The invention relates to a preparation method of a chemical solution of terbium-doped tungsten molybdate green fluorescent microcrystalline. The green microcrystalline provided by the invention can be expressed by a general formula A0.925(WO4)0.5(MoO4)0.5:Tb3+0.05, wherein A=Ca, Sr and Ba. The preparation method comprises the following steps of: preparing the molar ratio of various raw materials required by a certain amount of target system, A0.925(WO4)0.5(MoO4)0.5:Tb3+0.05 microcrystalline, weighing a certain consistency and relative volume of A(NO3)2, TbCl3 solutions in a polytertrafluoroethylene beaker, respectively adding the relative amounts of Na2MoO4 and Na2WO4 solutions, stirring at the room temperature for 15-30min, and putting the polytertrafluoroethylene beaker into a high-pressure reaction kettle; naturally cooling down to the room temperature after carrying out a hydrothermal reaction under 80-180 DEG C for 15-30h; and centrifugalizing and cleaning in deionized water sediments, and baking the sediments under 100-150 DEG C to obtain the A0.925(WO4)0.5(MoO4)0.5:Tb3+0.05 solid solution luminescent microcrystalline. The invention has the advantages of environment protection, energy conservation, simple preparation processes and devices and low reaction temperature. The terbium-doped tungsten molybdate green fluorescent microcrystalline prepared by the preparation method disclosed by the invention has the advantages of pure phase, uniform granularity, suitable grain size, regular appearance, highly pure and bright green and excellent practicability.