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NiS 2 hollow spheres with controllable size have been synthesized by a facile hydrothermal method through the exchanging reaction between rod-like supramolecular precursor and l -cysteine. Through modifying the diameter of rod-like precursor as template, accompanied by concomitant Rayleigh instability and chemical nonequilibrium interdiffusion, the size of NiS 2 hollow sphere can be tuned ranging from nanosize to microsize. The hollow morphology of as-obtained product was attributed to the Kirkendall effect involving different transport rates for Ni and S ions. Owing to the relatively large specific area, the as-obtained nanoscale NiS 2 hollow sphere manifest remarkable photo co-catalytic performance for H 2 production, which generate 5.8 mmol of H 2 gas under the irradiation of visible light after 6 h and 0.97 mmol/h of average H 2 production rate, indicating superior H 2 production performance of NiS 2 hollow spheres. [ABSTRACT FROM AUTHOR]