Annealing and Ni content effects on EPR and structural properties of Zn_1–xNi_xO aerogel nanoparticles

Zn_1-xNi_xO aerogel nanopowders with nickel concentration in the range of 0.05 ≤ x ≤ 0.25, were synthesized by the sol-gel processing technique and post-annealed in air at 500 °C. Structural, vibrational, thermal and magnetic properties of the as-prepared and annealed Zn_1-xNi_xO powdered samples were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman scattering, thermal gravimetric analysis (TGA) and electron paramagnetic resonance (EPR) spectroscopy. In addition to the ZnNiO phase, XRD analysis revealed the formation of a secondary NiO phase when the Ni content was greater than or equal to 10 %. The TEM images confirm that the particle size is in the range of 20 nm to 40 nm, in accordance with XRD results, and the particles are well dispersed. Raman scattering measurements confirm the wurtzite structure of the synthesized Zn_1-xNi_xO nanopowders and show that intrinsic host-lattice defects are activated when Ni²⁺ ions are substituted to the Zn sites. Room temperature ferromagnetic order was observed in all of the samples and was strongly dependent on the Ni content and thermal annealing. These results indicate that the observed room temperature ferromagnetism in ZnNiO may be attributed to the substitutional incorporation of Ni at Zn sites.