Formation and structural characterization of Ni nanoparticles embedded in SiO₂

Face-centered cubic Ni nanoparticles were formed in SiO₂ by ion implantation and thermal annealing. Small-angle x-ray scattering in conjunction with transmission electron microscopy was used to determine the nanoparticle size as a function of annealing temperature, whereas the local atomic structure was measured with x-ray absorption spectroscopy. The influence of finite-size effects on the nanoparticle structural properties was readily apparent and included a decrease in coordination number and bond length and an increase in structural disorder for decreasing nanoparticle size. Such results are consistent with the non-negligible surface-to-volume ratio characteristic of nanoparticles. In addition, temperature-dependent x-ray absorption spectroscopy measurements showed the mean vibrational frequency (as obtained from the Einstein temperature) decreased with decreasing nanoparticle size. This reduction was attributed to the greater influence of the loosely bound, under-coordinated surface atoms prevailing over the effects of capillary pressure, the former enhancing the low frequency modes of the vibrational density of states.