Mixed metal nitrides, M2Si5N8:Ce3+ (M = Ca, Sr, Ba), were synthesized from M2-yCeySi5 or an appropriate mixture of MSiHx, Si3N4 and CeF3, by a direct nitriding process in N-2 gas: 2 MSiHx + Si3N4 + CeF3 -> M2Si5N8:Ce3+. Also, charge-compensated materials, M2AlzSi5-zN8:Ce3+, were prepared (from an appropriate mixture of MSiHx, MAlSiHx, Si3N4 and CeF3) and the luminescence properties were characterized. The resultant phosphors showed green emission suitable for LED illumination by optimizing the mixing ratio of metal elements.