Ultramicroscopy最新文献_第4页

TEM-EDS microanalysis: Comparison between different electron sources, accelerating voltages and detection systems TEM-EDS微分析：不同电子源、加速电压和检测系统的比较

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-17 DOI: 10.1016/j.ultramic.2025.114201

Roberto Conconi , María del Mar Abad Ortega , Fernando Nieto , Paolo Buono , Giancarlo Capitani

{"title":"TEM-EDS microanalysis: Comparison between different electron sources, accelerating voltages and detection systems","authors":"Roberto Conconi , María del Mar Abad Ortega , Fernando Nieto , Paolo Buono , Giancarlo Capitani","doi":"10.1016/j.ultramic.2025.114201","DOIUrl":"10.1016/j.ultramic.2025.114201","url":null,"abstract":"<div><div>Two TEM-EDS quantification methods based on standards of known compositions, namely the Cliff and Lorimer approximation and the absorption correction method based on electroneutrality are employed and the results obtained with three different TEMs and EDS systems, compared. The three TEM instruments differ in source type (field emission vs. thermionic), accelerating voltage (200 vs. 300 kV) and EDS system type (4 in-column silicon drift detector (SDD) vs. single SDD). We found that EDS calibration appears to be “strictly instrument specific”, i.e., no universally valid <em>k</em>-factors can exist, but only <em>k</em>-factor sets for a specific combination of microscope and EDS system. As expected, 4-in column SDD systems, because of their larger sensitive areas compared to classical single SDD, are more efficient in data collection and, therefore, have lower detection limits. However, other sources of error may influence the final output, sometimes subverting the expectations. EDS analyses performed with FEG-TEMs exhibit lower radiation-induced migration of weakly bounded elements than TEMs equipped with a conventional source and lower beam current. This result may be explained by the smaller spot size used with the conventional TEM that in total led to a higher electron dose per sample atom. In addition, this work confirms that the absorption correction method is to be preferred whenever dealing with thick and/or dense samples, whereas the Cliff and Lorimer approximation, because simpler and faster, in all the other cases. Finally, we renew the necessity to determine two distinct <em>k<sub>O/Si</sub></em> factors, one for lighter and one for denser compounds.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114201"},"PeriodicalIF":2.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365802","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}

引用次数: 0

Improving the elemental and imaging accuracy in atom probe tomography of (Ti,Si)N single and multilayer coatings using isotopic substitution of N 用N同位素取代提高（Ti,Si）N单层和多层涂层原子探针层析成像的元素和成像精度

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-17 DOI: 10.1016/j.ultramic.2025.114200

Saeideh Naghdali , Maximilian Schiester , Helene Waldl , Velislava Terziyska , Marcus Hans , Daniel Primetzhofer , Nina Schalk , Michael Tkadletz

{"title":"Improving the elemental and imaging accuracy in atom probe tomography of (Ti,Si)N single and multilayer coatings using isotopic substitution of N","authors":"Saeideh Naghdali , Maximilian Schiester , Helene Waldl , Velislava Terziyska , Marcus Hans , Daniel Primetzhofer , Nina Schalk , Michael Tkadletz","doi":"10.1016/j.ultramic.2025.114200","DOIUrl":"10.1016/j.ultramic.2025.114200","url":null,"abstract":"<div><div>This study addresses the challenges in analyzing (Ti,Si)N coatings using atom probe tomography (APT). Overlapping mass-to-charge state ratios in APT mass spectra hinder unambiguous identification of Si and N, thus, isotopic substitution of naturally abundant nitrogen by <sup>15</sup>N-enriched nitrogen was applied to disentangle the mass-spectral overlaps. A series of model coatings, namely, Ti-N, Si-N, and Ti-Si-N single layer coatings were utilized to investigate elemental accuracy, while their corresponding multilayer coatings were used to assess lateral resolution and imaging accuracy. The coatings were sputter-deposited using i) naturally abundant nitrogen and ii) <sup>15</sup>N-enriched nitrogen, respectively. Subsequently, the coatings were analyzed with a LEAP 5000 XR atom probe. Accuracy in obtained concentrations was cross-validated with elastic recoil detection analysis (ERDA) combined with Rutherford backscattering spectrometry (RBS). The investigation showed that isotopic substitution allows to differentiate the Si and N peaks in the mass spectra and significantly reduces compositional discrepancies between APT and ERDA/RBS results. Despite remaining minor peak overlaps, which can result in inaccuracies in determining the elemental composition, isotopic substitution has proven to be an effective method for peak differentiation and correcting the obtained elemental composition of Ti-Si-N. Moreover, isotopic substitution can predominantly increase the elemental accuracy and imaging accuracy of APT measurements of multilayer coatings.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114200"},"PeriodicalIF":2.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365801","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}

