Zn 2 GeO 4 :Mn 2þ nanophosphors are synthesized from germanium(IV) oxide and acetates of zinc and manganese(II) in a mixed solvent of water and diethylene glycol (DEG) by the solvothermal reaction at 200 °C for 2 h. Phase pure Zn 2 GeO 4 :Mn 2þ is obtained for the samples prepared at 0 e x DEG e 91.7, where x DEG is the volume percentage of DEG in the mixed solvent. The particle and crystallite sizes decrease with the increase in x DEG . The sample prepared at x DEG = 91.7 comprises the nanorods with 30.2 and 12.2 nm in mean length and width, respectively. The actual Mn concentration measured by X-ray fluorescence analysis increases with the increase in x DEG and approaches to the nominal concentration, 2.0 at %. The samples show green luminescence corresponding to the d-d transition of Mn 2þ under the irradiation of UV and near-UV light. The photoluminescence intensity reaches a maximum around x DEG ∼ 80. This is attributed to the competitive factors, the Mn concentration and the sizes of crystallites and particles.