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Ordered arrays of Pd nanowires electrochemically grown in nano-porous alumina represent a promising framework for hydrogen storage applications with controlled hydrogen absorption/release dynamics, as well as for sensing devices with high scalability. We investigated the structural evolution of such nanowires in situ by means of grazing-incidence transmission small- and wide-angle x-ray scattering (GTSAXS and GTWAXS), x-ray fluorescence (XRF) and 2-dimensional surface optical reflectance (2D-SOR). This shows how electrodeposition and the hydrogen evolution reaction (HER) compete and interact during Pd electrodepositon.