Electron-energy-loss spectroscopy (EELS) with an electron microscope and X-ray absorption spectroscopy (XAS) with a synchrotron are techniques for material characterization, both of which are based on exciting core electrons. Both techniques have a similar energy resolution, but while the spatial resolution of EELS can drop to atomic scales, the spatial resolution of XAS is typically limited to micrometer scales. Yet, XAS is commonly the preferred technique for analysis of the extended fine structure of ionization edges, mainly thanks to the excellent signal-to-noise ratio and the large range of ionization energies (from similar to 5 to similar to 40 keV) that can be probed at synchrotron end stations. In contrast, EELS is traditionally limited to ionization energies of less than or similar to 2 keV because electrons in the beam that lose more than 2 keV will be too distant from the operating energy of the electron microscope. Chromatic effects in the postsample lenses allow only some of such energy-loss electrons to reach the EELS detector, as the latter electrons will either suffer from being strongly defocused or will not make it to the detector at all. In this paper, we present results from our novel Iliad EELS spectrometer, which offers a greatly increased range of ionization energies up to 30 keV. We achieve this vast increase by carefully controlling the optics of our electron microscope and carefully matching the optics of our EELS spectrometer to it, such that all the chromatic effects are removed or compensated. We exemplify its performance by recording EELS nearedge fine structure (ELNES) of the Zr L-edges at 2.3 keV, extended fine structure EELS (EXELFS) of Cu K-edge at similar to 9 keV, and EELS of the Mo K-edge at 20 keV and Sb K-edge at similar to 30 keV. We benchmark our data against near-edge and extended fine structure X-ray absorption (XANES and EXAFS) data, and we quantitatively analyze the Cu K-edge EXELFS, demonstrating the capability to determine elementspecific bond lengths and to distinguish different oxidation states such as metallic Cu, Cu2O, or CuO on a submicrometer scale.

Summary Atomic electric fields in a thin GaN sample are measured with the centre‐of‐mass approach in 4D‐scanning transmission electron microscopy (4D‐STEM) using a 12‐segmented STEM detector in a Spectra 300 microscope. The electric fields, charge density and potential are compared to simulations and an experimental measurement using a pixelated 4D‐STEM detector. The segmented detector benefits from a high recording speed, which enables measurements at low radiation doses. However, there is measurement uncertainty due to the limited number of segments analysed in this study.

Nanomaterial properties and functionalities are influenced by their shape, size, and chemical composition. The importance of these parameters highlights the need for a statistically robust analysis of a large particle population, necessitating automation. This study introduces a neural network‐empowered smart scan technique that achieves a relative increase in speed compared to traditional energy‐dispersive X‐ray spectroscopy (EDX) mapping. The main advantage is that it reduces the required dose, decreasing potential damage to the sample by avoiding unnecessary exposure. It holds potential use in other multimodal scanning transmission electron microscopy or scanning‐based imaging approaches. In the first example, identifying particles in a matrix with a trained neural network reduces the acquisition time by two orders of magnitude. This acceleration enables a statistical compositional analysis of thousands of particles in less than 1 h. Similar improvements are observed for atomic resolution. The discrete positions of atoms identified by the trained network allow for selective EDX sampling at these centers, thereby identifying the atomic species of the column with much‐reduced sampling. Consequently, a lower sampling dose is required, enabling mapping of more delicate materials with high lateral resolution and at a high statistical confidence interval. Even though manual training is still required, this approach greatly benefits repetitive quality control tasks.

The relation between the energy-dependent particle and wave descriptions of electron–matter interactions on the nanoscale was analyzed by measuring the delocalization of an evanescent field from energy-filtered amplitude images of sample/vacuum interfaces with a special aberration-corrected electron microscope. The spatial field extension coincided with the energy-dependent self-coherence length of propagating wave packets that obeyed the time-dependent Schrödinger equation, and underwent a Goos–Hänchen shift. The findings support the view that wave packets are created by self-interferences during coherent–inelastic Coulomb interactions with a decoherence phase close to Δφ = 0.5 rad. Due to a strictly reciprocal dependence on energy, the wave packets shrink below atomic dimensions for electron energy losses beyond 1000 eV, and thus appear particle-like. Consequently, our observations inevitably include pulse-like wave propagations that stimulate structural dynamics in nanomaterials at any electron energy loss, which can be exploited to unravel time-dependent structure–function relationships on the nanoscale.

