The invention relates to research of a novel composite tungsten molybdenate phosphor, and especially relates to a novel fluorescent microcrystal prepared by a chemical solution method. The microcrystal provided by the invention can be expressed by a general formula of Na4-3xEux(WO4)2-y(MoO4)y, wherein 0<x<4/3 and 0<y<2. The preparation method comprises the following steps: according to a molar ratio of raw materials required for the preparation of a certain amount of Na4-3xEux(WO4)2-y(MoO4)y, measuring corresponding volumes of Na2MoO4 and Na2WO4 solutions in a polytetrafluoroethylene beaker, respectively adding a corresponding amount of EuCl3 solution, stirring at normal temperature for 15-30 min, adjusting the pH to 6-9, and finally putting the polytetrafluoroethylene beaker into a high pressure reaction vessel; performing a hydrothermal reaction at 80-160 DEG C for 15-30 hours, naturally cooling to room temperature; centrifuging the precipitates for separation, washing with deionized water, and drying at 100-150 DEG C to obtain the Na4-3xEux(WO4)2-y(MoO4)y microcrystal. The preparation method of the invention is simple in preparation process, low in reaction temperature. The prepared tungsten molybdenate fluorescent microcrystal is pure in phase, uniform in granularity, appropriate in particle size, and regular in morphology, can exhibit red light with high purity and brightness, and has good practicality.