The invention discloses a preparation method of a Fe5Ni4S8
hydrogen evolution electro-catalytic material. The method comprises the following specific steps: weighing nano
iron powder, nano
nickel powder and
sulfur powder; adding absolute ethyl
alcohol and
grinding; uniformly putting the mixture into a
mortar and transferring the
mortar into a tubular furnace; sealing the pipeline, introducing
nitrogen, cleaning the
quartz tube for 20 minutes, performing heating to 700 DEG C at a heating rate of 5 DEG C / min, keeping the temperature for 3 hours, performing heating to 1100 DEG C at the same heating rate, keeping the temperature for 10 hours, performing annealing to
room temperature, taking out the mixture, uniformly
grinding the obtained sample, adding
ethanol, and carrying out ball milling for 10 hours by using a planetary
ball mill. According to the method, vacuum cladding operation is replaced by
nitrogen atmosphere calcination; a
quartz ampoule tube and a vacuum sealing
machine whichare required by vacuum cladding are not required; and meanwhile, the experiment risk possibly caused by high
sulfur pressure is also avoided due to the circulating gas
atmosphere, the microcosmic sizeof the sample reaches the nanometer level due to the added ball milling operation after
calcination, the active sites on the surface of the sample are increased, and the electro-catalytic
hydrogen evolution performance is improved.