Distinct nanostructures in (Co,Mn,Fe)3O4 were investigated using X-ray diffraction techniques combined with transmission and scanning transmission electron microscopy, as well as energy dispersive X-ray spectroscopy. The size of the checkerboard nanostructure increased with annealing, followed by the appearance of lamellar nanostructures comprising different types of platelike nanodomains because of nanoscopic spinodal decomposition of Mn and Fe ions. Remarkable local strain relaxation at the nanoscale associated with the domain size is suggested to play an important role in the stabilization of these checkerboard and lamellar nanostructures.
Controllability of the nanostructures in spinel-type manganese oxide ZnMnGaO4 by changing cooling rate was studied via transmission electron microscopy (with selected area electron diffraction and bright- and dark-field imaging) as well as X-ray diffraction. The Quench sample exhibited a tweed pattern, suggesting the coexistence of two phases at the nanometer scale. The nanostructural changes from a fine twin structure to a checkerboard nanostructure, followed by the emergence of a lamellar-type nanostructure, were clearly observed as the cooling rate decreased from quenching to 1 °C h−1. It was suggested that the diffusion of manganese ions accompanied by the Jahn–Teller distortion play an important role in the formation of nanostructures of this system.
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