LiNi y Ti1−y O2 (0.7≤y≤0.95) solid solution has been prepared by a wet process. According to X-ray diffraction analysis, these materials are found to have a rhombohedral layered structure(R 3 ̄ m) and are an isostructure LNiO2. The I(104)/I(003) intensity ratio is increased with Ti concentration, which indicates the cation mixing between transition metal layer and lithium layer is occurred. The LiNi y Ti1−y O2 compounds have well-developed layered structures and a particle size of ∼1μm. The titanium and nickel in the lattice is found to be trivalent and bivalent, respectively. The first discharge capacity of LiNi y Ti1−y O2 is 10–25mAhg−1. These values are inferior to those of LiNi y Ti1−y O2 prepared by a solid-state reaction (30mAhg−1). The low discharge capacities are due to local structural change during the first charge, where transition metal ions in the lithium layer block the diffusion of Li ions.