LAUSR

Bismuth ferrite (BiFeO3) is a promising Bi-based perovskite-type material, which is multiferroic due to the coexistence of anti-ferromagnetism and ferroelectricity. During the preparation of pure BiFeO3 nanoparticles, however, the phase structures and species of bismuth–iron-based precursor (BFOH) were still unclear, and so related precursors were prepared. X-ray diffraction, Raman, Fourier transform infrared, and X-ray absorption near-edge structure techniques were used to probe the phase structure and species of the precursors. It was found that the precursor BFOH is composed of Bi6O6(NO3)4(OH)2·2H2O, Bi6O5(NO3)5(OH)3·3H2O, Fe(OH)3, and α-Bi2O3. Calcination treatment and hydrothermal synthesis were used to prepare the pure BiFeO3 phase from the precursor BFOH. The calcination temperature was optimized as 400 °C for preparation of the pure BiFeO3 phase. Meanwhile, hydrothermal conditions for the synthesis of the pure BiFeO3 phase were also optimized as follows: the reaction solution was the mixture solution of Bi(NO3)3·5H2O and Fe(NO3)3·9H2O with cetyltrimethyl ammonium bromide (CTAB) as the surfactant and KOH as the mineralizer; the hydrothermal synthesis was performed at 180 °C for 48 h; the concentration of KOH should be at least 3 M; and the surfactant CTAB can be used to regulate the morphology of the as-prepared BiFeO3 nanoparticles. From the point of view of the microstructure, BiFeO3 nanoparticles prepared by calcination or hydrothermal methods have no notable differences. A formation mechanism from the precursor BFOH to the BiFeO3 product is proposed. By providing an understanding of the precursors, this work is very helpful in the synthesis of bismuth–iron-based nanoparticles.