Extended X-Ray Characteristic Fluorescence Fine Structure above the K-Edge of Ni and NiO by Fast Electron Excitation

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.

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EXELFS Studies of Carbon Fibers

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100133953 ◽

1990 ◽

Vol 48 (2) ◽

pp. 72-73

Author(s):

V. Serin ◽

K. Hssein ◽

G. Zanchi ◽

J. Sévely

Keyword(s):

Carbon Fibers ◽

Energy Analysis ◽

Electron Excitation ◽

Complex Structures ◽

High Modulus ◽

Promising Technique ◽

X Ray ◽

Fine Structures ◽

X Ray Absorption

The present developments of electron energy analysis in the microscopes by E.E.L.S. allow an accurate recording of the spectra and of their different complex structures associated with the inner shell electron excitation by the incident electrons (1). Among these structures, the Extended Energy Loss Fine Structures (EXELFS) are of particular interest. They are equivalent to the well known EXAFS oscillations in X-ray absorption spectroscopy. Due to the EELS characteristic, the Fourier analysis of EXELFS oscillations appears as a promising technique for the characterization of composite materials, the major constituents of which are low Z elements. Using EXELFS, we have developed a microstructural study of carbon fibers. This analysis concerns the carbon K edge, which appears in the spectra at 285 eV. The purpose of the paper is to compare the local short range order, determined by this way in the case of Courtauld HTS and P100 ex-polyacrylonitrile carbon fibers, which are high tensile strength (HTS) and high modulus (HM) fibers respectively.

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Extended Core Edge Fine Structure in the E.M.

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s1431927600000489 ◽

1980 ◽

Vol 38 ◽

pp. 120-121

Author(s):

R.D. Leapman

Keyword(s):

Fine Structure ◽

Electron Scattering ◽

Inelastic Electron ◽

High Resolution Imaging ◽

X Ray ◽

Analytical Electron ◽

Analytical Electron Microscope ◽

Core Electrons ◽

Resolution Imaging ◽

X Ray Absorption

Extended X-ray Absorption Fine Structure (EXAFS) analysis makes use of synchrotron radiaion to measure modulations in the absorption coefficient above core edges and hence to obtain information about local atomic environments. EXAFS arises when ejected core electrons are backscattered by surrounding atoms and interfere with the outgoing waves. Recently, interest has also been shown in using inelastic electron scattering1-4. Some advantages of Extended X-ray-edge Energy Loss Fine Structure (EXELFS) are: a) small probes formed by the analytical electron microscope give spectra from μm to nm sized areas, compared with mm diameter areas for the X-ray technique, b) EXELFS can be combined with other techniques such as electron diffraction or high resolution imaging, and c) EXELFS is sensitive to low Z elements with K edges from ˜200 eV to ˜ 3000 eV (B to Cl).

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Some Aspects of Exelfs Analysis in the Electron Microscope

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s1431927600000477 ◽

1980 ◽

Vol 38 ◽

pp. 118-119

Author(s):

D. E. Johnson ◽

S. Csillag

Keyword(s):

Fine Structure ◽

Electron Microscope ◽

Energy Loss ◽

Analytical Electron Microscopy ◽

Interference Effects ◽

Interatomic Distances ◽

X Ray ◽

Structure Information ◽

Microanalytical Technique ◽

Analytical Electron

Recently, the applications area of analytical electron microscopy has been extended to include the study of Extended Energy Loss Fine Structure (EXELFS). Modulations past an ionization edge in the energy loss spectrum (EXELFS), contain atomic fine structure information similar to Extended X-ray Absorbtion Fine Structure (EXAFS). At low momentum transfer the main contribution to these modulations comes from interference effects between the outgoing excited inner shell electron waves and electron waves backscattered from the surrounding atoms. The ability to obtain atomic fine structure information (such as interatomic distances) combined with the spatial resolution of an electron microscope is unique and makes EXELFS an important microanalytical technique.

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