The work reports the synthesis and of 9CaO-91ZrO₂ (mol.%) precursor, synthesized by co-precipitation from mixed water-acetone solution. By SEM and adsorption-desorption analysis it was shown that acetone addition acts as cryoprotectant effectively reducing the growth of large hexagonal ice crystals during freeze-drying and results in microporous flakes-like particles. STA analysis showed the decreased crystallization enthalpy comparing to values for powder, obtained from aqueous solution. For the first time the systematic investigation of thermal evolution of agglomerates, crystallites and phase composition of powder obtained from mixed water-7vol.% acetone solution has been performed via PSD and XRD.