Pub Date : 2025-07-05DOI: 10.1016/j.ultramic.2025.114202
Caleb Whittier , Nabil D. Bassim
Scanning transmission electron microscopy (STEM) allows for high spatial-resolution analysis of materials and, when coupled with electron energy loss spectroscopy (EELS), becomes capable of providing substantial insight into both chemical and optical properties. In recent years, focus has moved towards understanding material properties at the atomic level using EELS. However, there are still significant barriers when attempting to perform high-energy resolution monochromated STEM-EELS analysis on large structures. Off-axis distortions cause additional aberrations to couple into the spectrometer when scanning across large regions. This often limits STEM-EELS mapping to small areas to maintain the energy resolution or requires sacrificing this resolution to spectrum maps spanning multiple microns. We propose here a methodology enabling low-loss STEM-EELS spectrum mapping to be performed over tens to hundreds of microns while maintaining high energy-resolution through modification of the EELS collection conditions. This is accomplished not only through careful alignment of the scan/descan coils, but, more importantly, through implementation of elongated camera lengths that effectively magnify the object over the EELS entrance aperture, cutting out higher order aberrations and reducing shifts on the spectrometer.
{"title":"High-energy resolution monochromated STEM-EELS mapping across large areas","authors":"Caleb Whittier , Nabil D. Bassim","doi":"10.1016/j.ultramic.2025.114202","DOIUrl":"10.1016/j.ultramic.2025.114202","url":null,"abstract":"<div><div>Scanning transmission electron microscopy (STEM) allows for high spatial-resolution analysis of materials and, when coupled with electron energy loss spectroscopy (EELS), becomes capable of providing substantial insight into both chemical and optical properties. In recent years, focus has moved towards understanding material properties at the atomic level using EELS. However, there are still significant barriers when attempting to perform high-energy resolution monochromated STEM-EELS analysis on large structures. Off-axis distortions cause additional aberrations to couple into the spectrometer when scanning across large regions. This often limits STEM-EELS mapping to small areas to maintain the energy resolution or requires sacrificing this resolution to spectrum maps spanning multiple microns. We propose here a methodology enabling low-loss STEM-EELS spectrum mapping to be performed over tens to hundreds of microns while maintaining high energy-resolution through modification of the EELS collection conditions. This is accomplished not only through careful alignment of the scan/descan coils, but, more importantly, through implementation of elongated camera lengths that effectively magnify the object over the EELS entrance aperture, cutting out higher order aberrations and reducing shifts on the spectrometer.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114202"},"PeriodicalIF":2.1,"publicationDate":"2025-07-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144597064","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}
Pub Date : 2025-07-01DOI: 10.1016/j.ultramic.2025.114203
Ujjval Bansal , Amit Sharma , Barbara Putz , Christoph Kirchlechner , Subin Lee
Four-dimensional scanning transmission electron microscopy (4D-STEM) is a powerful tool that allows for the simultaneous acquisition of spatial and diffraction information, driven by recent advancements in direct electron detector technology. Although 4D-STEM has been predominantly developed for and used in conventional TEM and STEM, efforts are being made to implement the technique in scanning electron microscopy (SEM). In this paper, we push the boundaries of 4D-STEM in SEM and extend its capabilities in three key aspects: (1) faster acquisition rate with reduced data size, (2) higher angular resolution, and (3) application to various materials including conventional alloys and focused ion beam (FIB) lamella. Specifically, operating the MiniPIX Timepix3 detector in the event-driven mode significantly improves the acquisition rate by a factor of a few tenths compared to conventional frame-based mode, thereby opening up possibilities for integrating 4D-STEM into various in situ SEM testing. Furthermore, with a novel stage-detector geometry, a camera length of 160 mm is achieved which improves the angular resolution amplifying its utility, for example, magnetic or electric field imaging. Lastly, we successfully imaged a nanostructured platinum-copper thin film with a grain size of 16 nm and a thickness of 20 nm, and identified annealing twins in FIB-prepared polycrystalline copper using virtual dark-field imaging and orientation mapping. This work demonstrates the potential of synergetic combination of 4D-STEM with in situ experiments, and broadening its applications across a wide range of materials.