引用次数: 0

Can low energy (1–20 eV) electron microscopy produce damage-free images of biological samples? 低能量（1-20 eV）电子显微镜能产生无损伤的生物样品图像吗？

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-16 DOI: 10.1016/j.ultramic.2025.114197

Yi Zheng, Léon Sanche

{"title":"Can low energy (1–20 eV) electron microscopy produce damage-free images of biological samples?","authors":"Yi Zheng, Léon Sanche","doi":"10.1016/j.ultramic.2025.114197","DOIUrl":"10.1016/j.ultramic.2025.114197","url":null,"abstract":"<div><div>Electron microscopy constitutes an efficient and well-established method to visualize biological material on the nanoscale. The image is usually produced by a high energy electron beam, which can damage the biological sample. To reduce image degradation, Neu et al. [Ultramicroscopy 222 (2021) 113,199] recently suggested the possibility of damage-free imaging of such samples at nm resolution using as a probe low energy electron (LEEs). The aims of the present article are to 1) present a simple and short description of LEE inelastic scattering and attachment in molecular solids in the 0–20 eV range, 2) show that principally due to the formation of transient anions (TAs) in biological material, by temporary LEE attachment to molecular sites, damage-free electron microscopy may be difficult to achieve and 3) suggest specimen conditions that reduce the damage produced by TAs to inflict minimum damage to biological samples in LEE microscopy. We provide examples of lesions induced by electrons of energies below 3 eV in short DNA strands composed of 16 base-pair oligonucleotides and on the 1–20 eV dependence of effective damage yields from LEE-bombarded plasmid DNA. The damaged samples were produced from 5-monolayer films lyophilized on tantalum substrates and transferred to ultra-high vacuum to be bombarded with LEEs. The products were identified and quantified ex-vacuo by LC-MS-MS and electrophoresis, respectively. Such effective yields, and the corresponding absolute cross sections derived from model analysis, should allow estimating beam damage and image quality in the visualization of thin biological films by LEE microscopy.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114197"},"PeriodicalIF":2.1,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307813","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}

引用次数: 0

Valence EELS study of the composition of a liquid phase in a Janus Sn-Ge nanoparticle over a temperature range of 250–750 °C 在250-750℃的温度范围内，对Janus Sn-Ge纳米颗粒液相组成的价态EELS研究

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-16 DOI: 10.1016/j.ultramic.2025.114199

