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We report magnetic and exchange bias studies on Ni-NiO nanoparticulate systems synthesized by a two-step process, namely, chemical reduction of a Ni salt followed by air annealing of the dried precipitate in the temperature range 400-550 °C. Size of Ni and NiO crystallites as estimated from X-ray diffraction line broadening ranges between 10.5-13.5 nm and 2.3-4 nm, respectively. The magneto-thermal plots (M-T) of these bi-magnetic samples show a well developed peak in the vicinity of 130K. This has been identified as the superparamagnetic blocking temperature "TB" of NiO. Interestingly, all samples exhibit exchange bias even above their respective NiO blocking temperatures, right up to 300K, the maximum temperature of measurement. This is in contrast to previous reports since exchange bias requires the antiferromagnetic NiO to have a stable direction of its moment in order to pin the ferromagnet (Ni) magnetization, whereas such stability is unlikely above TB since the NiO is superparamagnetic, its moment flipping under thermal activation. Our observation is elucidated by taking into account the core-shell morphology of the Ni-NiO nanoparticles whereby clustering of some of these nanoparticles connects their NiO shells to form extended continuous regions of NiO, which because of their large size remain blocked at T > TB, with thermally stable spins capable of pinning the Ni cores and giving rise to exchange bias. The investigated samples may thus be envisaged as being constituted of both isolated core-shell Ni-NiO nanoparticles as well as clustered ones, with TB denoting the blocking temperature of the NiO shell of the isolated particles. [ABSTRACT FROM AUTHOR]

Porous films of Co/CoO magnetic nanoparticles have been obtained by inert gas condensation and partially oxidized in situ in the deposition chamber. These nanoparticle films were subjected to thermal treatments in high vacuum and the chemical and structural changes monitored by x-ray diffraction, transmission electron microscopy, transport and magnetic measurements (with a focus on the exchange-bias phenomenon), which evidence that for vacuum annealing temperatures above 360 °C, most of the CoO phase is reduced to metallic Co without requiring the presence of an external reducing agent (e.g., H2) or a plasma. Additionally, there is a certain degree of particle coalescence resulting in the formation of greater nanoparticles as the annealing temperature increases. This yields a smaller proportion of CoO compared to metallic Co and a reduction of the Co/CoO interface density, pinpointed by a drastic decrease of the exchange-bias field. The crucial roles of the vacuum level and the surface-to-volume ratio are evidenced by magnetic measurements, highlighting the potential of magnetometry as a probe for the reduction/oxidation of composite nanostructures. [ABSTRACT FROM AUTHOR]