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We demonstrate in this paper facile synthesis of CoS₂ and NiS₂ hollow spheres with various interiors through a solution‐based route. The obtained CoS₂ microspheres constructed by nanosheets display a three‐dimensional architecture with solid, yolk‐shell, double‐shell, and hollow interiors respectively, with continuous changes in specific surface areas and pore‐size distributions. Especially, the CoS₂ hollow spheres demonstrate excellent supercapacitive performance including high specific capacitance, good charge/discharge stability and long‐term cycling life, owing to the greatly improved faradaic redox reaction and mass transfer. Furthermore, CoS₂ hollow spheres exhibit superior electrocatalytic activity for disulfide/thiolate (T₂/T⁻) redox electrolyte in dye‐sensitized solar cells (DSCs). Therefore, this work provides a promising approach for the design and synthesis of structure tunable materials with largely …