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Organisationseinheit der BAM
TEM Characterization of the Interface Quality of MOVPE Grown Strained InGaAs/GaAs Heterostructures
(1995)
Efficiency and response functions were determined for a modern commercial energy-dispersive x-ray spectrometer in the photon energy range 0.1-5 keV using dispersed and undispersed synchrotron radiation. The spectrometer was equipped with an Si(Li) detector crystal, a thin-film window and a digital pulse processor. Monochromatized synchrotron radiation from the PTB VUV radiometry beamline at the electron storage ring BESSY was used for the absolute determination of the detection efficiency with a typical relative uncertainty of 1-2% in the photon energy range 0.1-1.5 keV by direct comparison with calibrated photodiodes. At higher photon energies, the efficiency was found by comparison of the measured and calculated undispersed synchrotron radiation spectrum. The absolute intensity of the synchrotron radiation was known with a relative uncertainty of less than 1%. In the overlapping region, the results from the two independent experiments are in full agreement. The energy dependence of the measured efficiency can be explained only with a detector model assuming that there is no dead layer. A simple model for the effect of incomplete charge collection (ICC) was applied to describe the measured response functions. Consequences of the ICC such as broadening and shift of low-energy peaks and redistribution of counts around 1.84 keV are explained with the model, in accordance with the experimental results.
Energy dispersive X-ray spectrometry offers the opportunity for fast composition determination of specimens by X-ray fluorescence or electron probe microanalysis. For fundamental parameter based quantification, the knowledge of the detection efficiency of the spectrometer is essential. At low energies the efficiency is strongly influenced by X-ray absorption in the radiation entrance window. State-of-the-art windows consist of polymer foil containing C, N, and O, coated with Al and in some cases with a special B compound. The foil is supported by a Si grid to withstand the atmosphere pressure. The absorption of all these components must be known to describe the detection efficiency.
The transmittance of three types of widely used commercial windows has been measured. Transmittance curves have been fitted by analytical expressions using tabulated mass absorption coefficients. Because tabulated mass absorption coefficients do not consider near edge effects, there are strong deviations between measured and calculated transmittance below 0.6 keV. It is proposed to model the spectrometer efficiency by the measured window transmittance and calculated absorptions from front contact and possible contaminations. This reduces the number of unknown parameters drastically.
Quality assurance according to ISO or EN norms entails a periodical check of critical instrumental parameters. Not yet all commercial software purchased with instruments supports the related measurements and their fast evaluation. EDXTOOLS consist of a programme library which complements the existing software for electron excited energy dispersive X-ray spectrometry (EDS) in this respect. EDXTOOLS can be used to check the detection efficiency by the evaluation of the L/K intensity ratio in a copper or nickel spectrum or by the calculation of the thickness of absorbing detector layers from experiments, which can be performed on any scanning electron microscope. Moreover, measured spectra can be modified by the transmission curve of absorbing media to estimate their influence on the result of quantitative analysis. EDXTOOLS allow the determination of the signal to background ratio from an Fe-55 spectrum and the fitting of measured FWHM's of K-lines to find the resolution curve DE = Ö{DE 2el + DE 2det}. They are completed by the possibility of calculating EDX spectra for the K-lines of light elements and to compare the resulting spectra for different formulae, physical data tables, and detector parameters chosen for the calculation. EDXTOOLS are written in MATLAB®, a wide spread interpreter language. This has the advantage that the programmes are readable text files. A user can check each computational step and modify it. The installation of MATLAB® and its optimization toolbox is necessary to work with EDXTOOLS.
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.
The results of an interlaboratory comparison of energy dispersive X-ray microanalysis of TiN0.84 and ZrN were presented. The microprobe group of the German Physical Society (DPG) and the Federal Institute for Materials Research and Testing (BAM) had initiated the interlaboratory comparison. The primary aim was to test modern EDX systems equipped with ultrathin windows concerning the accuracy and reliability of the analysis of compounds containing light elements. The participants from 23 laboratories performed the analysis at different primary energies, in the standard-less mode as well as on the base of own standards, and considering Ti-K or Ti-L in case of TiN0.84. The results show a slight overestimation of the nitrogen content and a large standard deviation from the mean value. Reasons for the scattering of the results are discussed.