Abstract. Synthesis of oxides, nitrides, and oxynitrides of silicon and aluminium by a pulsed microwave discharge in the mixtures of metal and dielectric powders is described. The microwave pulses were generated by high-power gyrotron (frequency 75 GHz, power up to 550 kW, pulse duration from 0.1 to 15ms). SiO 2 + β-Si 3 N 4 (1:1 by molar) and α-Al 2 O 3 + AlN (2:1 by molar) mixtures with Mg (1 and 5wt%) were treated in air with microwave pulses with power of 250÷400 kW and duration of 2÷8 ms. It was found that the discharge cannot be initiated for both mixtures in absence of Mg at any pulse power and duration. When 1% of Mg was added, the discharge was observed for both mixtures under 8 ms pulses of 400 kW; however, the amounts of materials produced were not enough for analysis. With 5% of Mg the discharge was observed for both mixtures under 8 ms pulses of 350 kW, and products of the plasma-chemical processes in the Al 2 O 3 + AlN mixture were analyzed.