Quantitative Analyse von Oxiden mit der Elektronenstrahl-Mikrosonde

The influence of a lack of sufficient electrical conductivity on the results of quantitative electron probe microanalysis has been investigated on a number of oxides. The effect of surface charging and the way it alters the emitted X-ray signals has been studied. It is shown that the presence of conducting coatings, such as carbon or copper, will affect the interelement X-ray intensity ratios, whatever the thickness of the coating may be. Although the effects for heavier elements may be acceptable, they cannot be ignored for a light element such as oxygen, where strong variations with coating thickness were observed. Quantitative analyses of oxygen, on uncoated well-conducting oxide specimens, using uncoated well-conducting hematite~Fe 2 O 3 ! as a standard yielded excellent results in the range between 4 and 40 kV with the w~rz! software used. As soon as coated nonconducting specimens were examined, using the same hematite standard, coated under exactly the same conditions, widely scattering and noncoherent results were obtained. These discrepancies can only be attributed to a lack of conductivity.

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“…In the past, copper coatings have been applied~Love et al., 1974;Weisweiler, 1974Weisweiler, , 1978! for quantitative EPMA of oxygen in~mostly!…”

Section: Influence Of a Coating On Quantitative Resultsmentioning

confidence: 99%

Quantitative Electron Probe Microanalysis of Nonconducting Specimens: Science or Art?

Bastin

Heijligers

2004

Microsc Microanal

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Quantitative electron probe microanalysis of carbon in binary carbides. I—principles and procedures

Bastin

Heijligers

1986

X-Ray Spectrometry

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Introductory investigations performed in order to make quantitative electron-probe microanalysis of very light elements such as boron, carbon, nitrogen or oxygen possible are described. The practical problems encountered in this kind of work are discussed in detail and, where possible, solutions are proposed. It is shown that with very light elements such as carbon it is no longer permitted to measure x-ray intensities at the position of the maximum of the emission peak as the shape of the carbon K a peak is subject to strong alterations, depending on the type of chemical bond involved. As a consequence, integral measurements have to be performed and it is shown that errors of 3040% can easily be made if this is neglected. The lengthy procedures, connected with integral intensity measurements, can be shortened considerably by the introduction of arealpeak factors, which, by definition, represent the ratio between the correct area (integral) and the peak intensity ratio. The accurate determination of such factors for 13 binary carbides is described. This set of factors will permit future measurements simply on the peak; multiplication of the peak intensity ratio by the appropriate aredpeak factors will then yield the correct integral intensity ratios.

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Nonconductive Specimens in the Electron Probe Microanalyzer—A Hitherto Poorly Discussed Problem

Bastin

Heijligers

1991

Electron Probe Quantitation

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Quantitative Analyse von Oxiden mit der Elektronenstrahl-Mikrosonde

Cited by 6 publications

References 24 publications

Quantitative Electron Probe Microanalysis of Nonconducting Specimens: Science or Art?

Quantitative Electron Probe Microanalysis of Nonconducting Specimens: Science or Art?

Quantitative electron probe microanalysis of carbon in binary carbides. I—principles and procedures

Nonconductive Specimens in the Electron Probe Microanalyzer—A Hitherto Poorly Discussed Problem

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