“…The observed two significant peaks at 856.78 and 875.18 eV for Ni 2 P, 856.83 and 875.23 eV for Ni 2 P/Ni 12 P 5 , and at 856.63 and 875.03 eV for Ni 12 P 5 correspond to the spin–orbital splitting of Ni 2p 3/2 and Ni 2p 1/2 , respectively. The respective binding energies substantiate the existence of surface-oxidized nickel species in the Ni 2+ oxidation state. ,− Also, it is observed that the peaks obtained at 852.21, 852.90, and 852.35 eV in Ni 2p spectra of Ni 2 P, Ni 2 P/Ni 12 P 5 , and Ni 12 P 5 , respectively, are quite close to the elemental-zero valence state of nickel, which conveys the small positive charge (Ni δ+ ) of Ni species in the prepared samples. − The P 2p spectrum of Ni 2 P shows a prominent peak around 133.62 eV and a marginal hump at 129.20 eV, which can be attributed to the oxidized P species and metallic P, respectively, whereas the P 2p spectra show two prominent peaks around 129.77, 134.34 eV on behalf of Ni 2 P/Ni 12 P 5 and 129.82, 134.32 eV intended for Ni 12 P 5 , which could be assigned to P δ− in the form of metal phosphide and oxidized P species observed at the surface due to the partial passivation of phosphide particles. ,− The P 2p binding energy at ∼129.20 eV is less than that of elemental P (130.20 eV), which indicates that the P species in Ni 2 P has a minimal negative charge (P δ− , 0 < δ < 1). , These results suggest that there is an electron transfer from Ni to P in all three nickel phosphide phases. Because of the XPS studies taken for the aged Ni–P samples after a year, the conspicuous presence of oxidized Ni and P peaks have been attributed to the surface oxidation of the sample.…”