The mechanisms involved in shape changes arising during sintering of complex materials like iron-based systems are still poorly understood. New information can be obtained by use of advanced techniques such as microtomography. In this study, the microstructural evolution of a Distaloy AE powder compact and of loose copper powder is investigated during a thermal cycle at the European Synchrotron in Grenoble (France). Both materials are sintered in a furnace set in front of a high-energy X-ray source in 30–45 keV range. At various steps of sintering, hundreds of radiographs are taken with different orientations of the specimen. From these images the 3D microstructure is reconstructed. This non-destructive method provides the 3D microstructural evolution of the material during sintering. Local and statistical information can be obtained and will be used in the future for modelling the sintering process. Special attention is given to the anisotropy induced by prior compaction and to its evolution through sintering.