Scanning electron probe microanalysis

K. F. J. Heinrich, Scanning electron probe microanalysis, NBS Technical Note 278, U.S. National Technical Information Service, Springfield, Virginia (1967). 

G. F. Bastin and H. J. M. Heijligers. Quantitative Electron Probe Microanalysis of Ultralight Elements (Boron—Oxygen). Scanning. 12, 225, 1990. 

A number of techniques have been employed that are capable of giving information about amorphous phases. These include infrared spectroscopy, especially the use of the attenuated total reflection (ATR) or Fourier transform (FT) techniques. They also include electron probe microanalysis, scanning electron microscopy, and nuclear magnetic resonance (NMR) spectroscopy. Nor are wet chemical methods to be neglected for they, too, form part of the armoury of methods that have been used to elucidate the chemistry and microstructure of these materials. 

Electron Probe Microanalysis in the Scanning Electron Microscope 137... 

ELECTRON PROBE MICROANALYSIS IN THE SCANNING ELECTRON MICROSCOPE... 

Electron probe microanalysis functions by direct examination of the primary X-rays produced when the specimen is used as a target for an electron beam. Focused electron beams allow a spot analysis of a 1 pm3 section of the specimen. One current development employs the electron beam within a scanning electron microscope to provide both a visual picture of the surface of the sample and an elemental analysis of the section being viewed. Spectra obtained from primary X-rays always have the characteristic emission peaks superimposed on a continuum of background radiation (Figure 8.32). This feature limits the precision, sensitivity and resolution of electron probe microanalysis. 

The evaluation of coal mineral matter by the ashing technique can be taken further insofar as attempts can then be made to determine the individual metal constituents of the ash. On the occasion when the mineral matter has been separated from the coal successfully, it is then possible to apply any one of several techniques (such as x-ray diffraction, x-ray fluorescence, scanning electron microscopy and electron probe microanalysis) not only to investigate the major metallic elements in coal but also to investigate directly the nature (and amount) of the trace elements in the coal (Jenkins and Walker, 1978 Prather et al., 1979 Raymond and Gooley, 1979 Russell and Rimmer, 1979 Jones et al., 1992). Generally, no single method yields a complete analysis of the mineral matter in coal and it is often necessary to employ a combination of methods. 

The toxicity of the mineral is such that quantitative characterization of erionite is extremely important. Samples should be characterized by using one or more of the following techniques (1) powder X-ray diffraction, (2) electron probe microanalysis or inductively coupled plasma-mass spectroscopy, (3) scanning electron microscopy equipped with wavelength dispersive spectroscopy (WDS) and/or energy dispersive spectroscopy (EDS), (4) transmission electron microscopy equipped with WDS and/or EDS and selected area electron diffraction, and (5) similar or better analytical techniques. 

XRD, X-ray diffraction XRF, X-ray fluorescence AAS, atomic absorption spectrometry ICP-AES, inductively coupled plasma-atomic emission spectrometry ICP-MS, Inductively coupled plasma/mass spectroscopy IC, ion chromatography EPMA, electron probe microanalysis SEM, scanning electron microscope ESEM, environmental scanning electron microscope HRTEM, high-resolution transmission electron microscopy LAMMA, laser microprobe mass analysis XPS, X-ray photo-electron spectroscopy RLMP, Raman laser microprobe analysis SHRIMP, sensitive high resolution ion microprobe. PIXE, proton-induced X-ray emission FTIR, Fourier transform infrared. 

The particle size distribution of powders in the range 0.2-0.5 pm can be determined by automated electron probe microanalysis, as developed for particle characterization work at the University of Antwerp (see e.g. Ref. [202]). Here the exciting electron beam of a microprobe scans a deposit of the aerosol particles collected on a Nuclepore filter under computer control, and from the detection of element specific x-ray fluorescence signals, the diameters of a large number of particles are determined automatically. As shown by results for AI2O3, the particle size distributions determined by automated electron probe microanalysis agree to a first approximation with those of stray laser radiation (Fig. 62) [203], Deviations, however,... 

The microstructure of the samples was examined by the x-ray diffraction (XRD), the scanning electron microscope (SEM), and the electron probe microanalysis (EPMA). The electrical conductivity and Seebeck coefficient were measured from 300 to 1200 K. The thermal conductivity was measured by the laser-flash method at room temperature. 

This paper describes ongoing studies of the electrodeposition thin films of the compound semiconductors CdTe and InAs, using the method of electrochemical atomic layer epitaxy (ALE). Surface limited electrochemical reactions are used to form the individual atomic layers of the component elements. An automated electrochemical flow deposition system is used to form the atomic layers in a cycle. Studies of the conditions needed to optimize the deposition processes are underway. The deposits were characterized using X-ray diffraction, scanning probe microscopy, electron probe microanalysis and optical/infrared absorption spectroscopy. 

Characterize nitride layer microstructure and composition by x-ray diffraction, electron probe microanalysis, scanning electron microscopy, and transmission electron microscopy. Use this information in a feedback loop to modify alloy chemistry and nitridation processing conditions to optimize the protectiveness of the nitride surface layer. 

EPMA Electron probe microanalysis SEM Scanning electron microscopy... 

X-Ray Fluorescence Spectrometry Terms associated with the broad technique of X-ray fluorescence spectrometry are electron spectrometry. X-ray spectrometry, electron microscopy, analytical electron microscopy, scanning transmission electron microscopy (STEM), electron diffraction, electron probe microanalysis. Auger electron spectrometry. X-ray photoelectron spec-... 

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