Phase evolution of copper-containing zirconium phosphates during the temperature treatment up to 900 °C and formation of active Cu0 particles on the surface of these materials in H2/Ar flow were studied. The materials were characterized by XRD, TEM, TPR-H2 at different steps of treatment. Temperature increase up to 900 °C led to removal of oxygen from the CuZr4P6O24 structure with formation of Cu+-containing compounds. Materials treated by H2-containing flow at 600 °C contained Cu0 particles with sizes from 2 nm to 1 μm. Mixed copper-zirconium phosphate was shown to adsorb CO above 80 °C, while pre-reduced materials adsorbed it starting from 30 °C with formation of CO2 above 100 °C.