Olha Khshanovska, Aleksandr Kryshtal

{"title":"Valence EELS study of the composition of a liquid phase in a Janus Sn-Ge nanoparticle over a temperature range of 250–750 °C","authors":"Olha Khshanovska, Aleksandr Kryshtal","doi":"10.1016/j.ultramic.2025.114199","DOIUrl":"10.1016/j.ultramic.2025.114199","url":null,"abstract":"<div><div>Mapping the composition of liquid alloy nanoparticles in TEM at relatively low electron doses is essential for emerging nanotechnologies. In this work, we used volume and surface plasmon energies to determine the composition across different regions of a single Sn-Ge nanoparticle over a temperature range of 250–750 °C. A 53 nm Janus nanoparticle, composed of liquid Sn and solid Ge sides, was heated in a TEM, inducing the gradual dissolution of Ge into liquid Sn. Low-loss electron energy loss spectral images were acquired at 50 °C intervals, and plasmon energies were accurately measured using model-based fitting.</div><div>We demonstrated that the free-electron gas Drude model, combined with Zen’s law of alloy volume-concentration relation, enables the reliable determination of the composition of liquid Sn-Ge alloy from both surface and volume plasmon energy shifts. The determined compositions of the liquid alloy were consistent with EDX measurements and the liquidus line of the phase diagram. A homogeneous distribution of chemical elements in the liquid Sn-Ge alloy was revealed. At the same time, the composition on the Ge side of the nanoparticle was inhomogeneous, indicating the formation of a thin liquid shell over the solid Ge core. As a result, Ge in the Sn-Ge Janus nanoparticle exhibited highly tunable surface plasmon resonance, with its energy varying between 10.75 and 9.25 eV over a temperature range of 250–750 °C.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114199"},"PeriodicalIF":2.1,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365803","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}

引用次数: 0

Electron backscattering coefficient, material contrast and response function of BSE- detectors in scanning electron microscopy 扫描电镜下BSE-探测器的电子后向散射系数、材料对比和响应函数

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-11 DOI: 10.1016/j.ultramic.2025.114196

E.I. Rau, S.V. Zaitsev

{"title":"Electron backscattering coefficient, material contrast and response function of BSE- detectors in scanning electron microscopy","authors":"E.I. Rau, 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<sub>B</sub>.</div><div>The obtained expressions give more precisely data of η than all previous publications in the wide energy range E<sub>B</sub> 1–30 keV. They were used to describe the dependence of the BSE signal I<sub>S</sub> from atomic number of the target material Z and SEM accelerating voltage E<sub>B</sub>. The image contrast as a function of Z -differences and E<sub>B</sub> is considered. Particular attention is paid to the influence of the response function F on the formation of the I<sub>S</sub> 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}

引用次数: 0

Simulation-based super-resolution EBSD for measurements of relative deformation gradient tensors 基于仿真的超分辨率EBSD相对变形梯度张量测量

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-10 DOI: 10.1016/j.ultramic.2025.114180

Aimo Winkelmann , Grzegorz Cios , Konrad Perzyński , Tomasz Tokarski , Klaus Mehnert , Łukasz Madej , Piotr Bała

{"title":"Simulation-based super-resolution EBSD for measurements of relative deformation gradient tensors","authors":"Aimo Winkelmann , Grzegorz Cios , Konrad Perzyński , Tomasz Tokarski , Klaus Mehnert , Łukasz Madej , 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}

引用次数: 0

Measurement of electron beam induced sample heating in SEM experiments 扫描电镜实验中电子束诱导样品加热的测量

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-09 DOI: 10.1016/j.ultramic.2025.114195

Christina Koenig, Alice Bastos da Silva Fanta, Joerg R. Jinschek

{"title":"Measurement of electron beam induced sample heating in SEM experiments","authors":"Christina Koenig, Alice Bastos da Silva Fanta, 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}

引用次数: 0

SEM characterization technique for air-sensitive all-solid-state lithium battery materials 气敏全固态锂电池材料的SEM表征技术

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-08 DOI: 10.1016/j.ultramic.2025.114194

Hongmin Zhou , Zhenqi Gu , Ming Li , Minghui Fan , Zhi Zhao , Shengquan Fu , Kai Wang

引用次数: 0

SEM manual rotary holder enhancing sample stability equipped with entomological pin adapter SEM手动旋转支架增强样品稳定性配备昆虫针适配器

IF 2.1 3区工程技术

Ultramicroscopy Pub Date : 2025-06-08 DOI: 10.1016/j.ultramic.2025.114193

Artur Taszakowski , Ariel Marchlewicz

引用次数: 0

CNT-PVP field electron source formed by thermo-mechanical pulling of carbon nanotubes 碳纳米管热机械拉扯形成CNT-PVP场电子源