Determination of manganese oxidation states in solids by electron energy-loss spectroscopy

James H. Rask; Barbara A. Miner; P R Buseck

doi:10.1016/0304-3991(87)90030-1

Determination of manganese oxidation states in solids by electron energy-loss spectroscopy

James H. Rask, Barbara A. Miner, P R Buseck

Earth and Space Exploration, School of (SESE)

Research output: Contribution to journal › Article › peer-review

123 Scopus citations

Abstract

Electron energy-loss spectra of manganese-bearing phases vary systematically with changes in the average oxidation state of manganese. The energy region recorded, 0 to 1000 eV, includes electronic transitions from manganese and oxygen core orbitals, as well as from states that have contributions from both elements. We used a spectrometer attached to a transmission electron microscope (TEM) to obtain reference spectra from manganese metal and from manganese oxides that contain Mn²⁺, Mn³⁺, and Mn⁴⁺. Such reference spectra can be used to estimate the manganese oxidation state for uncharacterized manganese-bearing solids. Areas with diameters as small as 0.1 μm can be analyzed, thus avoiding the uncertainties associated with bulk analyses of fine-grained, heterogeneous mixtures. Similar determinations of reference energy-loss spectra for other polyvalent elements will broaden the applicability of this technique for the study of small volumes of solids.

Original language	English (US)
Pages (from-to)	321-326
Number of pages	6
Journal	Ultramicroscopy
Volume	21
Issue number	4
DOIs	https://doi.org/10.1016/0304-3991(87)90030-1
State	Published - 1987

ASJC Scopus subject areas

Electronic, Optical and Magnetic Materials
Atomic and Molecular Physics, and Optics
Instrumentation

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10.1016/0304-3991(87)90030-1

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@article{2d0ed70171b742aa97f24d85b2011109,

title = "Determination of manganese oxidation states in solids by electron energy-loss spectroscopy",

abstract = "Electron energy-loss spectra of manganese-bearing phases vary systematically with changes in the average oxidation state of manganese. The energy region recorded, 0 to 1000 eV, includes electronic transitions from manganese and oxygen core orbitals, as well as from states that have contributions from both elements. We used a spectrometer attached to a transmission electron microscope (TEM) to obtain reference spectra from manganese metal and from manganese oxides that contain Mn2+, Mn3+, and Mn4+. Such reference spectra can be used to estimate the manganese oxidation state for uncharacterized manganese-bearing solids. Areas with diameters as small as 0.1 μm can be analyzed, thus avoiding the uncertainties associated with bulk analyses of fine-grained, heterogeneous mixtures. Similar determinations of reference energy-loss spectra for other polyvalent elements will broaden the applicability of this technique for the study of small volumes of solids.",

author = "Rask, {James H.} and Miner, {Barbara A.} and Buseck, {P R}",

note = "Funding Information: Our thanks go to C. Colliex, P. Rez, and O.L. Krivanek for valuable discussion, and to A. Higgs, K. Weiss, and J. Wheatley for technical assistance. Helpful reviews were provided by M. Otten, W. Glaunsinger, and R. Christoffersen. This research was supported by NSF grant EAR 8408169. The ASU HREM facility is supported by NSF Re- gional Instrumentation Program grant DMR-8306501 and Arizona State University.",

year = "1987",

doi = "10.1016/0304-3991(87)90030-1",

language = "English (US)",

volume = "21",

pages = "321--326",

journal = "Ultramicroscopy",

issn = "0304-3991",

publisher = "Elsevier",

number = "4",

}

TY - JOUR

T1 - Determination of manganese oxidation states in solids by electron energy-loss spectroscopy

AU - Rask, James H.

AU - Miner, Barbara A.

AU - Buseck, P R

N1 - Funding Information: Our thanks go to C. Colliex, P. Rez, and O.L. Krivanek for valuable discussion, and to A. Higgs, K. Weiss, and J. Wheatley for technical assistance. Helpful reviews were provided by M. Otten, W. Glaunsinger, and R. Christoffersen. This research was supported by NSF grant EAR 8408169. The ASU HREM facility is supported by NSF Re- gional Instrumentation Program grant DMR-8306501 and Arizona State University.

PY - 1987

Y1 - 1987

N2 - Electron energy-loss spectra of manganese-bearing phases vary systematically with changes in the average oxidation state of manganese. The energy region recorded, 0 to 1000 eV, includes electronic transitions from manganese and oxygen core orbitals, as well as from states that have contributions from both elements. We used a spectrometer attached to a transmission electron microscope (TEM) to obtain reference spectra from manganese metal and from manganese oxides that contain Mn2+, Mn3+, and Mn4+. Such reference spectra can be used to estimate the manganese oxidation state for uncharacterized manganese-bearing solids. Areas with diameters as small as 0.1 μm can be analyzed, thus avoiding the uncertainties associated with bulk analyses of fine-grained, heterogeneous mixtures. Similar determinations of reference energy-loss spectra for other polyvalent elements will broaden the applicability of this technique for the study of small volumes of solids.

AB - Electron energy-loss spectra of manganese-bearing phases vary systematically with changes in the average oxidation state of manganese. The energy region recorded, 0 to 1000 eV, includes electronic transitions from manganese and oxygen core orbitals, as well as from states that have contributions from both elements. We used a spectrometer attached to a transmission electron microscope (TEM) to obtain reference spectra from manganese metal and from manganese oxides that contain Mn2+, Mn3+, and Mn4+. Such reference spectra can be used to estimate the manganese oxidation state for uncharacterized manganese-bearing solids. Areas with diameters as small as 0.1 μm can be analyzed, thus avoiding the uncertainties associated with bulk analyses of fine-grained, heterogeneous mixtures. Similar determinations of reference energy-loss spectra for other polyvalent elements will broaden the applicability of this technique for the study of small volumes of solids.

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DO - 10.1016/0304-3991(87)90030-1

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VL - 21

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EP - 326

JO - Ultramicroscopy

JF - Ultramicroscopy

IS - 4

ER -

Determination of manganese oxidation states in solids by electron energy-loss spectroscopy

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