UltramicroscopyPub Date : 2025-03-04DOI: 10.1016/j.ultramic.2025.114119
Thibaud Denneulin, Benjamin Zingsem, Joseph Vas, Wen Shi, Luyan Yang, Michael Feuerbacher, Rafal E. Dunin-Borkowski
{"title":"Acquisition of object and temperature series in medium resolution off-axis electron holography with live drift correction","authors":"Thibaud Denneulin, Benjamin Zingsem, Joseph Vas, Wen Shi, Luyan Yang, Michael Feuerbacher, Rafal E. Dunin-Borkowski","doi":"10.1016/j.ultramic.2025.114119","DOIUrl":"10.1016/j.ultramic.2025.114119","url":null,"abstract":"<div><div>Collecting and averaging large datasets is a common practice in transmission electron microscopy to improve the signal-to-noise ratio. Averaging data in off-axis electron holography requires automated tools capable of correcting both the drift of the interference fringes and the drift of the specimen. This can be achieved either off-line, by post-processing hologram series, or on-line, through real-time microscope control. For on-line correction, a previously suggested method involves independently adjusting the position of the intereference fringes and the sample by controlling the beam tilt coils and the stage during hologram acquisition. In this study, we have implemented this on-line correction method in a Thermo Fisher Scientific Titan transmission electron microscope. The microscope is equipped with a piezo-enhanced CompuStage for positioning the sample with high precision. However, the control of the piezo stage via direct scripting is not supported. We first describe a workaround to enable automated sample position correction. We then demonstrate the benefits of live, program-controlled acquisitions for serial experiments in medium resolution off-axis electron holography. Application examples include the automatic acquisition of an object series such as a transistor array and an <em>in-situ</em> temperature series of magnetic skyrmions.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114119"},"PeriodicalIF":2.1,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143593126","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-02-27DOI: 10.1016/j.ultramic.2025.114124
Hannah R. Johnson, Legend Foster, Anikin Rae Domingo, Gregory P. Holland
{"title":"Negative stain TEM imaging of native spider silk protein superstructures","authors":"Hannah R. Johnson, Legend Foster, Anikin Rae Domingo, Gregory P. Holland","doi":"10.1016/j.ultramic.2025.114124","DOIUrl":"10.1016/j.ultramic.2025.114124","url":null,"abstract":"<div><div>Native <em>Latrodectus hesperus</em> (black widow) major ampullate spider silk proteins were imaged using negative stain transmission electron microscopy (NS-TEM) by isolating the silk protein hydrogel directly from the organism and solubilizing in urea. Heterogeneous micelle-like structures averaging 300 nm, similar to those imaged previously with CryoEM, were observed when stained with ammonium molybdate. A second smaller population averaging 50 nm was observed as well as large fibrils, highlighting the heterogeneous nature of the silk gland. The population of smaller silk protein micelles was enhanced at higher urea concentrations (5–8 M). This was further supported by dynamic light scattering (DLS), where two populations were observed at low urea concentrations while one small population dominated at high urea concentrations. The approach presented here provides a cost-effective route to imaging silk protein superstructures with conventional NS-TEM methods and may be applicable to other soft nanoparticle systems.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114124"},"PeriodicalIF":2.1,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143580328","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-02-24DOI: 10.1016/j.ultramic.2025.114120
William J. Davids, Mengwei He, Huma Bilal, Andrew J. Breen, Simon P. Ringer
{"title":"Using non-parametric statistical testing to quantify solute clustering in atom probe reconstructions","authors":"William J. Davids, Mengwei He, Huma Bilal, Andrew J. Breen, Simon P. Ringer","doi":"10.1016/j.ultramic.2025.114120","DOIUrl":"10.1016/j.ultramic.2025.114120","url":null,"abstract":"<div><div>Atom probe tomography (APT) is routinely used to investigate nano-scale solute architecture within multicomponent systems. However, there is no consensus on how to best quantify solute clustering within APT data. This contribution leverages recent developments in the field of non-parametric hypothesis testing of nearest-neighbour distributions to address this critical gap. We adapt a goodness-of-fit-type test statistic known as ‘the level of heterogeneity’ to quantitatively discern whether solute distributions exhibit clustering behaviour beyond what would be expected from a random distribution. Further, comparing APT datasets remains difficult due to the inability to directly compare their nearest-neighbour distributions. We present a method that leverages Monte-Carlo simulations, already used to calculate the non-parametric statistic, as a means of comparing APT data. The method is more powerful than comparing datasets through the Pearson coefficient, as is conventionally done.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114120"},"PeriodicalIF":2.1,"publicationDate":"2025-02-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143548520","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-02-16DOI: 10.1016/j.ultramic.2025.114118
Robert M. Glaeser
