The invention relates to a preparation method of trimethylgallium. The method comprises steps as follows: (1) iodine and molten gallium have a contact reaction in the inert atmosphere, and gallium triiodide is obtained; (2) trimethylaluminium and the gallium triiodide have a contact reaction in the presence of an initiator and in the inert atmosphere. With the adoption of the preparation method, the yield and the purity of the trimethylgallium can be significantly increased, the yield of the trimethylgallium can be higher than 90%, the purity can be 99.9999%, besides, a reaction kettle used in the method can be used as an evaporation kettle, the technology and equipment are simplified, the reaction process is easy to control, the prepared product can be separated from raw materials and byproducts more easily, the method is very applicable to industrial production, in addition, the byproducts can be used for synthesizing aluminum sulfate, almost no waste is produced, use of a large amount of highly toxic products, namely, methyl iodide, can be avoided in the technology, and the method is very environment-friendly.