Preparation of nanosized iron oxide and its application in low temperature CO oxidation

Abstract

A method to prepare iron oxide material which has a higher surface area and nanosized particle was developed. It was used as a catalyst for CO oxidation at low temperature. Iron oxide materials were prepared by precipitation under constant pH value. The effects of preparation parameters, such as iron salt (FeCl3, Fe(NO3)3 and FeCl2), pH value (between 8 and 12), drying temperature (between 120°C and 300°C), and feeding rate of the aqueous solution of the iron salt, on the characteristics of iron oxide have been investigated. The materials were characterized by N2 sorption, powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The surface area of iron oxide was greater than 400 m2/g using FeCl3 as the starting material with very low feeding rate of 10 ml/min, the pH value of 11, and drying at 120°C. The XRD patterns indicated that the iron oxide samples heated at a temperature below 180°C was either amorphous or of a particle size too small (<4 nm) for the samples prepared with FeCl3. Depending on the preparation conditions, the iron oxide samples showed a phase transition from amorphous to various crystalline phases. Large amount of hydroxyl groups were preserved if the drying temperature was below 200°C. TEM images showed that the particle diameters were less than 4 nm for the samples prepared with FeCl3 at pH value of 11 with a low feeding rate of 10 ml/min, and heated below 200°C. XPS Fe 2p3/2 spectra showed the phase transition of iron oxide from Fe3O4 to FeO. The feeding rate of starting material and pH value during precipitation played the important roles to obtain iron oxide with high surface area. The nanosized iron oxide demonstrated high activity for CO oxidation even at ambient condition. The higher activity of Fe x O y nanoparticles in CO oxidation was attributed to a small particle size, high surface area, high concentration of hydroxyl groups, and more densely populated surface coordination unsaturated sites.