Journal Article A New Superstructure in Beam Sensitive Cathode Material Revealed by Multimodal STEM Combining ADF, iDPC and EDX Mapping Techniques Get access Maria Meledina, Maria Meledina Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Corresponding author: maria.meledina@thermofisher.com Search for other works by this author on: Oxford Academic Google Scholar Alexander Meledin, Alexander Meledin Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Eric G T Bosch, Eric G T Bosch Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Ivan Lazić, Ivan Lazić Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Xiaochao Wu, Xiaochao Wu Institute of Inorganic Chemistry, RWTH Aachen University, Aachen, Germany Search for other works by this author on: Oxford Academic Google Scholar Ulrich Simon, Ulrich Simon Institute of Inorganic Chemistry, RWTH Aachen University, Aachen, Germany Search for other works by this author on: Oxford Academic Google Scholar Boy Markus, Boy Markus Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Bert Freitag, Bert Freitag Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Sorin Lazar, Sorin Lazar Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Paolo Longo Paolo Longo Thermo Fisher Scientific, Materials & Structural Analysis, Eindhoven, the Netherlands Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 29, Issue Supplement_1, 1 August 2023, Pages 1764–1765, https://doi.org/10.1093/micmic/ozad067.912 Published: 22 July 2023

Cation-disordered rocksalt (DRX) oxides are promising candidates as next-generation cathodes for lithium-ion batteries. Partial fluorination of the DRX oxides enhances their cyclability. However, the lattice position, concentration, and spatial distribution of fluorine within DRX lattices remain elusive. Here, we use atom location by channeling-enhanced microanalysis, energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy, and integrated differential phase contrast imaging in a scanning transmission electron microscope to gain atomic-level insights into DRX with nominal composition of Li1.2Mn0.7Ti0.1O1.7F0.3 and Li1.15Ni0.45Ti0.3Mo0.1O1.85F0.15. We reveal that fluorine substitutes oxygen in the DRX lattices. The O/F ratio in terms of O+F = 2 is in the range from 1.92:0.08 to 1.82:0.18. Spatially, fluorine is distributed in the proximity of the Li-rich regions but distinct from lithium fluoride. Additionally, we observe that incorporation of fluorine in the DRX lattice induces a larger variation in cation-anion separation. These observations provide insight into the guided design of oxyfluoride DRX cathodes for high-performance batteries.

Journal Article EELS at Very High Energy Losses - an Opportunity to Provide Complementary Information to X-ray Absorption Spectroscopy (XAS) Get access Sorin Lazar, Sorin Lazar Thermo Fisher Scientific, Eindhoven, The Netherlands Corresponding author: Sorin.Lazar@Thermofisher.com Search for other works by this author on: Oxford Academic Google Scholar Maria Meledina, Maria Meledina Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Claudia Schnohr, Claudia Schnohr Felix Bloch Institute for Solid State Physics, Leipzig, Germany Search for other works by this author on: Oxford Academic Google Scholar Thomas Hoeche, Thomas Hoeche Fraunhofer-Institut für Mikrostruktur von Werkstoffen und Systemen IMWS, Halle (Saale), Germany Search for other works by this author on: Oxford Academic Google Scholar Peter Tiemeijer, Peter Tiemeijer Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Paolo Longo, Paolo Longo Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Bert Freitag Bert Freitag Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 29, Issue Supplement_1, 1 August 2023, Pages 369–370, https://doi.org/10.1093/micmic/ozad067.172 Published: 22 July 2023

Ultra‐low‐dose electron diffraction is performed with a double metal cyanide catalyst (DMC) to understand how electron irradiation stimulates structural alterations in functional materials. The commonly fading diffraction patterns with dose accumulation depend on the irradiated area and the beam current even when below 50 femto Amperes. Heat generation is observed and modeled by statistical, inelastic scattering events to describe how phonon excitations modulate radiation hardness. Specifically, the characteristic 1/e‐decay of Bragg intensities from DMC is delayed from 6 to 30 eÅ −2 at room temperature, which is comparable to the effect of embedding radiation soft matter in ice. DMC's radiation hardness is enhanced by a latency dose that forms during a phase transformation. This unifying model predicts that a critical dose rate exists for any material that varies between 0.1 and 10 4 eÅ −2 s −1 because of a material dependent competition of heat generation and spread. It shows that Brillouin scattering causes time dependent perturbations in electron irradiated solids that trigger time‐temperature‐transformations on a time scale of nanoseconds to microseconds at room temperature, which is not included in traditional models describing the decay of Bragg intensities by radiolysis.

