pH is varied with acetic acid. The synthesis and characterization of TMAV3O7, a new vanadium oxide with tetramethylammonium ions residing between its layers is discussed. The intercalation of alkylamines, DMSO, and water into Li0.6V2−δO4−δ·H2O is described. Microwave hydrothermal synthesis is a new and alternate soft chemistry technique used to accelerate the synthesis of TMAV4O10. This method also aided in the formation of a new cluster compound, [Li(H2O)4]2TMA(V10O28)·4H2O.