We present a specimen preparation procedure for atom-probe tomography using SemGlu from Kleindiek Nanotechnik, an adhesive that hardens under electron beam irradiation. The SemGlu adhesive is used in place of focused-ion-beam-induced deposition of organo-metallic Pt, W, or C to form a bond between the sample and the substrate during the specimen preparation procedure. We demonstrate the utility of this adhesive-based specimen preparation technique with a correlated atom-probe tomography-scanning transmission electron microscopy study of the iron-nickel alloy kamacite (ferrite, ɑ-iron) in the Bristol iron meteorite and two steel specimens.

The capability to perform liquid in situ transmission electron microscopy (TEM) experiments provides an unprecedented opportunity to examine the real-time processes of physical and chemical/electrochemical reactions during the interaction between metal surfaces and liquid environments. This work describes the requisite steps to make the technique fully analytical, from sample preparation, through modifications of the electrodes, characterization of electrolytes, and finally to electrochemical corrosion experiments comparing in situ TEM to conventional bulk cell and microcell configurations.

In recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

Modern analytical electron microscopes equipped with silicon drift detectors now allow for a wide range of geometrical configurations capable of performing quantitative X-ray spectrometry. Recent work has improved the collection solid angles of these detectors, however, the impact of increasing the solid angle on detection sensitivity as measured by the peak/background ratio has not been addressed. This work compares theoretical and experimental peak/background ratios for incident electron energies in the range of 20–200 keV, with X-ray detectors in both conventional orientations (on the electron entrance surface) as well as new geometries (the electron exit surface). The implications of these parameters on detectability limits for the next generations of “Lab-in-the-Gap” analytical microscope are also considered. It was found that theoretical calculations of the angular distribution of bremsstrahlung and their effects on the peak/background ratio match well with experimental measurements, and indicate that new geometries which can result in large solid angles provided an added benefit in addition to increased characteristic signal, namely increased sensitivity for the analyst.