PREPARATION OF LITI2O4 SINGLE-CRYSTALS WITH THE SPINEL STRUCTURE

Single crystals of the spinel-type LiTi2O4 (Cubic, Fd3m, a=8.4095(12) Å) have been prepared by the reaction of lithium metal and TiO2 at 1373 K in a sealed iron vessel. The structure refinement by a single crystal X-ray diffraction study confirmed a normal spinel cation distribution: the lithium cations are located at the tetrahedral 8a sites, the titanium cations occupy the octahedral 16d sites, and the oxygen parameter u=0.2622(4) with the final R=3.8%(Rw=2.7%) for 60 independent observed reflections. The octahedral Ti-O distance is 2.005(3) Å, and the tetrahedral Li-O distance is 1.999(3) Å. The superconductivity for the crystals was observed by the magnetization measurements. © 1992 Academic Press, Inc.