The present study is concerned with the nanocasting preparation of Co3O4 nanostructures employing two-dimensional (2D) hexagonal SBA-15 and three-dimensional (3D) cubic KIT-6 as hard templates. The influence of framework connectivity of the parent silica and loading of the cobalt source are studied in detail. Structures can be tailored as isolated or randomly organized Co3O4 nanowires or as highly ordered mesoporous Co3O4 networks retaining the symmetry of the silica parent using 2D hexagonal parent materials. Applying cubic KIT-6 silica with suitable wall thickness and degree of framework interconnectivity as a template, we can vary the pore size of mesostructured Co3O4 from 3 nm up to values as high as 10 nm. To verify the influence of surface properties and texture, we employed different mesoporous silicas that were conventionally calcined at 550 °C and equivalent silica materials microwave treated in the presence of a concentrated H2O2/HNO3 mixture. The parent silica materials and the resulting Co3O4 were characterized in detail at different steps during the templating route by nitrogen physisorption measurements and powder X-ray diffraction. Transmission electron microscopy and scanning electron microscopy investigations were performed to visualize the structure and morphology of the nanocast materials, and thermogravimetry−differential thermal analyses (TG−DTA) were done to follow the formation of Co3O4. With our method, preparation of nanocast Co3O4 is highly reproducible, regardless of template shapes and sizes, which makes the pathway much more versatile for a great variety of templates.

Antiferromagnetic Co3O4 nanowires with an average diameter of about 8 nm have been synthesized by using the nanocasting route. The nanowires were characterized by powder X-ray diffraction, transmission electron microscopy, and a superconducting quantum interference device magnetometer. The magnetic measurements show a unidirectional exchange anisotropy accompanied by an enhancement of the field-cooled coercivity at low temperature. These effects suggest the presence of an exchange interaction between the antiferromagnetic core and the surface spins. A strong dependence of the exchange field on the magnitude of the cooling field and a training effect have been observed. The dependence of exchange bias field on temperature reveals the important role played by the antiferromagnetic core in the exchange coupling.