Dinickel phosphide (Ni2P), an efficient electrocatalyst
derived from commonly available elements, shows a noteworthy performance
in the hydrogen evolution reaction (HER). This research includes an
extensive analysis using diverse characterization techniques, including
scanning electron microscopy, transmission electron microscopy, energy
dispersive spectrometry, X-ray diffraction, X-ray absorption spectroscopy
(XAS), electron paramagnetic resonance (EPR), and in situ Raman spectroscopy,
revealing the structural change of Ni2P particles under
a 100 or 400 mV overpotential during HER. Employing methods like Fourier
transform infrared, in situ Raman spectroscopy, EPR, and XAS, the
study uncovers structural and chemical changes. These include the
emergence of nickel species, alterations in oxidation states, and
the indication of Ni–O bond formation. Additionally, considerable
morphological alterations in the particles are noted. These insights
contribute to a deeper understanding of Ni2P’s behavior
and properties in HER conditions, shedding light on its catalytic
efficiency and stability.