The mechanochemical process were employed to prepare the red phosphors (Y,Gd)BO_3:Eu3+. The main factors affecting particle size, particle distribution, and luminescent properties of the product were investigated in details. Particles sized around 200-600 nm are formed after intensive milling. The phosphors were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and photoluminescence spectrum. Results revealed that phosphors with different morphology, small particle size and high luminescence intensity could be obtained by mechanochemical process.