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A mixed alkali metal titanate of composition AxTi2-x/3Lix/3O4 (A = K, Rb, Cs) has been prepared and its ion-exchange/intercalation properties have been explored. Solid-state calcination of appropriate mixtures of TiO2 and alkali metal carbonates produced the titanate at a stoichiometry of x = 0.80 for A = K, 0.75 for Rb, and 0.70 for Cs. Rietveld refinement on neutron diffraction data confirmed that the orthorhombic structure is comprised of lepidocrocite-related host layers of Ti2-x/3Lix/3O4 and charge-balancing A ions in the interlayer domain. Complete extraction of both alkali metal ions was achieved by acid-leaching, producing a new protonic titanate of H4x/3Ti2-x/3O4·H2O. This phase is distinguished from isomorphous related compounds in terms of high proton content as a consequence of exchangeable Li ions located in the host framework. The material took up alkali metal ions and organoammonium ions from aqueous media. These ion-exchange and intercalation reactions brought about expansion/contraction of the gallery height and lateral displacement of the layers. The resulting various types of layer sequence can be understood in terms of the nature of the interlayer species.
Sasaki et al. (Tue,) studied this question.