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A microfocus X-ray source mounted on the analysis chamber of an SEM was used to excite X-ray fluorescence spectra and to detect chemical elements with concentrations below the detection limit of the electron-excited X-ray spectra conventionally measured with SEM/EDS. An aluminium alloy and a hard material ceramics were analysed as representative examples. It is demonstrated that the combination of the three analytical methods: (1) SEM imaging for surface morphology characterisation; (2) electron-excited X-ray spectroscopy with its high spatial resolution for element analysis of inclusions or precipitates; and (3) X-ray fluorescence for the detection of elements with concentrations below 0.1 mass% considerably improves the performance of SEM/EDX analyses.
A new microfocus X-ray source iMOXS for high sensitive XRF analysis in scanning electron microscopes
(2004)
Scanning electron microscopes are usually equipped with energy-dispersive X-ray detectors for electron probe microanalysis. This widespread analytical method allows investigators to determine the elemental composition of specimens with a spatial resolution of about 1 µm. However, owing to the electron-specimen interaction, the emitted spectra reveal, in addition to characteristic lines, also a high level of continuous bremsstrahlung background. As a result, elements with low concentrations cannot be identified. The minimum detection limit can be diminished by two orders of magnitude if the characteristic lines are excited as fluorescence by an additional x-ray source. In this case, the emergence of bremsstrahlung is considerably reduced. Combining a high-brilliance microfocus x-ray tube with efficient polycapillary optics enables one to realize an experimental arrangement for performing local fluorescence analysis at the same point where the electron beam hits the sample. The polycapillary optics under consideration focuses the emitted x-radiation onto focal spots between 30 and 100 µm in diameter. Count rates of several thousands cps have been achieved. Elemental maps have been obtained by means of the motorized specimen stage of the microscope. Copyright © 2005 John Wiley & Sons, Ltd.