In this paper, for the first time a simple batch process was utilized for the facile synthesis of cubic FeS(2) and flower-like FeSe(2). By adjusting the amount of solvents and surfactants added, pure pyrite FeS(2) with a defined crystalline structure was obtained. It was found that the reaction temperatures and iron sources had significant influence on the purities and morphologies of FeS(2) and FeSe(2) particles. Raman spectra of the FeS(2) and FeSe(2) samples presented characteristic peaks of S-S and Se-Se active modes at 337, 372 cm(-1), and 180, 217, 254 cm(-1), respectively. The absorption properties of the FeS(2) and FeSe(2) samples were also investigated and the results demonstrated that these samples had broad optical absorption in NIR. Moreover, the synthetic approach demonstrated here may be of great potential for the controlled synthesis of other metal chalcogenides.