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Crystallite size effect in the selective oxidation of butene to butadiene on iron oxide. 1. Moessbauer, X-ray, and magnetization characterization of the catalysts

Journal Article · · J. Phys. Chem.; (United States)
DOI:https://doi.org/10.1021/j150656a019· OSTI ID:5827374
A series of silica-supported and unsupported iron oxide catalysts were characterized by X-ray diffraction, room-temperature Moessbauer spectroscopy, and low-temperature magnetization measurements. The average crystallite sizes were determined by the X-ray line-broadening technique. They ranged from 2.5 to 9.5 nm for the supported samples and from 14.5 to 61 nm for the unsupported samples. X-ray diffraction detected only the presence of ..cap alpha..-Fe/sub 2/O/sub 3/. Fourier line-shape analyses showed that the samples were rather strain free, and the width of the crystallite size distribution increased with increasing average crystallite size. The Moessbauer parameters of both components are consistent with the assignment of ..cap alpha..-Fe/sub 2/O/sub 3/. In particular, no component with zero quadrupole splitting assignable to ..gamma..-Fe/sub 2/O/sub 3/ was observed. Magnetization measurements showed that the small crystallite samples possess magnetic moments higher than that of bulk ..cap alpha..-Fe/sub 2/O/sub 3/ but much lower than that of ..gamma..-Fe/sub 2/O/sub 3/. The data was explained by the absence of Morin transition and incomplete cancellation of spins in very small crystallites of ..cap alpha..-Fe/sub 2/O/sub 3/. 29 references, 6 figures, 3 tables.
Research Organization:
Northwestern Univ., Evanston, IL
OSTI ID:
5827374
Journal Information:
J. Phys. Chem.; (United States), Journal Name: J. Phys. Chem.; (United States) Vol. 88:12; ISSN JPCHA
Country of Publication:
United States
Language:
English