Abstract

A new method for analyzing the cation distribution of spinel crystals by extended X‐ray absorption fine‐structure spectroscopy has been developed to overcome the disadvantage of X‐ray diffraction, which cannot readily distinguish among different transition‐metal ions. EXAFS analysis was conducted on Ni2+ and Fe3+ ions in nickel aluminate ferrites, and the cation distributions obtained were in good agreement with values obtained by other methods. The ratio of tetrahedral sites occupied by Ni2+ ions decreases with increasing iron content. Fe3+ ions distribute nearly equally to both tetrahedral and octahedral sites. Apparently, not only crystal‐field stabilization energy but also ion size affects cation distribution.

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