Gianluca Ruffato, Marco Beleggia, Amir Hossein Tavabi, Enzo Rotunno, Lorenzo Viani, Paolo Rosi, Payam Habibzadeh Kavkani, Caterina Chiari, Stefano Frabboni, Gian Carlo Gazzadi, Giulio Pozzi, Giovanni Bertoni, Peter Tiemeijer, Rafal Edward Dunin-Borkowski, Vincenzo Grillo
{"title":"Three-dimensional Stacking of Phase Plates for Advanced Electron Beam Shaping.","authors":"Gianluca Ruffato, Marco Beleggia, Amir Hossein Tavabi, Enzo Rotunno, Lorenzo Viani, Paolo Rosi, Payam Habibzadeh Kavkani, Caterina Chiari, Stefano Frabboni, Gian Carlo Gazzadi, Giulio Pozzi, Giovanni Bertoni, Peter Tiemeijer, Rafal Edward Dunin-Borkowski, Vincenzo Grillo","doi":"10.1093/mam/ozae108","DOIUrl":"https://doi.org/10.1093/mam/ozae108","url":null,"abstract":"<p><p>Tuneable phase plates for free electrons are a highly active area of research. However, their widespread implementation, similar to that of spatial light modulators in light optics, has been hindered by both conceptual and technical challenges. A specific technical challenge involves the need to minimize obstruction of the electron beam by supporting films and electrodes. Here, we describe numerical and analytical mathematical frameworks for three-dimensional stacks of phase plates that can be used to provide near-arbitrary electron beam shaping with minimal obstruction.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142730364","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
D Keith Coffman, Khalid Hattar, Jian Luo, Shen Dillon
{"title":"Spectral Pyrometry for Practical Temperature Measurement in the TEM.","authors":"D Keith Coffman, Khalid Hattar, Jian Luo, Shen Dillon","doi":"10.1093/mam/ozae114","DOIUrl":"https://doi.org/10.1093/mam/ozae114","url":null,"abstract":"<p><p>Recent work in ultra-high temperature in situ electron microscopy has presented the need for accurate, contact-free temperature determination at the microscale. Optical measurement based on thermal radiation (pyrometry) is an attractive solution but can be difficult to perform correctly due to effects, such as emissivity and optical transmission, that must be accounted for. Here, we present a practical guide to calibrating and using a spectral pyrometry system, including example code, using a Czerny-Turner spectrometer attached to a transmission electron microscope. Calibration can be accomplished using a thermocouple or commercial heated sample holder, after which arbitrary samples can be reliably measured for temperatures above ∼600∘C. An accuracy of 2% can be expected with the possibility of sub-second temporal resolution and sub-Kelvin temperature resolution. We then demonstrate this capability in conjunction with traditional microscopic techniques, such as diffraction-based strain measurement for thermal expansion coefficient, or live-video sintering evolution.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142730362","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marcel Schloz, Thomas C Pekin, Hamish G Brown, Dana O Byrne, Bryan D Esser, Emmanuel Terzoudis-Lumsden, Takashi Taniguchi, Kenji Watanabe, Scott D Findlay, Benedikt Haas, Jim Ciston, Christoph T Koch
{"title":"Improved Three-Dimensional Reconstructions in Electron Ptychography through Defocus Series Measurements.","authors":"Marcel Schloz, Thomas C Pekin, Hamish G Brown, Dana O Byrne, Bryan D Esser, Emmanuel Terzoudis-Lumsden, Takashi Taniguchi, Kenji Watanabe, Scott D Findlay, Benedikt Haas, Jim Ciston, Christoph T Koch","doi":"10.1093/mam/ozae110","DOIUrl":"10.1093/mam/ozae110","url":null,"abstract":"<p><p>A detailed analysis of ptychography for three-dimensional (3D) phase reconstructions of thick specimens is performed. We introduce multi-focus ptychography, which incorporates a 4D-STEM defocus series to enhance the quality of 3D reconstructions along the beam direction through a higher overdetermination ratio. This method is compared with established multi-slice ptychography techniques, such as conventional ptychography, regularized ptychography, and multi-mode ptychography. Additionally, we contrast multi-focus ptychography with an alternative method that uses virtual optical sectioning through a reconstructed scattering matrix (S-matrix), which offers more precise 3D structure information compared to conventional ptychography. Our findings from multiple 3D reconstructions based on simulated and experimental data demonstrate that multi-focus ptychography surpasses other techniques, particularly in accurately reconstructing the surfaces and interface regions of thick specimens.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142668369","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Single Electron Self-coherence and Its Wave/Particle Duality in the Electron Microscope.","authors":"C Kisielowski, P Specht, J R Jinschek, S Helveg","doi":"10.1093/mam/ozae107","DOIUrl":"https://doi.org/10.1093/mam/ozae107","url":null,"abstract":"<p><p>Intensities in high-resolution phase-contrast images from electron microscopes build up discretely in time by detecting single electrons. A wave description of pulse-like coherent-inelastic interaction of an electron with matter implies a time-dependent coexistence of coherent partial waves. Their superposition forms a wave package by phase decoherence of 0.5 - 1 radian with Heisenbergs energy uncertainty ΔEH = ħ/2 Δt-1 matching the energy loss ΔE of a coherent-inelastic interaction and sets the interaction time Δt. In these circumstances, the product of Planck's constant and the speed of light hc is given by the product of the expression for temporal coherence λ2/Δλ and the energy loss ΔE. Experimentally, the self-coherence length was measured by detecting the energy-dependent localization of scattered, plane matter waves in surface proximity exploiting the Goos-Hänchen shift. Chromatic-aberration Cc-corrected electron microscopy on boron nitride (BN) proves that the coherent crystal illumination and phase contrast are lost if the self-coherence length shrinks below the size of the crystal unit cell at ΔE > 200 eV. In perspective, the interaction time of any matter wave compares with the lifetime of a virtual particle of any elemental interaction, suggesting the present concept of coherent-inelastic interactions of matter waves might be generalizable.