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Time-resolved in situ small angle X-ray scattering measurements were carried out to monitor the formation of nanoparticles of cadmium sulfide, from a solution containing the corresponding acetate and thioacetamide under solvothermal conditions. Analysis of the SAXS data shows that spherical cadmium sulfide particles of ca 105 Å in radius form within the first minutes of the reaction and then grow uniformly to form cylindrical nanoclusters over a period of a few hours, resulting in a highly monodispersed particles distribution.