Co-doped praseodymium nickelates PrNi1 - xCoxO3 - δ and their composites with yttrium doped ceria Ce0.9Y0.1O2 - δ are known to be promising materials for intermediate temperature solid oxide fuel cells and membranes for oxygen separation. Powdered samples were obtained via Pechini route and ultrasonic dispersion followed by mechanical activation. Pellets were sintered at 870-1100 °C by using microwave radiation. In comparison with conventionally sintered materials, the phase transition leading to Ruddlesden-Popper phase formation was shifted down for about 50 °C-100 °C. The effect of sintering by microwave radiation consisted of dramatically increased sample density, improved phase purity and enhanced oxygen mobility. When undesirable phase transitions at elevated sintering temperatures hinder gas-tight layers preparation, the microwave sintering technique can be used without any deterioration of transport properties of materials in comparison with conventional calcination.