Yellow-emitting a-SiAlON:Eu 2+ phosphors were synthesized by the gas reduction and nitridation of a homogeneous oxide precursor in a CaO-Al 2 O 3 -SiO 2 -Eu 2 O 3 system at 1400-1450 1C using an NH 3 -CH 4 mixture gas as a reduction-nitridation agent. The precursor was prepared by a sol-gel process using a low-cost nitrate, tetraethyl orthosilicate and citric acid as the starting materials. The effects of reaction parameters such as heating rate, temperature, holding time and CH 4 content on the composition, microstructure and photoluminescence of the prepared powders were investigated. Nearly single-phase a-SiAlON was successfully synthesized by the onestep gas reduction and nitridation without the need for post-annealing at a higher temperature. The prepared powders consisted of relatively well-dispersed and uniform crystals with a hexagonal shape. The photoluminescence spectra of Eu-doped Ca-a-SiAlON phosphors excited by near-ultraviolet or blue light showed a broad, yellow emission band at 500-700 nm, which agrees well with that obtained from phosphors prepared by the conventional solid-state reaction. r