The carbon contents in carburized steels were investigated by electron probe microanalysis (EPMA) for a range of carbon levels in the solid solution less than 1 wt%. This article describes the difficulties encountered with the classic analytical procedure using the k ratio of X-ray intensities and the φ(ρz) model. Here, a suitable calibration curve method is presented with emphasis on the metallographic study of standard specimens and on the carbon decontamination of samples.

Scanning electron microscopy (SEM) is widely used in surface studies and continuous efforts are carried out in the search of estimators of different surface characteristics. By using the variogram, we developed two of these estimators that were used to characterize the surface roughness from the SEM image texture. One of the estimators is related to the crossover between fractal region at low scale and the periodic region at high scale, whereas the other estimator characterizes the periodic region. In this work, a full study of these estimators and the fractal dimension in two dimensions (2D) and three dimensions (3D) was carried out for emery papers. We show that the obtained fractal dimension with only one image is good enough to characterize the roughness surface because its behavior is similar to those obtained with 3D height data. We show also that the estimator that indicates the crossover is related to the minimum cell size in 2D and to the average particle size in 3D. The other estimator has different values for the three studied emery papers in 2D but it does not have a clear meaning, and these values are similar for those studied samples in 3D. Nevertheless, it indicates the formation tendency of compound cells. The fractal dimension values from the variogram and from an area versus step log–log graph were studied with 3D data. Both methods yield different values corresponding to different information from the samples.

A Nion spherical-aberration (Cs) corrector was recently installed on Lehigh University's 300-keV cold field-emission gun (FEG) Vacuum Generators HB 603 dedicated scanning transmission electron microscope (STEM), optimized for X-ray analysis of thin specimens. In this article, the impact of the Cs-corrector on X-ray analysis is theoretically evaluated, in terms of expected improvements in spatial resolution and analytical sensitivity, and the calculations are compared with initial experimental results. Finally, the possibilities of atomic-column X-ray analysis in a Cs-corrected STEM are discussed.

This article describes the effects of surface controlled decarburization on the structure of a nitrided steel. Samples of quenched and tempered 40CrMo4 steel were decarburized by air heat treatment (800–900°C) at different depths and submitted to gaseous nitriding. The microstructure of surface layers after decarburization and nitriding were investigated by optical (OM) and scanning electron microscopy (SEM). The nitrogen and carbon profiles in the diffusion layers were determined by a scanning electron microscope equipped with a wavelength dispersive spectrometer (EPMA-WDS). The effect of nitriding was determined by microhardness measurements. The increasing of time and temperature of decarburization slightly affect the surface hardness values, while case hardness depths decrease. In all the specimens, the nitriding depth, as determined by the WDS nitrogen profile, is larger than the one determined by the hardness profile.

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Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

Two recent developments in X-ray spectrometer technology provide dramatic improvements in analytical capabilities that impact the frontiers of electron microscopy. Silicon drift detectors (SDD) use the same physics as silicon (lithium) energy dispersive spectrometers [Si(Li) EDS] but differ in design: only 10% of the thickness of the Si(Li) EDS with an anode area below 0.1 mm2 and a complex rear surface electrode pattern that creates a lateral internal charge collection field. The SDD equals or betters the Si(Li) EDS in most measures of performance. For output versus input count rate, the SDD exceeds the Si(Li) EDS by a factor of 5 to 10 for the same resolution. This high throughput can benefit analytical measurements that are count limited, such as X-ray mapping and trace measurements. The microcalorimeter EDS determines the X-ray energy by measuring the temperature rise in a metal absorber. Operating at 100 mK, the microcalorimeter EDS achieves resolution of 2–5 eV over a photon energy range of 200 eV to 10 keV in energy dispersive operation, eliminating most peak interference situations and providing high peak-to-background to detect low fluorescence yield peaks. Chemical bonding effects on low energy (<2 keV) peak shapes can be measured.

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

We describe the recent introduction of low energy X-ray emission spectrometry as a metrology technique to control the fabrication process in the integrated circuit industry. The benefits of this particular analytical method and the wide field of potential applications are addressed.

Multivariate statistical analysis methods have been applied to scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectral images. The particular application of the multivariate curve resolution (MCR) technique provides a high spectral contrast view of the raw spectral image. The power of this approach is demonstrated with a microelectronics failure analysis. Specifically, an unexpected component describing a chemical contaminant was found, as well as a component consistent with a foil thickness change associated with the focused ion beam specimen preparation process. The MCR solution is compared with a conventional analysis of the same spectral image data set.

Microscopy and Microanalysis 2006 will be the premiere meeting of the year for scientists and technologists interested in learning about the latest advances in applications and techniques for the analysis of a broad range of materials in the biological and physical sciences, as well as nano- and bio-technology. M&M-2006 will again host the largest commercial exhibition of microscopy and microanalysis equipment and related accessories in the world. In addition to the usual sponsoring societies, the Microscopy Society of America (MSA), and the Microbeam Analysis Society (MAS), the International Metallographic Society (IMS) will again be a co-sponsoring society for the meeting. We are also fortunate that the Microscopical Society of Canada/Société de Microscopie du Canada (MSC/SMC) will also be co-sponsoring the meeting this year. The M&M-2006 Executive Program Committee, comprised of co-chairs from each of the sponsoring societies, has put together a comprehensive scientific program that will encompass the state-of-the art in microscopy and microanalysis in 2006, and we look forward to welcoming you to Navy Pier!

Microanalysis on the 10-nm level using imaging, diffraction, and spectroscopy of slow photo-emitted and reflected electrons is discussed. The instrumentation that uses a cathode lens is briefly reviewed, and a number of applications illustrate the power of this microanalysis method.

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

A new TEM sample preparation technique using electron-beam-induced deposition combined with low-energy ion milling was used to fabricate for two different shapes of sample, conical and plate. High-quality HREM images can be obtained from samples prepared by this technique. A desired sample position can be obtained with high accuracy, and the total sample preparation time can be much less than conventional techniques. Because the gas deposition system used can easily be integrated in a conventional SEM, the method can be performed in any laboratory equipped with a SEM and an ion milling machine.

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The process of electron-beam-induced deposition (EBID) was simulated with a dynamic Monte Carlo profile simulator, and the growth of carbon, silver, and tungsten supertips was investigated to study the dependence of material composition on the spatial resolution of EBID. Because light atoms have a smaller scattering angle and a longer mean free path, the carbon supertip has the smallest lateral size and the highest aspect ratio of a bottom tip compared to silver and tungsten supertips. Thus the best spatial resolution of EBID can be achieved on materials of low atomic number. The calculation also indicated a significant contribution of primary electrons to the growth of a supertip in EBID, which is consistent with the experimental observations. These results lead to a more comprehensive understanding of EBID, which is a complex interaction process between electrons and solids.

The focus of this review is on trace-element quantitation of microstructures in solids. This review is aimed at the nonspecialist who wants to know how secondary ion mass spectrometry (SIMS) quantitation is achieved. Despite 35 years of SIMS research and applications, SIMS quantitation remains a fundamentally empirical enterprise and is based on standards. The most used standards are “bulk standards”—solids with a homogeneous distribution of a trace element—and ion-implanted solids. The SIMS systematics of bulk standards and ion-implanted solids are reviewed.

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Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005