{"title":"Data-efficient 4D-STEM in SEM: Beyond 2D materials to metallic materials","authors":"Ujjval Bansal , Amit Sharma , Barbara Putz , Christoph Kirchlechner , Subin Lee","doi":"10.1016/j.ultramic.2025.114203","DOIUrl":"10.1016/j.ultramic.2025.114203","url":null,"abstract":"<div><div>Four-dimensional scanning transmission electron microscopy (4D-STEM) is a powerful tool that allows for the simultaneous acquisition of spatial and diffraction information, driven by recent advancements in direct electron detector technology. Although 4D-STEM has been predominantly developed for and used in conventional TEM and STEM, efforts are being made to implement the technique in scanning electron microscopy (SEM). In this paper, we push the boundaries of 4D-STEM in SEM and extend its capabilities in three key aspects: (1) faster acquisition rate with reduced data size, (2) higher angular resolution, and (3) application to various materials including conventional alloys and focused ion beam (FIB) lamella. Specifically, operating the MiniPIX Timepix3 detector in the event-driven mode significantly improves the acquisition rate by a factor of a few tenths compared to conventional frame-based mode, thereby opening up possibilities for integrating 4D-STEM into various <em>in situ</em> SEM testing. Furthermore, with a novel stage-detector geometry, a camera length of 160 mm is achieved which improves the angular resolution amplifying its utility, for example, magnetic or electric field imaging. Lastly, we successfully imaged a nanostructured platinum-copper thin film with a grain size of 16 nm and a thickness of 20 nm, and identified annealing twins in FIB-prepared polycrystalline copper using virtual dark-field imaging and orientation mapping. This work demonstrates the potential of synergetic combination of 4D-STEM with <em>in situ</em> experiments, and broadening its applications across a wide range of materials.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114203"},"PeriodicalIF":2.1,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144580153","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}
Pub Date : 2025-07-01DOI: 10.1016/j.ultramic.2025.114204
Chen Wang , Shaoshan Wang , Chuan Guo , Chengjian Yu , Qi Fu , Xiaopeng Xie , Changxi Zheng
Quantum materials exhibit phases such as superconductivity at low temperatures, yet imaging their phase transition dynamics with high spatial resolution remains challenging due to conventional tools' limitations—scanning tunneling microscopy offers static snapshots, while transmission electron microscopy lacks band sensitivity. Photoemission electron microscopy (PEEM) can resolve band structures in real/reciprocal spaces rapidly, but suffering from insufficient resolution for (near)atomic-scale quantum physics due to the unstable cooling designs. Here, we developed cryogen-free low-temperature PEEM (CFLT-PEEM) achieving 21.1 K stably. CFLT-PEEM attains a record-breaking resolution of 4.48 nm without aberration correction, enabling direct visualization of surface-state distribution characteristics along individual atomic steps. The advancement lies in narrowing the segment of band structures for imaging down to 160 meV, which minimizes the chromatic aberration of PEEM. CFLT-PEEM enables rapid, nondestructive high-resolution imaging of cryogenic electronic structures, positioning it as a powerful tool for physics and beyond.
