AbstractWe have prepared ZnO thin films by the sol–gel method from a 2‐methoxyethanol solution of zinc acetate dihydrate stabilized by 2‐aminoethanol on SiO2 substrates. The structure of the films showed a significant dependency on thermal treatment temperature, not only in the final thermal‐annealing process at several hundreds of degrees, but also in the heat‐treatment after spin coating at lower temperature, which is performed to evaporate the organic solvent in the films. The intensity of the (0002) peak in X‐ray diffraction showed significant dependence on the heat treatment conditions after spin coating, which ranged from 100 to 300 °C. The temperature employed in the initial 10 min of the heat treatment was found to be important in determining the structure of the film. The results indicate that the elimination condition of the organic components is important for achieving high crystallinity