The influence of tribophysical activation on Zn2TiO4 synthesis along with the changes in powders during tribophysical treatment was observed. Mixtures of ZnO and TiO2 powders were mechanically activated using a high-energy ball mill at different time intervals from 0 to 300 minutes. XRD was performed in order to obtain information about phase composition variations. Microstructure parameters were revealed from an approximation method. Particle size distribution along with scanning electron microscopy gave very useful information about powder morphology.