The invention discloses a preparation method of a ZIF-67-silver selenide nano composite material. The preparation method comprises the following steps: dissolving cobalt nitrate in a methanol solution, carrying out uniform ultrasonic dispersion to obtain a solution A, dissolving 2-methyl imidazole in the methanol solution, carrying out uniform ultrasonic dispersion to obtain a solution B; slowly dropwise adding the solution B into the solution A, standing, centrifuging, washing with methanol to obtain ZIF; weighing a proper amount of ZIF-67, dispersing ZIF-67 in 20 mL of water to obtain a solution a, weighing a proper amount of selenium powder, dissolving selenium powder in a hydrazine hydrate solution to obtain a solution b, adding the solutions a,b into a three-necked bottle, adding a magnet, putting the three-necked bottle in an oil bath, weighing a proper amount of silver nitrate, dissolving silver nitrate in water, adding the solution into the three-necked bottle, continuously reacting for 2 hours, centrifuging the obtained solution, and washing to obtain a finished product. The prepared nano composite ions are cubic, uniform in size, good in dispersity and low in toxicity, can show an efficient photo-thermal conversion performance under the irradiation of near-infrared light, and can be applied to the biomedical fields such as photo-thermal therapy of tumors. In addition,the method is simple in process, low in energy consumption, small in equipment number and convenient to popularize.