Synthesis and structure refinement of LiCoO2 single crystals

Single crystals of LiCoO2 have been successfully synthesized for the first time in a scaled gold tube by a flux method at 1173 K, A single-crystal X-ray diffraction study confirmed the trigonal R (3) over bar m space group and the lattice parameters a = 2.8161(5) Angstrom and c = 14.0536(5) Angstrom. No superstructure could be observed in the single-crystal S-ray diffraction photographs. The crystal structure has been refined to the conventional values R = 3.1% and wR = 3.5% for 217 independent observed reflections. The refined oxygen parameter, z is 0.23951(15), which is in good agreement with the previous result by powder neutron diffraction method. The short O-O contact distance of 2.614(2) Angstrom in the CoO6 octahedron is confirmed by the present structure refinement. (C) 1998 Academic Press.