{"title":"Cryogen-free low-temperature photoemission electron microscopy for high-resolution nondestructive imaging of electronic phases","authors":"Chen Wang , Shaoshan Wang , Chuan Guo , Chengjian Yu , Qi Fu , Xiaopeng Xie , Changxi Zheng","doi":"10.1016/j.ultramic.2025.114204","DOIUrl":"10.1016/j.ultramic.2025.114204","url":null,"abstract":"<div><div>Quantum materials exhibit phases such as superconductivity at low temperatures, yet imaging their phase transition dynamics with high spatial resolution remains challenging due to conventional tools' limitations—scanning tunneling microscopy offers static snapshots, while transmission electron microscopy lacks band sensitivity. Photoemission electron microscopy (PEEM) can resolve band structures in real/reciprocal spaces rapidly, but suffering from insufficient resolution for (near)atomic-scale quantum physics due to the unstable cooling designs. Here, we developed cryogen-free low-temperature PEEM (CFLT-PEEM) achieving 21.1 K stably. CFLT-PEEM attains a record-breaking resolution of 4.48 nm without aberration correction, enabling direct visualization of surface-state distribution characteristics along individual atomic steps. The advancement lies in narrowing the segment of band structures for imaging down to 160 meV, which minimizes the chromatic aberration of PEEM. CFLT-PEEM enables rapid, nondestructive high-resolution imaging of cryogenic electronic structures, positioning it as a powerful tool for physics and beyond.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"277 ","pages":"Article 114204"},"PeriodicalIF":2.1,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144614592","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}
Pub Date : 2025-06-28DOI: 10.1016/j.ultramic.2025.114192
Sheikh Shah Mohammad Motiur Rahman , Michel Salomon , Sounkalo Dembélé
This paper introduces a framework (EstimateNoiseSEM) to automate noise estimation in scanning electron microscopy (SEM) images. Within this framework, a classification network selection mechanism facilitates the choice of a more optimized classification approach. Consequently, the classification stage determines the image’s noise type, while the regression model predicts the corresponding noise level. Noise estimation, which includes the noise type and level, is necessary to perform denoising in most cases. This study targeted the noise in scanning electron microscopy (SEM) images. Indeed, depending on the dwell time, the SEM produces different types of noise (Gaussian or Gamma) that can pose uncertainty problems during denoising. That is why, the multi-stage scheme based on deep learning was proposed in this study. The proposed approach performed better in Gaussian noise classification with more than 80% Accuracy, Precision, Recall, and F1-score on synthetic noisy samples and 0.98+/-0.01 root squared error in Gaussian noise classification. The classification network once achieved 97% of accuracy for Gaussian noise classification which decreased to 80% later on because of the uncertainty of Gamma noise levels. However, this study also provides detailed insights into the Gamma noise estimation process. These insights may guide us or the community in developing deep learning-based Gamma noise estimation techniques.
{"title":"EstimateNoiseSEM: A novel framework for deep learning based noise estimation of scanning electron microscopy images","authors":"Sheikh Shah Mohammad Motiur Rahman , Michel Salomon , Sounkalo Dembélé","doi":"10.1016/j.ultramic.2025.114192","DOIUrl":"10.1016/j.ultramic.2025.114192","url":null,"abstract":"<div><div>This paper introduces a framework (EstimateNoiseSEM) to automate noise estimation in scanning electron microscopy (SEM) images. Within this framework, a classification network selection mechanism facilitates the choice of a more optimized classification approach. Consequently, the classification stage determines the image’s noise type, while the regression model predicts the corresponding noise level. Noise estimation, which includes the noise type and level, is necessary to perform denoising in most cases. This study targeted the noise in scanning electron microscopy (SEM) images. Indeed, depending on the dwell time, the SEM produces different types of noise (Gaussian or Gamma) that can pose uncertainty problems during denoising. That is why, the multi-stage scheme based on deep learning was proposed in this study. The proposed approach performed better in Gaussian noise classification with more than 80% Accuracy, Precision, Recall, and F1-score on synthetic noisy samples and 0.98+/-0.01 root squared error in Gaussian noise classification. The classification network once achieved 97% of accuracy for Gaussian noise classification which decreased to 80% later on because of the uncertainty of Gamma noise levels. However, this study also provides detailed insights into the Gamma noise estimation process. These insights may guide us or the community in developing deep learning-based Gamma noise estimation techniques.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114192"},"PeriodicalIF":2.1,"publicationDate":"2025-06-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144518010","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}
Pub Date : 2025-06-21DOI: 10.1016/j.ultramic.2025.114191
Laura Niermann
Modern semiconductor devices require control of the electrostatic potential landscape at nanometer scale, which is especially important for materials like the Group III-Nitrides, where polarization effects cause additional sheet charges at interfaces. In this work two complementary electron microscopic methods, differential phase contrast (DPC) and electron holography (EH), are used for characterization of a GaN p–n junction in one and the same sample. In comparison, the values obtained for the junction’s characteristics, like the built-in potential step, the maximum fields strength, and the width of the space charge region, were significantly larger and also closer to the expected values, when measured by means of EH. A key difference in the measurements is the vastly lower illumination dose rates within the EH experiments. Therefore, the lower generation rate of electron–hole pairs might lead to a lower beam induced bias during the EH measurement. These findings demonstrate that in future experiments the impact of the electron illumination must be considered for accurate nanoscale electrostatic field and potential measurements.
