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Eingeladener Vortrag
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More and more sub-micro and nano-materials shall be "quickly", but accurately characterized with respect to their morphology, shape, size or size distribution, but also to the chemical composition as well by means of an SEM/EDX (Scanning Electron Microscopy / X-Ray Energy Dispersive Spectrometry) system. This undertaking is becoming successful indeed if the transmission mode at low voltages such as those at a SEM, i. e. mostly up to 30 kV, and EDX, respectively is employed. The transmission mode at conventional SEM can e "activated" firstly by re-defining the specimen to be analyzed and preparing it as a thin specimen, which is quasi-transparent to electrons and by finding a way of collecting only the transmitted electrons for analysis. The first issue can be easily realized by using the conventional TEM grids (and the respective sample preparation); the second one becomes feasible either (i) by placing a socalled STEM semiconductor detector directly under the thin specimen or (ii) by using a Special transmission set-up, which enables to the conventional Everhart-Thornley detector to collect only transmitted electrons by blocking the direct collection of secondary electrons and guiding only the transmitted electrons onto it.
Results of an interlaboratory comparison on size characterization of SiO2 airborne nanoparticles using on-line and off-line measurement techniques are discussed. This study was performed in the framework of Technical Working Area (TWA) 34—'Properties of Nanoparticle Populations' of the Versailles Project on Advanced Materials and Standards (VAMAS) in the project no. 3 'Techniques for characterizing size distribution of airborne nanoparticles'. Two types of nano-aerosols, consisting of (1) one population of nanoparticles with a mean diameter between 30.3 and 39.0 nm and (2) two populations of non-agglomerated nanoparticles with mean diameters between, respectively, 36.2–46.6 nm and 80.2–89.8 nm, were generated for characterization measurements. Scanning mobility particle size spectrometers (SMPS) were used for on-line measurements of size distributions of the produced nano-aerosols. Transmission electron microscopy, scanning electron microscopy, and atomic force microscopy were used as off-line measurement techniques for nanoparticles characterization. Samples were deposited on appropriate supports such as grids, filters, and mica plates by electrostatic precipitation and a filtration technique using SMPS controlled generation upstream. The results of the main size distribution parameters (mean and mode diameters), obtained from several laboratories, were compared based on metrological approaches including metrological traceability, calibration, and evaluation of the measurement uncertainty. Internationally harmonized measurement procedures for airborne SiO2 nanoparticles characterization are proposed.
For ten years µ-XRF (micro-focus X-ray fluorescence) analysis has been performed with SEM/EDS (scanning electron microscope with an energy dispersive X-ray detector) so that non-destructive analysis of elements at trace level concentrations below 100 µg g-1 becomes possible. This can be considered as a valuable completion of the classical electron probe microanalysis by EDS, an analytical method 'suffering' from rather poor limits of detection in the range of one to two orders of magnitude higher than those of µ-XRF. Based on a representative actual application, namely analysis of RoHS relevant elements at trace concentration levels, the performance of the rather new analytical method with respect to its limits of detection is systematically evaluated. CRMs (certified reference materials) specially prepared to support the quantitative XRF analysis of RoHS relevant elements were employed. On the other side, based on calculations of µ-XRF spectra according to a recently developed physical model the optimization of the analytical performance is also successfully undertaken.