The invention provides a liquid phase synthesis method of an ultra-thin molybdenum diselenide nanosheet, which comprises the following steps of: mixing a molybdenum source, a selenium source and organic amine, and removing impurities to obtain a mixed solution; reacting the mixed solution at 240-300 DEG C for 20-60min to obtain an ultra-thin molybdenum diselenide nanosheet; wherein the molybdenumsource is selected from one or more of ammonium molybdate, sodium molybdate, ammonium phosphomolybdate, molybdenum trioxide, oxymolybdenum acetylacetonate and molybdenum acetate; the selenium source is selected from one or more of selenium powder, selenium methionine and dibenzyl diselenium. According to the invention, a precursor source (a molybdenum source and a selenium source) of a specific kind and an organic amine solvent are selected to promote spreading to form an ultra-thin molybdenum diselenide nanosheet with a large area and an uniform and smooth appearance; the raw materials are common raw materials, the conditions are mild, and the method is simple; the method has short preparation period and high yield. The nanosheet has a single-layer or several-layer morphology. That the molybdenum diselenide is a coexistent phase of 1T phase and 2H phase, which can be seen from a photoelectron spectrogram and a high-angle annular dark field image and is beneficial to the improvement ofthe conductivity.