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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.

With advancements in aberration-corrected electron optics, the resolution in scanning transmission electron microscopy (STEM) has been significantly improved. More importantly, the reduction of the probe size and the increase of the probe current density enable the acquisition of elemental maps at the atomic scale in a fast manner using both EELS and EDS. With the latest generations of EELS spectrometers, atomic resolution compositional and chemical maps allow interfaces, oxidation state, and even single atoms to be examined with increasing detail. These improvements have also enabled elemental and chemical maps to be acquired rapidly using both low- and high-energy edges from elements across the periodic table, including heavy atoms such Au or Pt. On the EDS side, the introduction of large-area silicon drift detectors (SDD) has allowed these high-beam-current sources to be fully utilized. Improved detector area and support for higher count rates, compared to the previous generation of EDS detectors, allows the acquisition of EDS intensity maps from most types of material in the STEM, even for moderately thin samples. For the case of light elements, the reduced detector dead layer of SDD-based systems partially overcomes the very low florescence yield typical of low-energy X-ray lines. Also as reported in, atomic-level X-ray maps using fast detectors and bright sources can now be collected under some conditions. Because EDS and EELS provide complementary information about the sample, and are both generated with the electron beam, it would be wasteful to not acquire both datasets with every sample run.

The practical advantages of an electron monochromator for electron energy-loss spectroscopy (EELS) in transmission electron microscopy are described. Typical examples from materials and nanoparticle research demonstrate the use of EELS with high energy and spatial resolution. Recent instrumental developments are also reviewed with a discussion of how the technique could be used to study catalyst structures of the future.

Measuring low energy losses in semiconductors and insulators with high spatial resolution becomes attractive with the increasing availability of modern transmission electron microscopes (TEMs) equipped with monochromators, Cs correctors and energy filters. In this paper, we demonstrate that Cerenkov losses pose a limit for the interpretation of low energy loss spectra (EELS) in terms of interband transistions and bandgap determination for many materials. If the velocity of a charged particle in a medium exceeds the velocity of light, photons are emitted leading to a corresponding energy loss of a few electronvolt. Since these losses are strong for energies below the onset of interband transitions, they change the apparent loss function of semiconductors and insulators, with the risk of erroneous interpretation of spectra. We measured low energy losses of Si and GaAs with a monochromated TEM demonstrating the effect of sample thickness on Cerenkov losses. Angle resolved EELS and energy filtered diffraction patterns (taken without a monochromator) show the extremely narrow angular distribution of Cerenkov losses. The latter experiment provides a method that allows to decide whether Cerenkov radiation masks the very low loss signal in EELS.

Energy-filtering transmission electron microscopy (EFTEM), developed about ten years ago, is now a routine analysis tool in the characterization of materials. Based on the physical principles of electron energy-loss spectrometry (EELS), but with the addition of in-column or post-column energy-filters, it forms images of microstructures using a narrow energy band of inelastically scattered electrons. Post-column energy-filters, developed commercially by Gatan (Gatan Imaging Filter, GIF) in the early 1990s, could be attached to nearly any TEM. Almost at the same time, the introduction of the EM-912 microscope with an integrated � -filter by Zeiss, made it possible to use in-column filters as well. These two developments made EFTEM possible on an almost routine basis. The operation of these filters is rather straightforward and it is now possible to acquire element specific images within a few minutes. However, the optimal setup for data acquisition, the judicious choice of experimental parameters to solve specific materials science problems and the interpretation of the results can be rather difficult. For best results, a fundamental knowledge of the underlying physics of EELS and a systematic development of the technical details is necessary. In this work, we discuss the current status of EFTEM in terms of spatial resolution and illustrate it with a few technologically relevant applications at the nanometer length scale. © 2004 Elsevier B.V. All rights reserved.

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.

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.

The analysis of TEM low-loss electron energy-loss spectra i.e. the range up to 50 eV, has recently become attractive and feasible with the advent of advanced TEM equipment and analysis instrumentation, such as monochromators and improved energy-filters / spectrometers [1,2]. The better energy resolution opens up new possibilities for a more accurate measurement of bandgaps and optical properties via the dielectric function. However, a crucial step in the analysis of valence EELS data is the separation of the zero-loss peak [3], ranging into the spectral regime between 0–5 eV. A monochromator can help shortening the tail by narrowing the peak itself, and secondly it makes the shape symmetric, facilitating the study of the band-gap region considerably, even with narrow band-gap semiconductors. On the other hand, physical effects like Cerenkov excitation may pose a limit to the accuracy of band structure investigations, which are further influenced by experimental parameters, bandgap character and / or specimen thickness. Despite the instrumental improvements, the handling of dynamically changing intensities in the low-loss area and the correction of artifacts caused by energy- and spatial drift as well as residual aberrations require an elaborated data acquisition and post-processing scheme, including extra interactivity, robustness and flexibility [4].

We demonstrate the imaging capabilities of energy-filtered transmission electron microscopy at high-energy resolution in the low-energy-loss region, reporting the direct image of a surface plasmon of an elongated gold nanoparticle at energies around 1 eV. Using complimentary model calculations performed within the boundary element method approach we can assign the observed results to the plasmon eigenmodes of the metallic nanoparticle.

In this work we show how energy-filtered imaging can be used to obtain spectrum images of electron energy-loss spectrometric data. Focus is placed on improved energy resolution within these data sets. Using two multilayer samples (GaN/AlN and InP/InAs), we demonstrate the advantages of spectrum-imaging and its extended mapping capabilities. Plasmon-ratio maps are used to quickly create high-contrast material maps with high signal-to-noise ratio, ratio-contrast plots are used to gain optimum settings for the ratio maps, and plasmon-position maps are used to map small shifts of the energy position of bulk plasmon peaks.

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.

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.

Energy filtering transmission electron microscopy (EFTEM) has become one of the most efficient tools for specimen characterization at nanometer length scales. EFTEM imaging is most often carried out in the core-loss region but image intensity becomes more and more a limiting factor with decreasing feature size. Alternatively, it is possible to record EFTEM images in the low-loss region, where intensities are essentially higher and where in many cases the images contain material specific contrasts. In this paper we investigate the influence of the important parameters on the material contrast between silicon and silicon dioxide, e.g. specimen thickness, specimen orientation, energy-loss and energy selecting slit width. We show that sample thickness plays an important role and present two methods to calculate material contrast as a function of energy-loss and sample thicknesses. The first method uses spectra taken from both materials at different sample thickness by electron energy-loss spectroscopy, the second calculates contrast directly from a series of energy filtered images. From the results we determine the ideal acquisition parameters for the Si/SiO 2 system and demonstrate imaging at sufficient resolution below 2 nm with a test sample of thin SiO 2 layers on Si.

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

Electron energy loss (EEL) spectroscopy and high angle annular dark field (HAADF) imaging in aberration-corrected electron microscopes are powerful techniques to determine the chemical composition and structure of materials at atomic resolution. Aberration correction enables the formation of angstrom sized electron probes that contain enough current for both low loss and near-edge core excitation spectroscopy to be performed. Therefore, spatially distributed EEL spectra can be collected and correlated with atomic resolution HAADF images.

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.