Characterization and effect of calcination temperature on structural properties of spinel zinc aluminate synthesized via Co-precipitation process

Zinc aluminate (ZnAl2O4) nanopowders were synthesized by co-precipitation method using zinc chloride and aluminum chloride as starting precursors. The calcination temperature which was a crucial preparation factor was varied and its influence on relevant physical properties of the product was investigated. Structural properties of synthesized nanoparticles were investigated by X-ray diffraction, X-ray absorption spectroscopy, scanning electron microscope, and Raman spectroscopy. The results suggest that that ZnAl2O4 in spinel structure with high crystallinity can be obtained after calcination beyond specific temperature affirmed by XRD results. Raman result indicates the correlated chemical bonding relating to the formation of ZnAl2O4 structure. Meanwhile, the Zn K-edge X-ray absorption near-edge structure (XANES) spectra of these samples with different calcination temperature obtained from the synchrotron X-ray absorption spectroscopy measurement show the existence of accurate oxidation state for zinc ion (Zn²⁺) in the spinel crystal structure. Moreover, it is revealed that the calcination temperature has significant effect on the local environment of the zinc absorbing atoms through the interesting change of white line appearance.