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623907","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Samuel S Welborn, Chris Harris, Stephanie M Ribet, Georgios Varnavides, Colin Ophus, Bjoern Enders, Peter Ercius
{"title":"Streaming Large-Scale Microscopy Data to a Supercomputing Facility.","authors":"Samuel S Welborn, Chris Harris, Stephanie M Ribet, Georgios Varnavides, Colin Ophus, Bjoern Enders, Peter Ercius","doi":"10.1093/mam/ozae109","DOIUrl":"https://doi.org/10.1093/mam/ozae109","url":null,"abstract":"<p><p>Data management is a critical component of modern experimental workflows. As data generation rates increase, transferring data from acquisition servers to processing servers via conventional file-based methods is becoming increasingly impractical. The 4D Camera at the National Center for Electron Microscopy generates data at a nominal rate of 480 Gbit s-1 (87,000 frames s-1), producing a 700 GB dataset in 15 s. To address the challenges associated with storing and processing such quantities of data, we developed a streaming workflow that utilizes a high-speed network to connect the 4D Camera's data acquisition system to supercomputing nodes at the National Energy Research Scientific Computing Center, bypassing intermediate file storage entirely. In this work, we demonstrate the effectiveness of our streaming pipeline in a production setting through an hour-long experiment that generated over 10 TB of raw data, yielding high-quality datasets suitable for advanced analyses. Additionally, we compare the efficacy of this streaming workflow against the conventional file-transfer workflow by conducting a postmortem analysis on historical data from experiments performed by real users. Our findings show that the streaming workflow significantly improves data turnaround time, enables real-time decision-making, and minimizes the potential for human error by eliminating manual user interactions.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623922","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Model-Fitting Weighted Least Squares as an Alternative to Principal Component Analysis for Analyzing Energy-Dispersive X-ray Spectroscopy Spectrum Images.","authors":"David Wahlqvist, Martin Ek","doi":"10.1093/mam/ozae106","DOIUrl":"https://doi.org/10.1093/mam/ozae106","url":null,"abstract":"<p><p>Spectrum imaging with energy-dispersive X-ray spectroscopy (EDS) has become ubiquitous in material characterization using electron microscopy. Multivariate statistical methods, commonly principal component analysis (PCA), are often used to aid analysis of the resulting multidimensional datasets; PCA can provide denoising prior to further analysis or grouping of pixels into distinct phases with similar signals. However, it is well known that PCA can introduce artifacts at low signal-to-noise ratios. Unfortunately, when evaluating the benefits and risks with PCA, it is often compared only against raw data, where it tends to shine; alternative data analysis methods providing a fair point of comparison are often lacking. Here, we directly compare PCA with a strategy based on (the conceptually and computationally simpler) weighted least squares (WLS). We show that for four representative cases, model fitting of the sum spectrum followed by WLS (mfWLS) consistently outperforms PCA in terms of finding and accurately describing compositional gradients and inclusions and as a preprocessing step to clustering. Additionally, we demonstrate that some common artifacts and biases displayed by PCA are avoided with the mfWLS approach. In summary, mfWLS can provide a superior option to PCA for analysis of EDS spectrum images as the signal is simply and accurately modeled.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623893","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ellis Kennedy, Emily Hollingworth, Alejandro Ceballos, Daisy O'Mahoney, Colin Ophus, Frances Hellman, Mary Scott
{"title":"Exploring Structural Anisotropy in Amorphous Tb-Co via Changes in Medium-Range Ordering.","authors":"Ellis Kennedy, Emily Hollingworth, Alejandro Ceballos, Daisy O'Mahoney, Colin Ophus, Frances Hellman, Mary Scott","doi":"10.1093/mam/ozae113","DOIUrl":"https://doi.org/10.1093/mam/ozae113","url":null,"abstract":"<p><p>Amorphous thin films grown by magnetron co-sputtering exhibit changes in atomic structure with varying growth and annealing temperatures. Structural variations influence the bulk properties of the films. Scanning nanodiffraction performed in a transmission electron microscope (TEM) is applied to amorphous Tb17Co83 (a-Tb-Co) films deposited over a range of temperatures to measure relative changes in medium-range ordering (MRO). These measurements reveal an increase in MRO with higher growth temperatures and a decrease