Hostname: page-component-745bb68f8f-v2bm5 Total loading time: 0 Render date: 2025-01-09T22:37:35.089Z Has data issue: false hasContentIssue false
  • English
  • Français

The development of X-ray photo-emission electron microscopy (XPEEM) for valence-state imaging of mineral intergrowths

Published online by Cambridge University Press:  05 July 2018

A. D. Smith ,
P. F. Schofield ,
G. Cressey ,
B. A. Cressey  and
P. D. Read
A. D. Smith*
Affiliation:
CLRC Daresbury Laboratory, Daresbury, Warrington WA4 4AD, UK
P. F. Schofield*
Affiliation:
Department of Mineralogy, Natural History Museum, Cromwell Road, London SW7 5BD, UK
G. Cressey
Affiliation:
Department of Mineralogy, Natural History Museum, Cromwell Road, London SW7 5BD, UK
B. A. Cressey
Affiliation:
Science & Engineering Electron Microscopy Centre, Department of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK
P. D. Read
Affiliation:
CLRC Rutherford Appleton Laboratory, Chilton, Didcot, Oxfordshire OX11 0QX, UK
*
*E-mail: [email protected]
†E-mail: [email protected]
Get access Rights & Permissions [Opens in a new window]

Abstract

We demonstrate the potential of X-ray photo-emission electron microscopy (XPEEM) to reveal valence-state images of the spatial distribution and relative concentration of metals in specific oxidation states. Additionally, XPEEM allows X-ray absorption spectra to be extracted from chosen pixel areas of the images. Using an in-house-built XPEEM instrument we show an application of the method in providing valence-state images of complex mineral intergrowths. The image resolution achieved with this instrument of simple design was ∼5 μm and reasonable quality X-ray absorption spectra were extracted from areas of ∼5×5 μm. These initial results suggest that by using commercial XPEEM instruments on 3rd generation, high-brightness synchrotron sources a spatial resolution of 100 nm or better could be achieved, with the ability to extract high-quality X-ray absorption spectra from areas of 0.1 μm2. Given that standard thin sections or polished blocks can be studied by XPEEM, and that each XPEEM image records ∼1000 μm2, XPEEM can be used in conjunction with other analytical methods such as EMPA and TEM-EELS/PEELS.

Keywords

X-ray photo-emission electron microscopyXPEEMvalence-state imagingXAScrystal chemistry
Type
Research Article
Information
Mineralogical Magazine , Volume 68 , Issue 6 , December 2004 , pp. 859 - 869
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2004

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Cressey, G., Henderson, C.M.B. and van der Laan, G. (1993) Use of L-edge X-ray absorption spectroscopy to characterize multiple valence states of 3d transition metals; a new probe for mineralogical and geochemical research. Physics and Chemistry of Minerals, 20, 111–119.CrossRefGoogle Scholar
de Groot, F.M.F., Figueirdo, M.O., Basto, M.J., Abbate, M., Petersen, H. and Fuggle, J.C. (1992) 2p X-ray absorption of Ti in minerals. Physics and Chemistry of Minerals, 19, 140–147.CrossRefGoogle Scholar
Garvie, L.A. and Buseck, P.R. (1998) Ratios of ferrous to ferric iron from nanometre-sized areas in minerals. Nature, 396, 667–670.CrossRefGoogle Scholar
Garvie, L.A. and Craven, A.J. (1994) High-resolution parallel electron energy-loss spectroscopy of Mn L2,3-edges in inorganic manganese compounds. Physics and Chemistry of Minerals, 21, 191–206.CrossRefGoogle Scholar
Garvie, L.A., Craven, A.J. and Brydson, R. (1994) Use of electron-energy loss near-edge fine structure in the study of minerals. American Mineralogist, 79, 411–425.Google Scholar
Gilbert, B., Frazer, B.H., Naab, F., Fournelle, J., Valley, J.W. and De Stasio, G. (2003) X-rayabsorption spectroscopyof silicates for in situ, sub-micrometer mineral identification. American Mineralogist, 88, 763–769.CrossRefGoogle Scholar
Henderson, C.M.B., Cressey, G. and Redfern, S.A.T. (1995) Geological applications of synchrotron radiation. Radiation Physics and Chemistry, 45, 459–481.CrossRefGoogle Scholar
Mythen, C.S., van der Laan, G. and Padmore, H.A. (1992) The undulator beamline at the SRS Daresbury. Review of Scientific Instruments, 63, 1313–1316.CrossRefGoogle Scholar
Pattrick, R.A.D., van der Laan, G., Vaughan, D.J. and Henderson, C.M.B. (1993) Oxidation state and electronic configuration determination of copper in tetrahedrite group minerals by L-edge X-ray absorption spectroscopy. Physics and Chemistry of Minerals, 20, 395–401.CrossRefGoogle Scholar
Roper, M.D. and Purton, J.A. (2001) Recent performance and developments on the Daresbury SRS soft X-ray undulator beamline. Nuclear Instruments and Methods in Physics Research. Section A – Accelerators, Spectrometers, Detectors and Associated Equipment, A467, 516–519.Google Scholar
Schofield, P.F., Henderson, C.M.B., Cressey, G. and van der Laan, G. (1995) 2p X-rayabsorption spectroscopyin the Earth sciences. Journal of Synchrotron Radiation, 2, 93–98.CrossRefGoogle Scholar
Schofield, P.F., Smith, A.D., Cressey, G., Cressey, B.A., Pattrick, R.A.D., Ohldag, H. and Scholl, A. (2002) Valence state imaging of mineral intergrowths. 18th General Meeting of the International Mineralogical Association, Edinburgh, Abstracts, A7–6, p. 109.Google Scholar
Smith, A.D., Cressey, G., Schofield, P.F. and Cressey, B.A. (1998) Development of X-ray photo-emission electron microscopy(X-PEEM) at the SRS. Journal of Synchrotron Radiation, 5, 1108–1110.CrossRefGoogle Scholar
Smith, A.D., Schofield, P.F., Scholl, A., Pattrick, R.A.D. and Bridges, J.C. (2003) PEEM valence state imaging of mineral intergrowths with a spatial resolution of 100 nm. Journal de Physique IV, 104, 373–376.Google Scholar
Tonner, B.P. and Dunham, D. (1994) Submicron spatial-resolution of a micro-xafs electrostatic microscope with bending magnet radiation – performance assessments and prospects for aberration correction. Nuclear Instruments and Methods in Physics Research. Section A – Accelerators, Spectrometers, Detectors and Associated Equipment, A347, 436–440.Google Scholar
Tonner, B.P. and Harp, G.R. (1988) Photoelectron microscopy with synchrotron radiation. Review of Scientific Instruments, 59, 853–858.CrossRefGoogle Scholar
van Aken, P.A., Liebscher, B. and Styrsa, V.J. (1998) Quantitative determination of iron oxidation states in minerals using Fe L2,3-edge electron energy-loss near-edge structure spectroscopy. Physics and Chemistry of Minerals, 25, 323–327.CrossRefGoogle Scholar
van der Laan, G. and Kirkman, I.W. (1992) The 2p absorption spectra of 3d transition metal compounds in tetrahedral and octahedral symmetry. Journal of Physics of Condensed Matter, 4, 4189–4204.CrossRefGoogle Scholar
van der Laan, G., Pattrick, R.A.D., Henderson, C.M.B. and Vaughan, D.J. (1992) Oxidation state variations in copper minerals studied with Cu 2p X-ray absorption spectroscopy. Journal of Physics and Chemistry of Solids, 53, 1185–1190.CrossRefGoogle Scholar