We investigated the structural evolution of electrochemically fabricated Pd nanowiresin situby means of grazing-incidence transmission small- and wide-angle x-ray scattering (GTSAXS and GTWAXS), x-ray fluorescence (XRF) and two-dimensional surface optical reflectance (2D-SOR). This shows how electrodeposition and the hydrogen evolution reaction (HER) compete and interact during Pd electrodepositon. During the bottom-up growth of the nanowires, we show thatβ-phase Pd hydride is formed. Suspending the electrodeposition then leads to a phase transition fromβ-phase Pd hydride toα-phase Pd. Additionally, we find that grain coalescence later hinders the incorporation of hydrogen in the Pd unit cell. GTSAXS and 2D-SOR provide complementary information on the volume fraction of the pores occupied by Pd, while XRF was used to monitor the amount of Pd electrodeposited.
Keywords: electrodeposition; hydrogen; nano-porous anodic alumina; nanowires; palladium; synchrotron; x-ray scattering.
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