The use of a membrane-based chip nanocalorimeter in a powder diffraction beamline is described. Simultaneous wide-angle X-ray scattering and scanning nanocalorimetric measurements are performed on a thin-film stack of palladium/amorphous silicon (Pd/a-Si) at heating rates from 0.1 to 10 K s⁻¹. The nanocalorimeter works under a power-compensation scheme previously developed by the authors. Kinetic and structural information of the consumed and created phases can be obtained from the combined techniques. The formation of Pd₂Si produces a broad calorimetric peak that contains overlapping individual processes. It is shown that Pd consumption precedes the formation of the crystalline Pd₂Si phase and that the crystallite size depends on the heating rate of the experiment.