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We outline a simple routine to correct for non-uniformities in the energy dispersion of a post-column electron energy-loss spectrometer for use in scanning transmission electron microscopy. We directly measure the dispersion and its variations by sweeping a spectral feature across the full camera to produce a calibration that can be used to linearize datasets post-acquisition, without the need for reference materials. The improvements are illustrated using core excitation electron energy-loss spectroscopy (EELS) spectra collected from NiO and diamond samples. The calibration is rapid and will be of use in all EELS analysis, particularly in assessments of the chemical states of materials via the chemical shift of core-loss excitations.

We present and compare two different imaging techniques for plasmonic excitations in metallic nanoparticles based on high energy-resolution electron energy-loss spectroscopy in a monochromated transmission electron microscope. We demonstrate that a recently developed monochromated energy-filtering (EFTEM) approach can be used in addition to the well established scanning technique to directly obtain plasmon images in the energy range below 1 eV. The EFTEM technique is described in detail, and a double experiment performed on the same, triangular gold nanoparticle compares equivalent data acquired by both techniques, respectively.

Energy-filtering TEM (EFTEM) has turned out to be a very efficient and rapid tool for the chemical characterization of a specimen on a nanometer and even subnanometer length scale. Especially, the detection and measurement of very thin layers has become a great application of this technique in many materials science fields, e.g. semiconductors and hard disk technology. There, the reliability of compositional profiles is an important issue. However, the experimentally obtainable spatial resolution strongly influences the appearance of a thin layer in an EFTEM image, when dimensions reach subnanometer levels, which mainly leads to a broadening of the layer in the image. This fact has to be taken into account, when measuring the thickness of such a thin layer. Additionally, the convolution decreases contrast which makes the layer less visible in the image and finally determines the detection limit. In this work we present a systematic study on specifically designed Mn/PdMn multilayer test specimens to explore the practical aspects of spatial resolution and detection limits in EFTEM. Although specific to the ionization edges used, we will present general conclusions about the practical limitations in terms of EFTEM spatial resolution. Additionally, work will be shown about low energy-loss imaging of thin oxide layers, where delocalization is the main factor responsible for broadening.

While FIB sample preparation for transmission electron microscopy is a well established technique, few examples exist of samples of sufficient quality for atomic resolution imaging by aberration corrected (scanning) transmission electron microscopy (STEM). In this work we demonstrate the successful preparation of such samples from five different materials and present the refined lift-out preparation technique, which was applied here. Samples with parallel surfaces and a general thickness between 20 and 40 nm over a range of several μm were repeatedly prepared and analyzed by Cs-corrected STEM at 60 and 100 kV. Here, a novel ‘wedge pre-milling’ step helps to keep the protective surface layers intact during the whole milling process, allowing features close to or at the sample surface to be analyzed without preparation damage. Another example shows the cross-sectional preparation of a working thin film solar cell device to a final thickness of 10 to 20 nm over μm sized areas in the region of interest, enabling atomic resolution imaging and elemental mapping across general grain boundaries without projection artefacts. All sample preparation has been carried out in modern Dual-Beam FIB microscopes capable of low-kV Ga+ ion milling, but without additional preparation steps after the FIB lift-out procedure.

Electronic defects at interfaces between different materials or at extended structural defects such as grain boundaries (GB) or dislocations can deteriorate the performance of a semiconductor device considerably. Cu(In,Ga)Se2 (CIGS) thin-film solar cells consist of several interfaces between individual layers of different materials. In addition, the main light-absorbing layer, the CIGS absorber, exhibits a high density of GBs (i.e., the average grain size is typically smaller than the layer thickness) as well as of dislocations (up to 10 10 cm -2 in high-efficiency solar cells [1]). Still, CIGS solar cells exhibit highest power-conversion efficiencies of up to 20.8 % [2]. Today, the roles of interfaces and extended structural defects in the solar-cell device are not yet fully understood, although extensive research efforts have been made. We applied various methods in transmission electron microscopy (TEM), such as inline electron holography, electron energy-loss spectroscopy (EELS), as well as energy-dispersive X-ray spectroscopy (EDS) in order to obtain more information about these features.

