Grazing Incidence Small-Angle X-ray Scattering (GISAXS) is a versatile technique for the analysis of nano and micro thin films surfaces. The scattering data depend strongly on the form and distribution of the scattering objects. In the present work GISAXS is used to study hafnium dioxide (HfO2) thin films deposited by magnetron sputtering using different deposition processes and post-deposition annealing conditions. Two distinct types of 15 nm thick samples were produced using different sputtering targets and different gas mixtures. The GISAXS results show that the ellipsoids that compose the thin films present a reduction in their size for both samples sets. For the sputtered Hf metal target samples, the ellipsoid diameter value shifted from 9 nm (as-deposited) to 6 nm following a 800 °C thermal treatment. For the sputtered HfO2 target samples the diameter value shifts from 19 nm (as-deposited) to 3 nm after a 800 °C anneal in oxygen. The size distribution, for both sets of samples, follows a Gaussian distribution function.