{"title":"Commonsense and common nonsense opinions: PROSPECTS for further reducing beam damage in electron microscopy of radiation-sensitive specimens","authors":"Robert M. Glaeser","doi":"10.1016/j.ultramic.2025.114118","DOIUrl":"10.1016/j.ultramic.2025.114118","url":null,"abstract":"<div><div>Biological molecules are easily damaged by high-energy electrons, thus limiting the exposures that can be used to image such specimens by electron microscopy. It is argued here that many-electron, volume-plasmon excitations, which promptly transition into multiple types of single-electron ionization and excitation events, seem to be the predominant cause of damage in such materials. Although reducing the rate at which primary radiolysis occurs would allow one to record images that were much less noisy, many novel proposals for achieving this are unlikely to be realized in the near future, while others are manifestly ill-founded. As a result, the most realistic option currently is to more effectively use the available “budget” of electron exposure, i.e. to further improve the “dose efficiency” by which images are recorded. While progress in that direction is currently under way for both “conventional” (i.e. fixed-beam) and scanning EM, the former is expected to set a high standard for the latter to surpass.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114118"},"PeriodicalIF":2.1,"publicationDate":"2025-02-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143511910","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-02-16DOI: 10.1016/j.ultramic.2025.114117
Peter S. Neu , Eugene E. Krasovskii , Rudolf M. Tromp , Sense Jan van der Molen
{"title":"Bi-directional LEEM and eV-TEM spectroscopy on a graphene-hBN heterostack","authors":"Peter S. Neu , Eugene E. Krasovskii , Rudolf M. Tromp , Sense Jan van der Molen","doi":"10.1016/j.ultramic.2025.114117","DOIUrl":"10.1016/j.ultramic.2025.114117","url":null,"abstract":"<div><div>Van der Waals heterostacks can exhibit emergent properties as a result of the coupling between the individual layers stacked. Here we focus on heterostacks of graphene and hBN, and study both coherent electron resonances (or unoccupied states) and inelastic losses. For this, we measure electron reflection and transmission spectra of the stack, as a function of electron energy. Special attention is paid to the symmetry upon flipping the heterostack, i.e., whether the electrons are first incident on the graphene or on the hBN surface: whereas electron reflection may be sensitive to sample orientation, electron transmission should not. Experimentally, we compare LEEM (reflection) and eV-TEM (transmission) IV spectra measured on free-standing graphene-hBN heterostacks with either the graphene or hBN side facing the LEEM objective lens. Resonances and inelastic loss are first modeled with the help of a simple wave interference toy model inspired by optics. More advanced calculations are performed to obtain the spatially resolved density of unoccupied states in the heterostack. We relate these calculations to the measured spectra, taking into account the finite probing depth of the reflected electron beam.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114117"},"PeriodicalIF":2.1,"publicationDate":"2025-02-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143600543","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-02-09DOI: 10.1016/j.ultramic.2025.114115
Bavley Guerguis , Ramya Cuduvally , Richard J.H. Morris , Gabriel Arcuri , Brian Langelier , Nabil Bassim
{"title":"Erratum to \"The impact of electric field strength on the accuracy of boron dopant quantification in silicon using atom probe tomography\"","authors":"Bavley Guerguis , Ramya Cuduvally , Richard J.H. Morris , Gabriel Arcuri , Brian Langelier , Nabil Bassim","doi":"10.1016/j.ultramic.2025.114115","DOIUrl":"10.1016/j.ultramic.2025.114115","url":null,"abstract":"","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"271 ","pages":"Article 114115"},"PeriodicalIF":2.1,"publicationDate":"2025-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143400325","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-01-17DOI: 10.1016/j.ultramic.2025.114105
Maximilian Schiester , Helene Waldl , Katherine P. Rice , Marcus Hans , Daniel Primetzhofer , Nina Schalk , Michael Tkadletz
{"title":"Effects of laser wavelength and pulse energy on the evaporation behavior of TiN coatings in atom probe tomography: A multi-instrument study","authors":"Maximilian Schiester , Helene Waldl , Katherine P. Rice , Marcus Hans , Daniel Primetzhofer , Nina Schalk , Michael Tkadletz","doi":"10.1016/j.ultramic.2025.114105","DOIUrl":"10.1016/j.ultramic.2025.114105","url":null,"abstract":"<div><div>The impact of the laser wavelength on accuracy in elemental composition analysis in atom probe tomography (APT) was investigated. Three different commercial atom probe systems — LEAP 3000X HR, LEAP 5000 XR, and LEAP 6000 XR — were systematically compared for a TiN model coating studying the effect of shorter laser wavelengths, especially in the deep ultraviolet (DUV) range, on the evaporation behavior. The findings demonstrate that the use of shorter wavelengths enhances the accuracy in elemental composition, while maintaining similar electric field strengths. Thus, thermal effects are reduced, which in turn improves mass resolving power. An important aspect of this research includes the estimation of energy density ratios of the different instruments. The reduction in wavelength is accompanied by increasing energy densities due to smaller laser spot sizes. Furthermore, advancements in the detector technology were studied. Finally, the detector dead-times were determined and dead-zones were evaluated to investigate the ion pile-up behavior in APT measurements of nitrides with the LEAP 6000 XR.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"270 ","pages":"Article 114105"},"PeriodicalIF":2.1,"publicationDate":"2025-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143012396","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-01-17DOI: 10.1016/j.ultramic.2025.114106
