Synthesis of magnetic nickel spinel ferrite nanospheres by a reverse emulsion-assisted hydrothermal process

Nickel ferrite nanospheres were successfully synthesized by a reverse emulsion-assisted hydrothermal method. The reverse emulsion was composed of water, cetyltrimethyl ammonium bromide, polyoxyethylene(10)nonyl phenyl ether, iso-amyl alcohol and hexane. During the hydrothermal process, β-FeO(OH) and Ni0.75Fe0.25(CO3)0.125(OH)2·0.38H2O (INCHH) nanorods formed first and then transformed into nickel spinel ferrite nanospheres. The phase transformation mechanism is proposed based on the results of X-ray powder diffraction, transmission electron microscopy and energy-dispersive X-ray spectroscopy, etc. Nickel ferrite may form at the end of the INCHH nanorods or from the solution accompanied by the dissolution of β-FeO(OH) and INCHH nanorods. The X-ray photoelectron spectroscopy analysis shows that a few Fe3+ ions have been reduced to Fe2+ ions during the formation of nickel ferrite. The maximum magnetization of the nickel ferrite nanospheres obtained after hydrothermal reaction for 30 h is 55.01 emu/g, which is close to that of bulk NiFe2O4.