{"title":"Differences between differential phase contrast and electron holographic measurements of a GaN p-n junction","authors":"Laura Niermann","doi":"10.1016/j.ultramic.2025.114191","DOIUrl":"10.1016/j.ultramic.2025.114191","url":null,"abstract":"<div><div>Modern semiconductor devices require control of the electrostatic potential landscape at nanometer scale, which is especially important for materials like the Group III-Nitrides, where polarization effects cause additional sheet charges at interfaces. In this work two complementary electron microscopic methods, differential phase contrast (DPC) and electron holography (EH), are used for characterization of a GaN p–n junction in one and the same sample. In comparison, the values obtained for the junction’s characteristics, like the built-in potential step, the maximum fields strength, and the width of the space charge region, were significantly larger and also closer to the expected values, when measured by means of EH. A key difference in the measurements is the vastly lower illumination dose rates within the EH experiments. Therefore, the lower generation rate of electron–hole pairs might lead to a lower beam induced bias during the EH measurement. These findings demonstrate that in future experiments the impact of the electron illumination must be considered for accurate nanoscale electrostatic field and potential measurements.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"276 ","pages":"Article 114191"},"PeriodicalIF":2.1,"publicationDate":"2025-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144338804","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}
Pub Date : 2025-06-17DOI: 10.1016/j.ultramic.2025.114201
Roberto Conconi , María del Mar Abad Ortega , Fernando Nieto , Paolo Buono , Giancarlo Capitani
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 k-factors can exist, but only k-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 kO/Si factors, one for lighter and one for denser compounds.
采用Cliff和Lorimer近似法和基于电中性的吸收校正法两种基于已知组分标准的TEM-EDS定量方法,并比较了三种不同tem和EDS体系的结果。这三种TEM仪器在源类型(场发射vs热离子)、加速电压(200 vs 300 kV)和EDS系统类型(4列硅漂移检测器(SDD) vs单列SDD)上有所不同。我们发现EDS校准似乎是“严格特定于仪器”,即不存在普遍有效的k因子,而只有特定显微镜和EDS系统组合的k因子集。正如预期的那样,4-in柱SDD系统,由于与传统的单SDD相比具有更大的敏感区域,因此在数据收集方面更有效,因此具有更低的检测限。但是,其他错误来源可能会影响最终输出,有时会破坏预期。用feg - tem进行的EDS分析显示,弱边界元素的辐射诱导迁移比配备常规源和较低光束电流的tem低。这一结果可以解释为使用传统TEM的光斑尺寸较小,总的来说导致每个样品原子的电子剂量较高。此外,这项工作证实了吸收校正方法在处理厚和/或致密样品时是首选的,而Cliff和Lorimer近似在所有其他情况下都更简单,更快。最后,我们重申有必要确定两个不同的kO/Si因子,一个用于较轻的化合物,一个用于较致密的化合物。
{"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}
Pub Date : 2025-06-17DOI: 10.1016/j.ultramic.2025.114200
Saeideh Naghdali , Maximilian Schiester , Helene Waldl , Velislava Terziyska , Marcus Hans , Daniel Primetzhofer , Nina Schalk , Michael Tkadletz
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 15N-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) 15N-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.
{"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}
Pub Date : 2025-06-16DOI: 10.1016/j.ultramic.2025.114197
Yi Zheng, Léon Sanche
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.
{"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}
Pub Date : 2025-06-16DOI: 10.1016/j.ultramic.2025.114199
Olha Khshanovska, Aleksandr Kryshtal
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.
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.
{"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}
Pub Date : 2025-06-11DOI: 10.1016/j.ultramic.2025.114196
E.I. Rau, S.V. Zaitsev
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 EB.
The obtained expressions give more precisely data of η than all previous publications in the wide energy range EB 1–30 keV. They were used to describe the dependence of the BSE signal IS from atomic number of the target material Z and SEM accelerating voltage EB. The image contrast as a function of Z -differences and EB is considered. Particular attention is paid to the influence of the response function F on the formation of the IS 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.
{"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}