We report the structural and thermal characteristics of highly delithiated (lithium extracted) compounds Lix-NiO2, which can be called "nickel dioxide." We obtained Li0.10NiO2 and Li0.04NiO2 by treating LiNiO2 with sulfuric acid. Both products contained phases with NiO2 stacking similar to cadmium chloride (O3-type), but the latter also included a phase with NiO2 stacking similar to cadmium iodide (O1-type). We examined their thermal behavior using high temperature X-ray diffraction analysis together with thermogravimetric analysis and found that novel polymorphs, with similar chemical compositions but different structures, were obtained by heating them at appropriate temperatures. We discuss these results together with those for LixNiO2 obtained by electrochemical delithiation. We also report acid-treated products derived from Li0.93Ni1.07O2. (C) 2002 Elsevier Science.