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Related Experiment Video

Updated: Feb 5, 2026

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

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Published on: October 27, 2018

Atomic-Scale Determination of Cation Inversion in Spinel-Based Oxide Nanoparticles.

Pau Torruella, Alicia Ruiz-Caridad¹, Michael Walls¹

¹Laboratoire de Physique des Solides , Paris-Sud University , Orsay 91405 CEDEX , France.

|August 31, 2018

Summary

This study uses atomic-resolution electron microscopy and electron energy-loss spectroscopy to map cation distribution in iron oxide/manganese oxide nanoparticles. This provides new insights into the structure-property relationships of spinel oxides.

Keywords:

EELS Magnetic nanoparticles cation inversion core−shell spinel

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Area of Science:

Materials Science
Nanotechnology
Solid-State Chemistry

Background:

Transmission electron microscopy (TEM) excels at determining atomic structure but struggles with chemical information at the atomic column level.
Characterizing the precise cation distribution and oxidation states in complex nanostructures like spinel oxides is crucial for understanding their properties.

Purpose of the Study:

To develop and apply atomic-resolution techniques for chemical mapping in crystalline spinel Fe3O4/Mn3O4 core-shell nanoparticles.
To precisely determine the cation distribution and oxidation states within the core and shell of these nanoparticles.
To introduce methods for quantifying cation inversion in spinel lattices at the atomic scale.

Main Methods:

High-resolution scanning transmission electron microscopy (HR-STEM) for atomic structure imaging.
Atomic-resolution electron energy-loss spectroscopy (EELS) for mapping Mn and Fe oxidation states.
X-ray absorption spectroscopy (XAS) for bulk sample characterization.
Development of two EELS-based methods for local cation inversion evaluation.

Main Results:

Direct atomic-resolution mapping of Mn2+/Mn3+ in the shell and Fe2+/Fe3+ in the core was achieved.
Precise understanding of the core-shell interface and cation distribution within the nanoparticle lattice was obtained.
Two novel EELS methods successfully determined the cation inversion parameter and its spatial variations in both the iron oxide core and manganese oxide shell.
XAS confirmed the presence of cation inversion in the overall sample.

Conclusions:

Atomic-resolution EELS is a powerful tool for chemical analysis in nanostructured materials.
The developed methods enable precise quantification of cation inversion in spinel oxides at the nanoscale.
These findings advance the correlation between structural characteristics and functional properties of nanostructured spinel oxides.