Journal ArticleDOI
High-resolution parallel electron energy-loss spectroscopy of Mn L2,3-edges in inorganic manganese compounds
Laurence A. J. Garvie,Alan J. Craven +1 more
- Vol. 21, Iss: 4, pp 191-206
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TLDR
In this article, parallel electron energy loss spectroscopy (PEELS) was used to record the Mn L2,3-edges from a range of natural and synthetic manganese containing materials, covering valences 0, II, III, IV and VII, with an energy resolution of ca. 0.5 eV.Abstract:
Parallel electron energy-loss spectroscopy (PEELS) in a scanning transmission electron microscope (STEM) was used to record the Mn L2,3-edges from a range of natural and synthetic manganese containing materials, covering valences 0, II, III, IV and VII, with an energy resolution of ca. 0.5 eV. The Mn L2,3 electron-loss near-edge structure (ELNES) of these edges provided a sensitive fingerprint of its valence. The Mn2+ L2,3-edges show little sensitivity to the local site symmetry of the ligands surrounding the manganese. This is illustrated by comparing the Mn L2,3-edges from 4-, 6- and 8-fold coordinated Mn2+. In contrast, the Mn L3-edges from Mn3+ and Mn4+ containing minerals exhibited ELNES that are interpreted in terms of a crystal-field splitting of the 3d electrons, governed by the symmetry of the surrounding ligands. The Mn L3-edges for octahedrally coordinated Mn2+, Mn3+ and Mn4+ showed variations in their ELNES that were sensitive to the crystal-field strength. The crystal-field strength (10Dq) was measured from these edges and compared very well with published optically determined values. The magnitude of 10Dq measured from the Mn L3-edges and their O K-edge prepeaks of the manganese oxides were almost identical. This further confirms that the value of 10Dq measured at the Mn L3-edge is correct. Selected spectra are compared with theoretical 2p atomic multiplet spectra and the differences and similarities are explained in terms of the covalency and site symmetry of the manganese. The Mn L3-edges allow the valence of the manganese to be ascertained, even in multivalent state materials, and can also be used to determine 10Dq.read more
Citations
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Journal ArticleDOI
Oxidation state and chemical shift investigation in transition metal oxides by EELS
TL;DR: In this article, the transition metal L 2,3 electron energy-loss spectra for a wide range of V-, Mn- and Fe-based oxides were recorded and carefully analyzed for their correlation with the formal oxidation states of transition metal ions.
Journal ArticleDOI
Determination of Mn valence states in mixed-valent manganates by XANES spectroscopy
TL;DR: In this paper, a compilation of the X-ray absorption near-edge structure (XANES) spectra of most naturally occurring manganates, synthetic analogs of known structure and chemical composition, and pure-valence phase species is presented and made available as an open source.
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Penelope J. Boston,Michael N. Spilde,Diana E. Northup,Leslie A. Melim,D.S. Soroka,L.G. Kleina,Kathleen H. Lavoie,Louise D. Hose,L.M. Mallory,Clifford N. Dahm,Laura J. Crossey,Rachel T. Schelble +11 more
TL;DR: The cave/subsurface astrobiology model addresses the most important goals from both scientific and operational points of view and presents details of cave biosignature suites involving manganese and iron oxides, calcite, and sulfur minerals.
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Ratios of ferrous to ferric iron from nanometre-sized areas in minerals
TL;DR: In this paper, the authors used electron energy-loss spectroscopy with a transmission electron microscope to determine Fe3+/ΣFe in minerals at the nanometre scale.
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Unravelling structural ambiguities in lithium- and manganese-rich transition metal oxides.
TL;DR: The bulk of the oxides can be described as an aperiodic crystal consisting of randomly stacked domains that correspond to three variants of monoclinic structure, while the surface is composed of a Co- and/or Ni-rich spinel with antisite defects.
References
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Book
Advanced Inorganic Chemistry
TL;DR: Cotton and Wilkinson's Advanced Inorganic Chemistry (AIC) as discussed by the authors is one of the most widely used inorganic chemistry books and has been used for more than a quarter century.
Book
Electron Energy-Loss Spectroscopy in the Electron Microscope
Ray F. Egerton,Dale E. Newbury +1 more
TL;DR: In this article, the authors present an overview of the basic principles of energy-loss spectroscopy, including the use of the Wien filter, and the analysis of the inner-shell of the detector.
Journal ArticleDOI
Oxygen 1s x-ray-absorption edges of transition-metal oxides
F. M. F. de Groot,Marco Grioni,John C. Fuggle,Jacques Ghijsen,George A. Sawatzky,Harald Petersen +5 more
TL;DR: On a mesure les limites d'absorption des rayons X de l'oxygene 1s d'une serie d'oxydes de metaux de transition 3d dans les etats inoccupes du caractere metallique principal.
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