The invention relates to CuCo2S4 active substance diluent for a super-capacitor and a preparation method thereof. The preparation method comprises the following steps: putting copper source and cobalt source into glycerol in the active substance synthesis process, fast stirring, adding the sulfur source dissolved by using deionized water after the copper source and the cobalt source are completely dissolved, transferring to a high-voltage reaction kettle to perform the solve thermal reaction after the sufficient stirring; pouring out the mixed solution containing nanocrystal after the reaction is finished, diluting and centrifuging through the deionized water, drying to obtain the active substance-CuCo2S4 nanocrystal; and putting the CuCo2S4 nanocrystal into an ethanol solvent, taking the polyvinylpyrrolidone as the dispersing agent, namely acquiring the active substance diluent. The method disclosed by the invention has the advantages that the defect of the prior art can be overcome, the active substance with high specific ratio capacitance activity, high dispersity, good stability and easy industrial manufacturing for the super-capacitor can be acquired.