The invention provides a preparation method for a bismuth/montmorillonite photoluminescence material. The preparation method comprises the steps as follows: taking bismuth nitrate pentahydrate and na-montmorillonite as raw materials; dissolving; uniformly mixing; separating out deposit; drying the deposit; grinding into powder; placing the powder into a small crucible; placing the small crucible into a big crucible; sprinkling carbon powder around the big crucible; and finally baking to 400-1300 DEG C in a muffle furnace, insulating for 1-5 min and carrying out furnace cooling, wherein the bismuth nitrate pentahydrate and the na-montmorillonite are weighed according to the mass ratio of 4 to 1. The feature that positive ions are easily adsorbed by negative electricity between the layers of the montmorillonite is utilized in the preparation method. The preparation method further comprises the steps as follows: introducing trivalent bismuth ions between the layers of the montmorillonite in a solution; washing for multiple times to remove bismuth ions absorbed on the surface of the montmorillonite; and drying a sample, placing into a semi-reducing atmosphere created by the carbon powder, and calcining to prepare the bismuth/montmorillonite photoluminescence material.