Properties of highly crystalline NiO and Ni nanoparticles prepared by high-temperature oxidation and reduction

We describe here the use of high-temperature oxidation and reduction to produce highly crystalline nanoparticles of Ni and NiO. Starting with an amorphous Ni powder, we demonstrate that oxidation at 900 C produces faceted NiO nanocrystals with sizes ranging from 20 to 60 nm. High-resolution transmission electron microscopy measurements indicate near-perfect atomic order, truncated by (200) surfaces. Magnetization measurements reveal that the Neel temperature of these NiO nanoparticles is 480 K, substantially reduced by finite-size effects from the bulk value of 523 K. The magnetization of these faceted NiO nanoparticles does not saturate in fields as large as 14 T while a loop offset is observed which increases from 1000 Oe at 300 K to its maximum value of 3500 Oe at 50 K. We have used high-temperature reduction to transform the faceted NiO nanoparticles into highly ordered Ni nanoparticles, with a Curie temperature of 720 K and blocking temperatures in excess of 350 K. Subsequent efforts to reoxidize these Ni nanoparticles into the core-shell morphology found that the Ni nanoparticles are much more resistant to oxidation than the original Ni powder, perhaps due to the relative crystalline perfection of the former. At 800 C, an unusual surface roughening and subsequent instability was observed, where 50-nm-diameter NiO rods grow from the Ni surfaces. We have demonstrated that high-temperature oxidation and reduction in Ni and NiO are both reversible to some extent and are highly effective for creating the highly crystalline nanomaterials required for applications such as exchange-bias devices.