Since 1972, when the US Occupational Health and Safety Administration established the first limits on occupational exposure to asbestos fibers, numerous analytical methods employing several microscopy techniques have been developed to identify a group of minerals defined by legislation as asbestos. While transmission electron microscopy (TEM) is implemented in standardized analytical methods, these methods specify the use of selected area electron diffraction. Because of this constraint, the diffraction data a TEM can provide are often underutilized due to challenges associated with collecting and interpreting individual diffraction patterns. It has been shown that transmission electron backscatter diffraction (tEBSD) produces diffraction patterns nearly identical to electron backscatter diffraction, but from smaller crystal domains. This paper explores the utility of tEBSD for characterization of asbestiform particles from reference asbestos materials, a suite of amphibole minerals of varying morphologies to determine if there is a correlation between mineral habit (i.e., crystal form), microscopic particle shape preferred orientation, and mineral specimens from an industrial talc deposit to provide a case study of the utility and limitations of the technique.

The rapid advance and falling costs of computing power and data storage during the last 40 years have greatly enhanced the data reduction speed and analytical capacity of energy dispersive spectroscopy (EDS) systems. At the same time, the solid state X-ray detector [until recently, the Si(Li) diode] has seen performance increases due to the use of advanced materials and processing techniques. In addition, the performance of the electronic components (field effect transistor, preamp, and pulse processor) of an EDS system has been constantly improved. These technology advances have resulted in improved spectral quality, excellent light element detection, and increased count rate performance. The results have been truly remarkable and driven by the needs of the analyst. This article will summarize the progress made in these areas in the last 40 years and make a brief reference to prospects for future development in EDS system performance.

On February 2, 1968, R. Fitzgerald, K. Keil, and K.F.J. Heinrich published a seminal paper in Science (159, 528–530) in which they described a solid-state Si(Li) energy dispersive spectrometer (EDS) for electron probe microanalysis (EPMA) with, initially, a resolution of 600 eV. This resolution was much improved over previous attempts to use either gas-filled proportional counters or solid-state devices for EDS to detect X-rays and was sufficient, for the first time, to make EDS a practically useful technique. It ushered in a new era not only in EPMA, but also in scanning electron microscopy, analytical transmission electron microscopy, X-ray fluorescence analysis, and X-ray diffraction. EDS offers many advantages over wavelength-dispersive crystal spectrometers, e.g., it has no moving parts, covers the entire X-ray energy range of interest to EPMA, there is no defocusing over relatively large distances across the sample, and, of particular interest to those who analyze complex minerals consisting of many elements, all X-ray lines are detected quickly and simultaneously.

An oil painting by Claude Monet, Port-Goulphar, Belle-Ile 1887 (collection of the Art Gallery of New South Wales), was examined to determine both the identity of the pigments used by the artist in this painting and his technique of mixing colors and laying paint on the canvas. The extremely complex construction of the painting was revealed by optical microscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDS), and X-ray mapping (XRM) analysis of cross sections of paint flakes excised from damaged regions of Port-Goulphar, Belle-Ile. Nine different pigments were found on the painting. Many of the identified colors were modern pigments that became available only late in the 19th century as a result of scientific advances in pigment chemistry. Although similar colors were available in a natural mineral form, they lacked the vivid color of their manufactured counterparts. The use of these new synthetic metallic oxide colors by Monet accounts for the brilliance of his paintings. In addition, a separation between successive paint layers was observed in some areas of paint chip cross sections, indicating that oil-based paint was applied to paint that had dried, and consequently, Port-Goulphar, Belle-Ile was painted over a long period of time. This observation is contrary to the general perception of Monet's technique of painting freely and quickly.

The depth profile of thin film layers on bulk substrate, avoiding the cross-sectioning of samples, is commonly performed by techniques such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectroscopy (SIMS). Techniques based on X-ray emission intensity measurements by energy dispersive spectroscopy (EDS), with conventional matrix or ZAF correction, are normally applied to cross-sectioned samples. This article compares XPS with surface X-ray intensity measurements by EDS, carried out with a more realistic X-ray generation and absorption model, known as the ϕ(ρ Z) model. The ϕ(ρ Z) approach has been adopted together with Monte Carlo simulation for the proper selection of SEM accelerating voltages, in conjunction with the analysis of SEM morphological images for thin film density correction. The method discussed hereafter and compared with the XPS technique, has advantages of higher lateral resolution, non-destructive elemental analyses, morphological visualization, low cost, and faster performance. This methodology has been followed to verify the layered structure of SnO2/metal-based gas sensors. X-ray intensities were measured using an EDS ultra-thin window detector. Two different porous layers, 25-nm thick of SnO2 and 10-nm thick of Cu, were detected, showing better agreement with their nominal thickness compared to results obtained using XPS measurements where porosity affects XPS data. If confirmed to be reliable and as effective as XPS depth profiling, this technique may be adopted for process quality control purposes.

As part of the Microbeam Analysis Society (MAS) symposium marking 50 years of electron microprobe analysis, this article reviews the important advances made over the decades to the automation of data collection and computerized analysis of data from the electron microprobe. Out of many innovations that contributed to the advance of microprobe automation, we have chosen to focus on a few developments that the authors feel represent the major trends in advancement of the “state of the art” of this instrumentation. After providing brief summaries of the three generations of advances in the hardware and software of automation systems, several key applications developments are described, followed by our prediction of which current developments may impact the future automation of the microprobe.

Transmission electron microscope samples of two types of metal matrix composites were prepared using both traditional thinning methods and the more novel focused ion beam miller. Electropolishing methods were able to produce, very rapidly, thin foils where the matrix was electron transparent, but the ceramic reinforcement particles remained unthinned. Thus, it was not possible in these foils to study either the matrix-reinforcement interface or the microstructure of the reinforcement particles themselves. In contrast, both phases in the composites prepared using the focused ion beam miller thinned uniformly. The interfaces in these materials were clearly visible and the ceramic reinforcement was electron transparent. However, microstructural artifacts associated with ion beam damage were also observed. The extent of these artifacts and methods of minimizing their effect were dependent on both the materials and the milling conditions used.