Single crystals of LiCoO2 and LiNiO2 have been successfully grown for the f
irst time by a flux method. A single-crystal X-ray diffraction study confir
med trigonal symmetry, and their lattice parameters were a = 2.8161(5) Angs
trom and c = 14.0536(5) Angstrom for LiCoO2, and a = 2.8899(13) Angstrom an
d c = 14.1938(17) Angstrom for LiNiO2, respectively. The cation distributio
n in Li0.92Ni1.08O2 was determined to be (Li0.74Ni0.26)(3a)[Li0.18Ni0.82](3
b)O-2 with a final R value of 2.7% by a single-crystal X-ray structure anal
ysis. LiCoO2 proved to show a semiconducting behavior below room temperatur
e by an in-plane electrical resistivity measurement using the single crysta
l specimen.