The invention belongs to the fields of nano / micron material preparation technology and hydro-thermal synthesis technology, and particularly relates to a method for preparing a nano-sheet assembled bismuthyl
bromide superstructure by adjusting and controlling a surfactant. The method comprises the following steps: using
bismuth nitrate,
sodium bromide or hexadecyl trimethyl
ammonium bromide as a reactant, adding PEG4000 or PVP4000 as an adjusting and controlling agent, using ethanediol as a
solvent, preparing a precursor solution under ultrasonic agitation, and moving the precursor solution into a hydro-
thermal reaction kettle in a packing ratio of between 60 and 80 percent; putting the hydro-
thermal reaction kettle filled with the mixture into a box-type resistance furnace, heating the kettle to a temperature of between 90 and 150 DEG C, keeping the temperature for 2 to 48 hours, taking the kettle out of the furnace, and cooling the kettle to the
room temperature naturally; and washing and centrifugally separating the mixture in the kettle to obtain the required product. The method has the advantages of simple process, easy construction of a whole preparation
system, simple and convenient operation, easily controlled condition, low cost, easily controlled product shape and size, high purity, good
crystallinity and convenient
processing of the product, and is suitable for large scale industrial production.