A novel synthesis route for the production of Sr3MgSi2O8:Eu2+,Dy3+ sub-micron quasisphere phosphor powder is reported. Both the host and activator cations were co-precipitated in water-ethanol mixed solutions and precipitation was performed with analytical grade ammonium citratetribasic. As the dispersion media, optimum concentration for PEG in the precursor solution is determined to be 0.08 g/mL. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM) and fluorescence spectrophotometer were employed to characterize the phosphor. The effect of the calcining temperature on the crystalline particle and luminescence properties of Sr3MgSi2O8:Eu2+,Dy3+ is systematically discussed. Sr3MgSi2O8:Eu2+,Dy3+ single phased quasi-sphere phosphor was achieved by calcining the asprecipitated precursor at 1100°C. Sr2SiO4 was identified as the intermediate phase during the calcination process. Despite the small particle size, the emission intensities were higher by the present method. However, the afterglow characteristic was not better than that prepared by solidstate reaction in the comparable condition.