A series of boride (TiB2, ZrB2, NbB2, CeB6, PrB6, SmB6, EuB6, LaB6), carbide (SiC, TiC, NbC, WC), and nitride (TiN, BN, AlN, MgSiN2, VN) micro/nanocrystals are prepared from the corresponding metal oxides and amorphous boron/active carbon/NaN3 in the presence of metallic Na and elemental S (autoclave, 150 °C, 2 h).