Journal Article Benefits of Using a 4 srad XEDS Detector in Quantitative 3D-Compositional Analysis of Core@shell Nanoparticles Get access Qiongyang Chen, Qiongyang Chen Electron Microscopy for Materials Science, University of Antwerp, Antwerp, Belgium Search for other works by this author on: Oxford Academic Google Scholar Adrian Pedrazo-Tardajos, Adrian Pedrazo-Tardajos Electron Microscopy for Materials Science, University of Antwerp, Antwerp, Belgium Search for other works by this author on: Oxford Academic Google Scholar Maarten Wirix, Maarten Wirix Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Lin Jiang, Lin Jiang Thermo Fisher Scientific, Hillsboro, OR, USA Search for other works by this author on: Oxford Academic Google Scholar Bert Freitag, Bert Freitag Thermo Fisher Scientific, Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar Sara Bals Sara Bals Electron Microscopy for Materials Science, University of Antwerp, Antwerp, Belgium Corresponding author: sara.bals@uantwerpen.be Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 554–555, https://doi.org/10.1017/S143192762200280X Published: 01 August 2022

The shape, size, chemical composition and distribution of nanoparticles influence their properties and function especially in catalysis applications. The relevance of such measurements depends greatly on a statistically significant analysis on sufficiently large numbers of particles. Therefore, an automatic, fast, and reliable way of characterizing these parameters is pivotal in nanoparticle research. We demonstrated a relative speed up of two orders of magnitude compared to the classical procedure based on full frame XEDS mapping.

The correlation between particle and wave descriptions of electron-matter interactions is analyzed by measuring the delocalization of an evanescent field using electron microscopy. Its spatial extension coincides with the energy-dependent, self-coherence length of propagating wave packets that obey the time-dependent Schrödinger equation and undergo a Goos-Hänchen shift. In the Heisenberg limit they are created by self-interferences during coherent-inelastic Coulomb interactions with a decoherence phase Δϕ = 0.5 rad and shrink to particle-like dimensions for energy losses of more than 1000 eV.

Journal Article Latency Dose Formation In DMC By Inelastic Electron Scattering Get access P Specht, P Specht Department of MSE, University of California Berkeley, Berkeley, CA 94720, USA Corresponding author: specht@berkeley.edu Search for other works by this author on: Oxford Academic Google Scholar C Kisielowski, C Kisielowski TMF, Lawrence Berkeley National Laboratory, One Cyclotron Rd., Berkeley, CA 94720, USA Search for other works by this author on: Oxford Academic Google Scholar B Freitag, B Freitag Thermo Fisher Scientific, Achtseweg Noord 5, 5651 GG Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar ER Kieft, ER Kieft Thermo Fisher Scientific, Achtseweg Noord 5, 5651 GG Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar S Rozeveld, S Rozeveld The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar J Kang, J Kang The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar AJ Fielitz, AJ Fielitz The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar TR Fielitz, TR Fielitz The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar D van Dyck, D van Dyck EMAT, University of Antwerp, 2020 Antwerp, Belgium Search for other works by this author on: Oxford Academic Google Scholar DF Yancey DF Yancey The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 2216–2217, https://doi.org/10.1017/S1431927622008558 Published: 01 August 2022

Journal Article Coherence and Inelastic Scattering in Electron Microscopy Get access C Kisielowski, C Kisielowski TMF, Lawrence Berkeley National Laboratory, One Cyclotron Rd., Berkeley, CA 94720, USA Corresponding author: CFKisielowski@lbl.gov Search for other works by this author on: Oxford Academic Google Scholar P Specht, P Specht Department of MSE, University of California Berkeley, Berkeley, CA 94720, USA Search for other works by this author on: Oxford Academic Google Scholar B Freitag, B Freitag Thermo Fisher Scientific, Achtseweg Noord 5, 5651 GG Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar ER Kieft, ER Kieft Thermo Fisher Scientific, Achtseweg Noord 5, 5651 GG Eindhoven, The Netherlands Search for other works by this author on: Oxford Academic Google Scholar S Rozeveld, S Rozeveld The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar J Kang, J Kang The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar AJ Fielitz, AJ Fielitz The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar TR Fielitz, TR Fielitz The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar DF Yancey, DF Yancey The Dow Chemical Company, Midland, MI 48667, USA Search for other works by this author on: Oxford Academic Google Scholar D van Dyck D van Dyck EMAT, University of Antwerp, 2020 Antwerp, Belgium Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 2762–2763, https://doi.org/10.1017/S143192762201039X Published: 01 August 2022

Understanding the thermal stability of bimetallic nanoparticles is of vital importance to preserve their functionalities during their use in a variety of applications. In contrast to well-studied bimetallic systems such as Au@Ag, heat-induced morphological and compositional changes in Au@Pt nanoparticles are insufficiently understood, even though Au@Pt is an important material for catalysis. To investigate the thermal instability of Au@Pt nanorods at temperatures below their bulk melting point, we combined in situ heating with two- and three-dimensional electron microscopy techniques, including three-dimensional energy-dispersive X-ray spectroscopy. The experimental results were used as input for molecular dynamics simulations, to unravel the mechanisms behind the morphological transformation of Au@Pt core-shell nanorods. We conclude that thermal stability is influenced not only by the degree of coverage of Pt on Au but also by structural details of the Pt shell.