Jennifer L.W. Carter , Tugce Karakulak Uz , Buhari Ibrahim , Jeffrey S. Pigott , Jerard V. Gordon
{"title":"A comparison of energy dispersive spectroscopy in transmission scanning electron microscopy with scanning transmission electron microscopy","authors":"Jennifer L.W. Carter , Tugce Karakulak Uz , Buhari Ibrahim , Jeffrey S. Pigott , Jerard V. Gordon","doi":"10.1016/j.ultramic.2025.114106","DOIUrl":"10.1016/j.ultramic.2025.114106","url":null,"abstract":"<div><div>The objective of this work was to explore the capabilities of a field emission gun scanning electron microscope (FEG-SEM) equipped with a transmission scanning electron detector (TSEM) and energy dispersive spectroscopy (EDS) to identify nanoscale chemical heterogeneities in a gas atomization reaction synthesis (GARS) steel sample. The results of this analysis were compared to the same study conducted with scanning transmission electron microscopy (STEM) with EDS mapping. TSEM-EDS was performed using the standard spectral analysis approach, i.e., pixel-by-pixel identification of elements from the spectra, and a new principal component analysis approach to detect regions of similar spectra before identifying elemental contributions to each spectrum. It was determined that features over 200 nm were detectable with the TSEM-EDS standard spectra analysis technique but the PCA analysis approach was necessary for observing smaller features that contained trace elements. Monte Carlo simulations indicated that the spatial resolution expected from a 150 nm thick foil was consistent with those observed in experimental analysis. Simulations also confirm that thinner samples enable higher spatial resolution scans although smaller interaction volumes may require longer acquisition times.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"270 ","pages":"Article 114106"},"PeriodicalIF":2.1,"publicationDate":"2025-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143041510","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
UltramicroscopyPub Date : 2025-01-13DOI: 10.1016/j.ultramic.2025.114104
Supriya Ghosh, Fengdeng Liu, Sreejith Nair, Rishi Raj, Bharat Jalan, K. Andre Mkhoyan
{"title":"Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM","authors":"Supriya Ghosh, Fengdeng Liu, Sreejith Nair, Rishi Raj, Bharat Jalan, K. Andre Mkhoyan","doi":"10.1016/j.ultramic.2025.114104","DOIUrl":"10.1016/j.ultramic.2025.114104","url":null,"abstract":"<div><div>To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. It is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO<sub>3</sub> grown on a SrTiO<sub>3</sub> substrate and metal oxide IrO<sub>2</sub> on a TiO<sub>2</sub> substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"270 ","pages":"Article 114104"},"PeriodicalIF":2.1,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143012410","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}
UltramicroscopyPub Date : 2025-01-13DOI: 10.1016/j.ultramic.2024.114101
Christian Zietlow, Jörg K.N. Lindner
{"title":"An applied noise model for low-loss EELS maps","authors":"Christian Zietlow, Jörg K.N. Lindner","doi":"10.1016/j.ultramic.2024.114101","DOIUrl":"10.1016/j.ultramic.2024.114101","url":null,"abstract":"<div><div>Electron energy-loss spectroscopy (EELS) performed in a scanning transmission electron microscope (STEM) is susceptible to noise, just like every other measurement. EELS measurements are also affected by signal blurring, related to the energy distribution of the electron beam and the detector point spread function (PSF). Moreover, the signal blurring caused by the detector introduces correlation effects, which smooth the noise. A general understanding of the noise is essential for evaluating the quality of measurements or for designing more effective post-processing techniques such as deconvolution, which especially in the context of EELS is a common practice to enhance signals. Therefore, we offer theoretical insight into the noise smoothing by convolution and characterize the resulting noise correlations by Pearson coefficients. Additional effects play a role in EELS mapping, where multiple spectra are acquired sequentially at various specimen positions. These three-dimensional datasets are affected by energy drifts of the electron beam, causing spectra to shift relative to each other, and by beam current deviations, which alter their relative proportion. We investigate several energy alignment techniques to correct energy drifts on a sub-channel level and describe the intensity normalization necessary to correct for beam current deviations. Both procedures affect noises and uncertainties of the measurement to various degrees. In this paper, we mathematically derive an applied noise model for EELS measurements, which is straightforward to use. Therefore, we provide the necessary methods to determine the most important noise parameters of the EELS detector enabling users to adapt the model. In summary, we aim to provide a comprehensive understanding of the noises faced in EELS and offer the necessary tools to apply this knowledge in practice.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"270 ","pages":"Article 114101"},"PeriodicalIF":2.1,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143012394","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}