The growth of precipitates in a deformed Cu–Ni–Si alloy with an aging treatment and the rearrangement of dislocations were investigated using small-angle X-ray scattering method and XRD line-profile analysis. The small-angle X-ray scattering method was used for characterizing the growth behavior of the precipitates. The results showed that the precipitates grew gradually to a few nanometers in radius when aged under the condition that the alloy exhibited a maximum of the hardness due to precipitation hardening. The growth rate rose from the onset of the overaging, where the hardness started to decrease. The line-profile analysis of copper-based alloy diffraction peaks using modified Williamson–Hall and modified Warren–Averbach procedures yielded a variation in the dislocation densities of the alloy as a function of the aging time. The dislocation density of the alloy before the aging treatment was estimated to be 1.7×1015 m−2 and its high value was held up to the peak-aging time. With the onset of the overaging, however, the dislocation density distinctly decreased by about 1 order of magnitude indicating that a large amount of the dislocations rearranged to release the alloy from the high dislocation-density state. The results suggest that the massive rearrangement of dislocations was accompanied with coarsening of the precipitates.