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This invention discloses a mica nanosheet and its preparation method, belonging to the field of two-dimensional nanofiller technology. The preparation method disclosed in this invention involves heat-treating bulk mica, followed by purification in an aqueous nitric acid solution to obtain pretreated mica powder; dispersing the pretreated mica powder in a solvent to obtain a mixed slurry; adding an oxidant to the mixed slurry and stirring the mixture, then adding a small-molecule lithium salt to further react, obtaining a pretreated slurry; adding grinding beads to the pretreated slurry for sand milling to achieve exfoliation; subsequently releasing the exfoliated slurry and performing post-processing to obtain mica nanosheets. This method solves the technical problem of simultaneously achieving efficient, green, and controllable exfoliation, and possesses scalability potential, which is difficult to achieve with existing methods.