The synthesis of zinc ferrite spinel: Determination of pH value in the co-precipitation step

Abstract

Zinc ferrite (ZnFe2O4) nanomaterial can be facilely and conveniently synthesized via the co-precipitation method from aqueous Zn2+ and Fe3+ salt solutions using sodium hydroxide as the precipitant. However, zinc hydroxide is amphoteric and can be soluble at low and high pH values; therefore, the study on pH for simultaneous precipitation of Fe3+ and Zn2+ to achieve pure ZnFe2O4 spinel is essential. In the present study, we elaborate a theoretical equation expressing the relationship between the zinc concentration in complex formation and pH value in the co-precipitation step. Since then, we synthesized ZnFe2O4 spinel and analyzed the products via various techniques such as thermoanalysis (TG-DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV-Vis spectra to investigate the appropriate pH for simultaneous precipitation of Fe3+ and Zn2+. The results indicate that in a wide range of pH values, from 7 to 12, ZnFe2O4 single-phase spinel ferrite structure is formed after calcination of the precipitate at 800 degrees C, the average particle sizes (SEM, nm) of ZnFe2O4 samples are in the range of 59.5 nm-85.5 nm (but is non-linear change), and their bandgap values are similar, around 1.96 eV. However, the unwanted appearance of alpha-Fe2O3 phase, the shifting in peak position and the decrease in intensity in the XRD pattern of the spinel products synthesized at pH of 6 and 13, respectively, reflect that the stoichiometric ratio of Zn2+ to Fe3+ in the spinel products is not achieved to 1:2. Such results provide a fundamental basis for choosing the appropriate pH in synthesizing ZnFe2O4 nanoparticles with orientationally structural and optical characteristics.