The purpose of the research is to investigate the changes in microstructure and physicochemical characteristics, mainly surface charge (i.e. zeta potential) of zirconia membrane top layer during calcination. Zirconia is one of the most commonly preferred materials for ceramic membrane top layers due to its superior durability. The physicochemical properties of the top layer composed of submicron / nano particles is necessary not only for Donnan exclusion but also for dynamics of membrane fouling. In the present research the possibility of preparation of zirconia top layers with varying surface charge with changing calcination temperature was shown and a correlation between phase transformation and surface charge was determined.