Ultramicroscopy最新文献

{"title":"Electron backscattering coefficient, material contrast and response function of BSE- detectors in scanning electron microscopy","authors":"E.I. Rau,&nbsp;S.V. Zaitsev","doi":"10.1016/j.ultramic.2025.114196","DOIUrl":"10.1016/j.ultramic.2025.114196","url":null,"abstract":"<div><div>An empirical expression for the electron backscattering coefficient η, mean backscattered energy coefficient ε and response function F of backscattered electrons (BSE) detectors in scanning electron microscope (SEM) are established for bulk specimens in dependence of atomic number Z and primary electrons energy E_B.</div><div>The obtained expressions give more precisely data of η than all previous publications in the wide energy range E_B 1–30 keV. They were used to describe the dependence of the BSE signal I_S from atomic number of the target material Z and SEM accelerating voltage E_B. The image contrast as a function of Z -differences and E_B is considered. Particular attention is paid to the influence of the response function F on the formation of the I_S signal. All consideration were carried out with commercial semiconductor or scintillation BSE – detectors installed in SEM in standard position below from objective lens and right above the sample. The characteristics were compared with similar of the multichannel plate (MCP) detector.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114196"},"PeriodicalIF":2.1,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144297109","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simulation-based super-resolution EBSD for measurements of relative deformation gradient tensors","authors":"Aimo Winkelmann ,&nbsp;Grzegorz Cios ,&nbsp;Konrad Perzyński ,&nbsp;Tomasz Tokarski ,&nbsp;Klaus Mehnert ,&nbsp;Łukasz Madej ,&nbsp;Piotr Bała","doi":"10.1016/j.ultramic.2025.114180","DOIUrl":"10.1016/j.ultramic.2025.114180","url":null,"abstract":"<div><div>We summarize a data analysis approach for electron backscatter diffraction (EBSD) which uses high-resolution Kikuchi pattern simulations to measure isochoric relative deformation gradient tensors from experimentally measured Kikuchi patterns of relatively low resolution. Simulation-based supersampling of the theoretical test diffraction patterns enables a significant precision improvement of tensor parameters obtained in best-fit determinations of strains and orientations from low-resolution experimental patterns. As an application, we demonstrate high-resolution orientation and strain analysis for the model case of hardness test indents on a Si(100) wafer, using Kikuchi patterns of variable resolution. The approach shows noise levels near <span><math><mrow><mn>1</mn><mo>×</mo><mn>1</mn><msup><mrow><mn>0</mn></mrow><mrow><mo>−</mo><mn>4</mn></mrow></msup></mrow></math></span> in the relative deviatoric strain norm and in the relative rotation angles on nominally strain-free regions of the silicon wafer. The strain and rotation measurements are interpreted by finite element simulations. While confirming the basic findings of previously published studies, the present approach enables a potential reduction in the necessary pattern data size by about two orders of magnitude. We estimate that pattern resolutions in the order of 256 × 256 pixels should be enough to solve a majority of EBSD analysis tasks using pattern matching techniques.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114180"},"PeriodicalIF":2.1,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144291263","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Measurement of electron beam induced sample heating in SEM experiments","authors":"Christina Koenig,&nbsp;Alice Bastos da Silva Fanta,&nbsp;Joerg R. Jinschek","doi":"10.1016/j.ultramic.2025.114195","DOIUrl":"10.1016/j.ultramic.2025.114195","url":null,"abstract":"<div><div>Scanning Electron Microscopy (SEM) experiments provide detailed insights into material microstructures, enabling high-resolution imaging as well as crystallographic analysis through advanced techniques like Electron Backscatter Diffraction (EBSD). However, the interaction of the high-energy electron beam with the material can lead to localized heating, which may significantly impact specimen integrity, especially in applications requiring prolonged beam exposure, for instance when mapping the crystal structure using EBSD. This study examines electron-beam-induced heating effects on a model metal sample (iron), directly measuring the locally deposited electron beam energy with a MEMS-based heating device and validating these measurements through simulations, including Monte Carlo and Finite Element methods. The analysis focuses on the effects of various experimental parameters such as acceleration voltage (from 5 to 30 kV), beam current (from 0.17 nA to 22 nA), dwell time (from 1µs to 1 ms) and sample tilt (0° to 70°). The findings reveal that local sample temperatures can increase by up to 70 °C during EBSD experiments, primarily affected by the choice in beam current and acceleration voltage, with beam current having the most significant impact.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114195"},"PeriodicalIF":2.1,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144271069","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"SEM characterization technique for air-sensitive all-solid-state lithium battery materials","authors":"Hongmin Zhou ,&nbsp;Zhenqi Gu ,&nbsp;Ming Li ,&nbsp;Minghui Fan ,&nbsp;Zhi Zhao ,&nbsp;Shengquan Fu ,&nbsp;Kai Wang","doi":"10.1016/j.ultramic.2025.114194","DOIUrl":"10.1016/j.ultramic.2025.114194","url":null,"abstract":"<div><div>Scanning electron microscopy (SEM) is an important tool for investigating the surface morphologies, chemical compositions, and failure mechanisms of functional materials. However, the microstructures of some materials change during the transfer to SEM, resulting in the inability to characterize them accurately because of the air-sensitive nature of the materials (e.g., battery materials and active metals). Herein, we have designed an airtight transfer box that is simple and feasible for the SEM characterization of air-sensitive materials, realizing that air-sensitive materials are not exposed to air throughout the transfer process. In addition, the ratio of the cathode active material to solid-state electrolytes in the composite cathode of all-solid-state lithium batteries is nondestructively investigated using an airtight transfer box, providing theoretical guidance for the design of high-specific energy composite cathodes.