in MRO with higher annealing temperatures. The trend in MRO indicates a relationship between the growth conditions and local atomic ordering. By tilting select films, the TEM measures variations in the local atomic structure as a function of orientation within the films. The findings support claims that preferential ordering along the growth direction results from temperature-mediated adatom configurations during deposition, and that oriented MRO correlates with increased structural anisotropy, explaining the strong growth-induced perpendicular magnetic anisotropy found in rare earth-transition metal films. Beyond magnetic films, we propose the tilted FEM workflow as a method of extracting anisotropic structural information in a variety of amorphous materials with directionally dependent bulk properties, such as films with inherent bonding asymmetry grown by physical vapor deposition.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623881","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Connor J Parker, Kathryn M Peruski, Samantha K Cary
{"title":"Quantitative Particle Analysis of Neptunium-237 Oxides: Optimization of MAMA Analysis for Modified Direct Denitration Products.","authors":"Connor J Parker, Kathryn M Peruski, Samantha K Cary","doi":"10.1093/mam/ozae112","DOIUrl":"https://doi.org/10.1093/mam/ozae112","url":null,"abstract":"<p><p>The production of plutonium-238 through irradiation of neptunium-237 (237Np) target materials for the use in radioisotope thermoelectric generators is paramount for continued deep space exploration. This work employs scanning electron microscopy to analyze 237Np materials coupled with a well-developed image analysis framework (Morphological Analysis for Material Attribution, or MAMA) to determine the degree of micron-scale homogeneity in the materials. This work demonstrated how the quantification of particle characteristics can validate production materials and affirm the qualitative similarities observed in micrographs. The 237Np oxide particle analysis determined that the materials from five production runs were quantitatively homogenous (significant at α = 0.05) in particle area, circularity, equivalent circular diameter, and ellipse aspect ratio, with two of the sampling dates having statistically significant different means for one of the four characteristics. These metrics not only confirm general homogeneity of the material but also expand the application of MAMA workflows to 237Np materials, demonstrating the utility of MAMA analysis for a wider breadth of nuclear materials than previously reported. In the open literature, this study is the first time that these microanalytical techniques were applied to 237Np materials to this degree.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623900","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Laser-Assisted Field Evaporation of Chromia with Deep Ultraviolet Laser Light.","authors":"Severin Jakob, Andrea Fazi, Mattias Thuvander","doi":"10.1093/mam/ozae111","DOIUrl":"https://doi.org/10.1093/mam/ozae111","url":null,"abstract":"<p><p>In this work, samples of chromia (Cr2O3) scale have been prepared for atom probe tomography and field evaporated with deep ultraviolet laser light (258 nm wavelength). The investigated range of laser energies spans more than three orders of magnitude between 0.03 and 90 pJ. Furthermore, the effects of detection rate and temperature were investigated. Simultaneous voltage and laser pulses were employed on additional needle specimens to reduce the standing voltage and minimize background noise during the measurement. Smooth evaporation with minimal mass spectrum peak tails was maintained over the whole range of measurement parameters. High laser energies result in significant underestimation of the oxygen content. Only laser energies below 1 pJ resulted in measured values near the expected oxygen content of 60 at%, the closest being about 58 at%.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623887","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ian MacLaren, Andrew T Fraser, Matthew R Lipsett, Colin Ophus
{"title":"Digital Dark Field-Higher Contrast and Greater Specificity Dark Field Imaging Using a 4DSTEM Approach.","authors":"Ian MacLaren, Andrew T Fraser, Matthew R Lipsett, Colin Ophus","doi":"10.1093/mam/ozae104","DOIUrl":"https://doi.org/10.1093/mam/ozae104","url":null,"abstract":"<p><p>A new method for dark field imaging is introduced, which uses scanned electron diffraction (or 4DSTEM-4-dimensional scanning transmission electron microscopy) datasets as its input. Instead of working on simple summation of intensity, it works on a sparse representation of the diffraction patterns in terms of a list of their diffraction peaks. This is tested on a thin perovskite film containing structural ordering resulting in additional superlattice spots that reveal details of domain structures, and is shown to give much better selectivity and contrast than conventional virtual dark field imaging. It is also shown to work well in polycrystalline aggregates of CuO nanoparticles. In view of the higher contrast and selectivity, and the complete exclusion of diffuse scattering from the image formation, it is expected to be of significant benefit for characterization of a wide variety of crystalline materials.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":""},"PeriodicalIF":2.9,"publicationDate":"2024-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142623871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}