In the present study the thermal decomposition of a freeze-dried copper(II) acetate monohydrate powder, (CH 3 COO) 2 Cu . H 2 O, (FDCuAcH 2 O), was analysed by a combination of high-temperature X-ray diffractometry; differential scanning calorimetry and thermogravimetry, up to 700 °C. The structure and morphology of the calcined freeze-dried powders were analysed by scanning electron microscopy and X-ray diffractometry. The results showed that FDAcCuH 2 O decomposes during heating in two stages: I) (25-225 °C) FDCuAcH 2 O dehydrates giving rise to copper(II) acetate, (CH 3 COO) 2 Cu, (AcCu), and II) (225-525 °C) AcCu decomposes to CuO through complex oxidation reactions of Cu and Cu 2 O, simultaneously. SEM showed that FDCuAcH 2 O powder has a scale-like morphology, which is created in the freezing stage and retained after freeze-drying. After calcination at 125 and 225 °C, clusters of elongated tubes (or filaments) compose the resulting powder (AcCu). Subsequent calcination at temperatures above 325 °C resulted in hard clusters of spheroid-like CuO particles.