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114194"},"PeriodicalIF":2.1,"publicationDate":"2025-06-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144254183","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"SEM manual rotary holder enhancing sample stability equipped with entomological pin adapter","authors":"Artur Taszakowski ,&nbsp;Ariel Marchlewicz","doi":"10.1016/j.ultramic.2025.114193","DOIUrl":"10.1016/j.ultramic.2025.114193","url":null,"abstract":"<div><div>We present an SEM manual rotary holder equipped with an entomological pin adapter, which allows the free rotation of samples in three axes and guarantees appropriate stability. During imaging, the presented device allows for increased safety when working with fragile and valuable specimens (e.g., holotypes) while maintaining parameters at least as good as previously used techniques. The design of the solution allows it to be integrated with many SEM systems and commercial adapters, significantly increasing its usefulness and versatility. Simultaneously, it does not require additional accessories for manipulation during operation. Additionally, learning to use the proposed solution requires only minor experience. An interesting additional application of the SEM manual rotary holder is its possible usage in other microscopy systems, such as stereoscopic microscopes or even for sample preparation purposes for holding samples.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114193"},"PeriodicalIF":2.1,"publicationDate":"2025-06-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144263511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"CNT-PVP field electron source formed by thermo-mechanical pulling of carbon nanotubes","authors":"Paweł Urbański,&nbsp;Piotr Szyszka,&nbsp;Tomasz Grzebyk","doi":"10.1016/j.ultramic.2025.114183","DOIUrl":"10.1016/j.ultramic.2025.114183","url":null,"abstract":"<div><div>The article presents a novel nanomaterial-based field electron source intended for use in MEMS (microelectromechanical system). The emitter structure consists of a composite of carbon nanotubes (CNTs) and cross-linked polyvinyl-pyrrolidone (PVP). Its production process is based on the thermo-mechanical extraction method. This source is characterized by a low threshold voltage, high current, high thermal resistance and the possibility of uninterrupted operation for many hours. Due to their ease of forming and high thermal resistance, CNT-PVP composites are perfect as electron sources for MEMS systems. Such emitters perfectly withstand the conditions of anodic bonding without compromising their emission properties after the process.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114183"},"PeriodicalIF":2.1,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144263512","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Transmission electron microscope with a mirror objective free of spherical and axial chromatic aberrations","authors":"S.B. Bimurzaev,&nbsp;Z.S. Sautbekova","doi":"10.1016/j.ultramic.2025.114168","DOIUrl":"10.1016/j.ultramic.2025.114168","url":null,"abstract":"<div><div>The basic scheme of a transmission electron microscope (TEM) with a mirror objective free of spherical and axial chromatic aberrations, which are the main factors limiting the resolution of electron microscopes, is considered. As an objective, an axisymmetric electrostatic mirror (ASEM), the electrodes of which are coaxial cylinders of equal diameter, separated by gaps of finite width, is considered. Based on previously developed aberration concepts, taking into account relativistic effects, the families of three-electrode ASEM are calculated that satisfy the condition of eliminating spherical and axial chromatic aberrations simultaneously at a fixed focal length and a finite width of the interelectrode gaps. From the whole variety of theoretical data, mirrors have been identified that are most suitable for practical use as an aberration-free TEM mirror objective, the geometric and electrical parameters of which ensure the formation of Gaussian planes of the object and the image outside the mirror field. The dependences of the geometric and electrical parameters of such a mirror objective on the energy of the illuminating beam of relativistic electrons are presented.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114168"},"PeriodicalIF":2.1,"publicationDate":"2025-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144471693","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Multiscale characterization of nanomechanical behavior and dislocation mechanisms in Cantor CrMnFeCoNi HEA using 3D EBSD and atomistic modeling","authors":"M.A. Stróżyk,&nbsp;F.J. Domínguez-Gutiérrez,&nbsp;K. Mulewska,&nbsp;I. Jóźwik","doi":"10.1016/j.ultramic.2025.114184","DOIUrl":"10.1016/j.ultramic.2025.114184","url":null,"abstract":"<div><div>High-entropy alloys (HEAs) are an emerging class of materials renowned for their exceptional mechanical strength, hardness, and resistance to corrosion and irradiation, making them promising candidates for applications in extreme operating conditions. In this study, the nanomechanical response of a single-grain Cantor CrMnFeCoNi HEA, synthesized in-house, is investigated through nanoindentation testing and characterized