ZnO, Li doped and Li,Ni co-doped ZnO powders to be later used as transparent conductive oxide (TCO) thin film were prepared by heat treatment of gels obtained from alcoholic Zn(CH 3 COO) 2 •2H 2 O, LiNO 3 •nH 2 O and NiSO 4 •6H 2 O solutions with (CH 3 CH 2 OH) 3 N as chelating agent. The properties of the powders and their thermal treatment were studied by thermogravimetric and termodifferential anlysis (TG/DTA), differential scanning calorimetry (DSC), evolved gas analysis coupled with mass spectroscopy (EGA-MS), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive X-ray (SEM/ EDX). The as-prepared gels consisted of submicron platelet-like particles and contained zinc acetate dihydrate and hydrozincite in different amount and with different preferred orientations. During annealing the gels, zinc-acetate decomposed between 110-350 °C with the release of CH 3 COOH, acetone and CO 2 . The N content of the chelating agent was responsible for NH 3 and NO evolution. The thermal behavior of the doped 3 gels was similar, but there were also differences in the mass losses, amount of released gases.Based on TG/DTA data, ZnO powders were obtained from the gels by annealing both at 275 and 500 °C. After heating at 275 °C, the obtained powders consisted of spherical 1-2 micron grains of wurtzite. The inclusion of the dopants was successful according to EDX and cell parameter data. Thermal study of the powder annealed at 275 °C confirmed that they still contain some zinc acetate. In the case of the doped samples the mass loss was smaller, since the Li and Ni dopants catalized the composition of zinc acetate during the previous annealing at 275 °C. After annealing the gels at 500 °C, stable un-doped ZnO or doped ZnO particles were obtained.