PubMed · 5648161
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S J Reed. 1968. Probe current stability in electron-probe microanalysis.. https://doi.org/10.1088/0022-3735%2F1%2F2%2F412
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The formability of galvanneal steel sheets used in the automotive industry is influenced by the presence and distribution of brittle and difficult to distinguish Zn-Fe intermetallics in the coating. Characterization of these intermetallics requires a high spatial resolution technique such as analytical transmission electron microscopy (ATEM). Sample preparation by ion milling is impossible due to iron redeposition, and traditional ultramicrotomy using water affects the coating chemistry. A technique based on dry ultramicrotomy has therefore been developed. To optimize the technique, different parameters (knife angle, cutting medium, thickness setting on the ultramicrotome, cutting speed) have been investigated for the preparation of galvanneal coatings and pure A1 sections. Results show that dry cutting does not affect the coating chemistry but shortens the life of the knife. Knife quality (cleanliness, sharpness and absence of defects) is a major factor to obtain good dry sections. The best results for the more ductile pure A1 are obtained with a 35 degrees knife whilst for the harder galvanneal coating it is recommended to use a 55 degrees knife. These results suggest that the sectioning mechanism for the harder material involves more a cleavage-fracture mechanism whilst a greater amount of shear is involved when sectioning relatively ductile A1. The optimum parameters for sectioning galvanneal coatings are established and results obtained by parallel electron energy loss spectrum imaging and energy dispersive X-ray spectrometry in the TEM are given. This study shows that with a good control of all the sectioning parameters it is possible to obtain good sections repeatedly and rapidly.
Uranium-contaminated soils from the U.S. Department of Energy (DOE) Fernald Site, Ohio, have been examined by a combination of backscattered electron imaging (BSE) and analytical electron microscopy with electron diffraction (AEM). The inhomogeneous distribution of particulate uranium phases in the soil required the development of a method for using ultramicrotomy to prepare transmission electron microscopy (TEM) thin sections from the SEM mounts. A water-miscible resin was selected that allowed comparison between SEM and TEM images, permitting representative sampling of the soil. Uranium was found in iron oxides, silicates (soddyite), phosphates (autunites), and uraninite (UO2 + x). No uranium was detected in association with phyllosilicates in the soil.
Tobacco products are known to cause oral soft-tissue lesions, but they may also directly affect the teeth. Abrasive particles contained in tobacco products may contribute to dental attrition. We studied tobacco samples from 16 brands of cigars, eight brands of snuff, four brands of chewing tobacco and several unprocessed tobacco leaves used as cigar wrappers. Insoluble particulate matter made up about 0.5 percent of the weight of an average tobacco sample.