using three-dimensional Electron Backscatter Diffraction (3D EBSD) reconstruction. This advanced technique enables high-resolution mapping of geometrically necessary dislocation (GND) density and grain reference orientation deviation (GROD) angles, providing critical insights into localized deformation features and strain gradients. To complement the experimental observations, molecular dynamics (MD) simulations were employed to capture atomistic-scale structural responses, achieving qualitative agreement with mesoscale experimental findings. The integration of 3D EBSD and MD simulations underscores the synergy between advanced experimental characterization and computational modeling, revealing complex dislocation nucleation and evolution mechanisms during nanoindentation. This study highlights the potential of combined multiscale approaches to deepen our understanding of deformation phenomena in HEAs.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114184"},"PeriodicalIF":2.1,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144241238","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chromatic aberration (Cc) corrected cryo-EM: The structure of pseudorabies virus (PRV) using both zero-loss and energy loss electrons","authors":"J. Wu ,&nbsp;C. Liu ,&nbsp;A.J. Wang ,&nbsp;Y.Z. Gao ,&nbsp;L.T. Fu ,&nbsp;Z. Liu ,&nbsp;J.L. Dickerson ,&nbsp;C.J. Russo ,&nbsp;P. Wang","doi":"10.1016/j.ultramic.2025.114182","DOIUrl":"10.1016/j.ultramic.2025.114182","url":null,"abstract":"<div><div>Here we have investigated the potential improvement in imaging vitrified biological specimens with the help of a chromatic aberration (Cc)-corrector. Using a newly developed chromatic aberration-corrected electron cryomicroscope (cryo-EM), the phase contrast micrographs comprising signals from both the zero loss and low energy loss (1-100 eV) channels were used to determine the structure of a pseudorabies virus (PRV). Using an energy selecting, electron energy loss spectrometer after the Cc corrector, datasets were collected separately yet sequentially on the same specimen to allow quantification of the signal in each of the respective channels. Both zero-loss first and low-loss first datasets were acquired. For further comparison, datasets from non-Cc-corrected cryo-EM were also collected. 3D reconstructions of the virus from all 4 above datasets are presented including two maps reconstructed only from electrons having lost 18-28 eV of energy whilst transiting the specimen. Although the amplitude contrast of the signals in the low-loss micrographs is opposite in sign to that of typical defocused images using only elastically scattered electrons, we show that the inelastic maps also contain detailed structural information which can be recovered using Cc correction. This can be verified by comparing the maps from each of the channels. Interestingly, the resolution of the reconstructed volume from the low-loss electrons decreases with defocus independently of the purely elastic electron images taken from the same specimen, which is consistent with previous theoretical predictions and experimental measurements of specimen induced decoherence using room temperature test specimens. Together, these results indicate that the inelastically scattered electrons do indeed contain useful phase contrast signals, particularly for thick specimens, but their recovery requires imaging as close to in-focus as possible. Combing the optical correction demonstrated here, with a lossless phase plate for in focus imaging, may offer the most straightforward way to achieve this in the future.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114182"},"PeriodicalIF":2.1,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144241239","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of an image-forming system for the magnetic field-free electron microscope","authors":"T. Maekawa ,&nbsp;Y. Kohno ,&nbsp;A. Yasuhara ,&nbsp;S. Morishita ,&nbsp;T. Inoue ,&nbsp;Y. Ueda ,&nbsp;K. Arakawa","doi":"10.1016/j.ultramic.2025.114181","DOIUrl":"10.1016/j.ultramic.2025.114181","url":null,"abstract":"<div><div>The successful development of a magnetic field-free objective lens for high-resolution imaging has enabled the acquisition of atomic-resolution scanning transmission electron microscopy (STEM) images under magnetic field-free conditions around the sample. Utilizing this magnetic field-free objective lens for conventional transmission electron microscopy (TEM) observations is expected to offer advantages for the comprehensive characterization of magnetic materials. This approach is particularly significant in the context of <em>in-situ</em> observations. To obtain conventional TEM images, such as bright- and dark-field images, it is important to position the objective lens aperture in a diffraction plane, typically the back focal plane of the objective lens. However, positioning the objective lens aperture around the back focal plane, which is surrounded by multiple magnetic poles, is not feasible for the magnetic field-free objective lens. In this study, we describe the development of an image-forming system that can position the aperture in a diffraction plane conjugate to the back focal plane. In addition, the development of a wide-gap pole piece for the magnetic field-free objective lens has enabled the use of sample holders with thick tips for <em>in-situ</em> observations. The magnetic field-free electron microscope, which integrates a newly developed pole piece and image-forming system with higher-order aberration correctors, offers not only atomic-resolution TEM/STEM observations but also a versatile approach for the characterization of magnetic materials in a magnetic field-free environment.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114181"},"PeriodicalIF":2.1,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144205703","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}