In situ hydride breathing during the template-assisted electrodeposition of Pd nanowires
Abstract
We investigated the structural evolution of electrochemically fabricated Pd 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. During the bottom-up growth of the nanowires, we show that β-phase Pd hydride is formed. Suspending the electrodeposition then leads to a phase transition from β- to α-phase Pd hydride. 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.
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