Using polyethylene glycol (PEG), Tween-80, sodium dodecyl sulphonate (SAS) and cetyltrimethylammonium bromide (CTAB) as surfactants, CaMoO 4 : Eu 3+ red phosphors were prepared by co-precipitation method and their morphology, structure and luminescent properties were investigated by scanning electron microscope (SEM), X-ray diffraction (XRD) and fluorescence spectrometer. The results showed that the introduction of surfactants did not change the crystal structure of CaMoO 4 : Eu 3+ phosphors, but greatly influenced their morphology. CaMoO 4 : Eu 3+ red phosphors were prepared with 5wt% PEG20000 having small-sized and regularly spherical morphology, and there were greater improvement in the luminescent intensity than phosphors prepared with other surfactants.