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The structural evolution of the nanocrystalline material obtained from the amorphous compound Fe73.5CuNb3Si13.5B9 was investigated by small-angle X-ray scattering. Four sets of amorphous metallic ribbons were produced by melt spinning using different quenching rates. Samples of each set were annealed above the crystallization temperature; X-ray diffraction analysis showed the formation of an ordered Fe-Si solid solution with average grain sizes ranging from 9 to 11 nm. Small-angle scattering curves of the samples in the initial amorphous states revealed different intensities for different quenching rates, caused by the presence of heterogeneities with dimensions larger than those of the crystallites formed after thermal treatment. In addition, scattering measurements carried out in situ during isothermal annealing showed an intensity evolution as a function of time, attributed to electron-density contrast variation caused by the atomic diffusion process that occurs during crystallization.