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Dion-Jacobson phases CsCa 2 Nb 2 FeO 9 and CsCa 2 Nb 2 AlO 9 were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of NbO 6 -MO 4 -NbO 6 in tripled slab, in fact, were mixed phases of n=3 Dion-Jacobson phases and impurities such as Ca 2 NbFeO 6 and Ca 3 Al 2 O 6 . The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of CsCa 2 Nb 2 FeO 9 was calculated into Cs 0.59 Ca 2.64 Nb 2.92 Fe 0.81 in small agglomerate crystals and Cs 0.95 Ca 1.97 Nb 3.08 Fe 0.15 in long plate-like crystals.

Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)