<p>In the present study, we extensively studied the phonon and magnon excitations in nickel oxide (NiO) and Ni/NiO hybrid nanostructures using Raman scattering analyses. The NiO nanostructures were synthesized by facile hydrothermal route and annealed under air and argon (Ar) atmosphere at 800°C. Interestingly, Ar annealed NiO nanostructure shows fine sized particles and the formation of Ni/NiO hybrid. The morphological, structural and phonon vibrational modes of the synthesized nanostructures were investigated by transmission electron microscopy (TEM), grazing incident X-ray diffraction (GIXRD), and Raman scattering techniques. The TEM and GIXRD measurements confirm the formation of face centered cubic phase in NiO and Ni/NiO nanostructures. The surface optical phonon mode is observed in both NiO and Ni/NiO hybrid nanostructure and its theoretical peak positions are estimated using dielectric continuum model. Magnon modes do not appear in Ni/NiO nanostructure, which could be correlated to the reduction in the spin correlated length and super exchange interactions due to the symmetry breaking in the next nearest neighbor of Ni²⁺ ions in the linear atomic chain, Ni²⁺–O²⁻–Ni²⁺ of the crystal lattice.</p>