We present a fully automated method for three-dimensional (3D) elemental analysis demonstrated using a ceramic sample of chemistry (Ca)MgTiO(x). The specimen is serially sectioned by a focused ion beam (FIB) microscope, and energy-dispersive X-ray spectrometry (EDXS) is used for elemental analysis of each cross-section created. A 3D elemental model is reconstructed from the stack of two-dimensional (2D) data. This work concentrates on issues arising from process automation, the large sample volume of approximately 17 x 17 x 10 microm(3), and the insulating nature of the specimen. A new routine for post-acquisition data correction of different drift effects is demonstrated. Furthermore, it is shown that EDXS data may be erroneous for specimens containing voids, and that back-scattered electron images have to be used to correct for these errors.

This paper deals with the application of high-energy resolution EFTEM image series and the corrections needed for reliable data interpretation. The detail of spectral information gained from an image series is largely determined by the intrinsic energy resolution. In this work we show that energy resolution values of as low as 0.8 eV in spectra extracted from EFTEM image series can be obtained with a small energy-selecting slit. At this resolution level aberrations of the energy filter, in particular the non-isochromaticity, can no longer be neglected. We show that the four most prominent factors for EFTEM image series data correction--spatial drift, non-isochromaticity, energy drift and image distortion--must not be treated independently but have to be corrected in unison. We present an efficient algorithm for this correction, and demonstrate the applied correction for the case of a GaN/AlN multilayer sample.

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Software is an integral part of all electron microscopy systems, encompassing hardware control, data acquisition and processing. It is unlikely that any one software system will meet all the requirements of experienced users. However, if the software supports custom scripting, then users are well placed to address any shortcomings by writing their own software. In this paper, we highlight the scripting capability within Gatan Inc.'s Digital Micrograph™ (DM) software, a widely used program for TEM imaging and EELS spectroscopy. We show how scripting can greatly extend the capabilities of the DM software, in tasks ranging in complexity from simple image manipulation through to full-blown microscope/imaging filter control and data acquisition. Scripting enables customised software tools to be developed to meet individual experimental needs, something which no software manufacturer could ever hope to do on a commercial basis. In essence, scripting allows the microscopist to drive the software rather than the software drive the microscopist. To foster an increased awareness and interest in DM scripting we have developed a web-based archive for DM scripts, which is freely accessible via the internet.

Energy filtering transmission electron microscopy (EFTEM) is a widely used technique in many areas of scientific research. Image contrast in energy-filtered images arises from specific scattering events such as the ionization of atoms. By combining a set of two or more images, relative sample thickness maps or elemental distribution maps can be easily created. It is also possible to acquire a whole series of energy-filtered images to do more complex data analysis. However, whenever several images are combined to extract certain information, problems are introduced due to sample drift between the exposures. In order to obtain artifact-free information, this spatial drift has to be taken care of. Manual alignment by overlaying and shifting the images to find the best overlap is usually very accurate but extremely time consuming for larger data sets. When large amounts of images are recorded in an EFTEM series, manual correction is no longer a reasonable option. Hence, automatic routines have been developed that are mostly based on the cross-correlation algorithm. Existing routines, however, sometimes fail and again make time consuming manual adjustments necessary. In this paper we describe a new approach to the drift correction problem by incorporating a statistical treatment of the data and we present our statistically determined spatial drift (SDSD) correction program. We show its improved performance by applying it to a typical EFTEM series data block.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

BiFeO3 has been the subject of intense interest in recent years on account of possible multiferroic properties. Recently, Reaney and co-workers demonstrated that rare-earth doping can induce the formation of antipolar order with similarities to the PbZrO3 structure. This study reports for the first time studies of the atomic structure and chemistry of nanoscale defects in such materials.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2008 in Albuquerque, New Mexico, USA, August 3 – August 7, 2008

Extended abstract of a paper presented at MC 2007, 33rd DGE Conference in Saarbrücken, Germany, September 2 – September 7, 2007

Extended abstract of a paper presented at MC 2007, 33rd DGE Conference in Saarbrücken, Germany, September 2 – September 7, 2007

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

The 'lift-out' technique using a focused ion beam microscope was applied to prepare cross-sectional specimens of organic light-emitting diodes for use in transmission electron microscopy. The focused ion beam equally thins the organic/inorganic hybrid devices despite the difference in material hardness of the compounds. This allowed to overcome preparation difficulties of conventional techniques such as ion thinning or ultra-microtomy. Two different samples were prepared and studied by both conventional transmission electron microscopy and analytical electron microscopy to display some of the investigation possibilities which become available with this sample preparation method.