Europium activated yttrium oxide phosphors were prepared by reagent simultaneous addition technique, using oxalic acid as precipitating reagent. The aim of the paper is to establish the flux influence and thermal regime on photoluminescence and morpho-structural characteristics of phosphor powders. In this respect different mineralising agents such as sodium/lithium carbonate, sodium tetraborate ans sodium pyrophosphate were used during the thermal synthesis stage. Thermal analysis, X-ray diffraction, scanning electron microscopy, infrared spectroscopy and photoluminescence measurements were used to investigate precursor and phosphor powders. The correlation between the phosphor properties and precursor quality enabled us to select the optimal synthesis conditions.