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采用微乳液‐水热法合成一系列NaLa（MoO4）2∶Eu3＋／Tb3＋／Tm3＋单／共掺的荧光粉（NLM ）。采用X射线衍射（XRD）、扫描电子显微镜（SEM ）、荧光光谱对荧光粉的晶体结构、形貌特征和发光性质进行了测试和研究。结果表明：所制备的样品均为四方晶系单晶，Eu3＋，Tb3＋，Tm3＋均以取代的方式进入La3＋的格位；样品的形貌为四方片状结构，颗粒尺寸1～1.5μm ；当Eu3＋掺杂浓度为是9％时，NLM ∶9％ Eu3＋荧光粉在616 nm发射峰是最强的，此时在NLM基质中Eu3＋之间的临界传递距离（Rc）约为15.20?。在NLM∶9％ Eu3＋的发射光谱中，591 nm处的发射峰为Eu3＋的5 D0→7 F1的磁偶极跃迁；616 nm处的发射峰为Eu3＋的5 D0→7 F2的电偶极跃迁，电偶极跃迁发射强度约是磁偶极跃迁强度的10倍，表明Eu3＋位于无反演对称中心格位。采用固定Eu3＋（T b3＋）的浓度，改变T b3＋（Eu3＋）浓度的方法，研究了Eu3＋与T b3＋之间的能量传递机理。通过调节Eu3＋，T b3＋和T m3＋的掺杂浓度，实现在单一基质条件下可见光区域的光色调节，在360 nm激发下NLM ∶ x％ Eu3＋，y％ Tb3＋，z％ Tm3＋荧光粉的发光由蓝光（0.205，0.135）调到伪白光（0.305，0.266）。“,”A series of Eu3+ /Tb3+ /Tm3+ single/co‐doped NaLa(MoO4 )2 (NLM ) phosphors have been synthesized by microemul‐sion‐hydrothermal method .Phosphor crystal structure ,morphology and luminescent properties were tested and studied by X‐ray diffraction (XRD) ,scanning electron microscopy (SEM ) and fluorescence spectroscopy .The results show that the prepared samples are all tetragonal single crystals .By way of substitution ,the sites of La3+ are replaced by Eu3+ ,Tb3+ and Tm3+ .Mor‐phology of the samples are tetragonal sheet structure and the size of particles is 1~1.5 μm .When the doping concentration of Eu3+ is 9% ,NLM ∶9% Eu3+ phosphor emission peak is the strongest at 616 nm ,the critical transfer distance (Rc ) between Eu3+ in the NLM matrix is about 15.20 ? at this time .At the emission spectrum of NLM∶9% Eu3+ ,the peak at 591 nm is the magnetic dipole transition of 5 D0 to 7F1 of Eu3+ .The peak at 616 nm is the electric dipole transition of 5 D0 to 7 F2 of Eu3+ . Electric dipole transition emission intensity is about 10 times of the strength of the magnetic dipole transition .This indicates that Eu3+ is located at noninversion symmetry site .By Fixing Eu3+ (Tb3+ ) concentration and varying the concentration of Tb3+(Eu3+ ) ,the energy transfer mechanism between Eu3+ and Tb3+ was studied .By adjusting the Eu3+ ,Tb3+ and Tm3+ doping concentrations ,tunable luminescence of visible light region is implemented under the single matrix .The luminescence of NLM∶x% Eu3+ ,y% Tb3+ ,z% Tm3+ phosphors are translated from blue (0.205 ,0.135) to pseudo‐white (0.305 ,0.266) under 360 nm irradiation .