UltramicroscopyPub Date : 2025-05-03DOI: 10.1016/j.ultramic.2025.114157
Behnam Esmaeilzadeh , Muhammad Touqeer , Syed Asad Maqbool , Jihao Wang , Wenjie Meng , Yubin Hou , Yalin Lu , Qingyou Lu
{"title":"High-precision atomic imaging using an innovative vibration-isolated scanning tunneling microscope","authors":"Behnam Esmaeilzadeh , Muhammad Touqeer , Syed Asad Maqbool , Jihao Wang , Wenjie Meng , Yubin Hou , Yalin Lu , Qingyou Lu","doi":"10.1016/j.ultramic.2025.114157","DOIUrl":"10.1016/j.ultramic.2025.114157","url":null,"abstract":"<div><div>The stability of the scanning unit in a scanning tunneling microscope (STM) is essential for achieving high-resolution imaging. In this study, we present a non-metallic STM with a mechanically isolated scanning unit, ensuring long-term drift stability, low backlash, and high repeatability. By decoupling the piezoelectric scanning tube (PST) from the piezoelectric motor tube (PMT), the design effectively minimizes motor-induced instabilities and vibrations, significantly improving STM performance. The use of non-metallic materials for key components prevents eddy current interference and ensures long-term reliability. A sapphire-based frame provides high stiffness and compactness, with an eigenfrequency of 16.2 kHz in bending mode, reducing vibration noise during atomic imaging. The system exhibits excellent stability, maintaining low drift rates in both the X-Y plane and Z direction, ensuring precise tip-sample alignment. The performance of the home-built STM was validated through high-resolution atomic imaging of graphite and TaS<sub>2</sub> surfaces. The simple, compact, and high-precision stepping mechanism, along with its ability to operate at low voltage, reduces experimental complexity. These features facilitate advanced material studies in constrained environments, such as high magnetic fields and low temperatures.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"274 ","pages":"Article 114157"},"PeriodicalIF":2.1,"publicationDate":"2025-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143924223","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 : 2025-05-02DOI: 10.1016/j.ultramic.2025.114139
Ivo Alxneit
{"title":"Prediction of the morphology of nano particles based solely on atom counting data","authors":"Ivo Alxneit","doi":"10.1016/j.ultramic.2025.114139","DOIUrl":"10.1016/j.ultramic.2025.114139","url":null,"abstract":"<div><div>The framework to determine the morphology of nano particles from atomically resolved electron microscopy images and atom counting data is introduced. Focus is placed on electron microscopy data avoiding advanced geometry optimization of the particle. The problem is solved by simulated annealing with different fitness functions assessed. Even for small particles the solution space rapidly becomes too large to be exhausted. The concept of site occupation probabilities, <span><math><msub><mrow><mi>p</mi></mrow><mrow><mi>i</mi></mrow></msub></math></span>, is then used to analyze a subset, typically very few hundred solutions. This is shown to be sufficient to reach a relative error of below 10% for <span><math><mrow><msub><mrow><mi>p</mi></mrow><mrow><mi>i</mi></mrow></msub><mo>></mo><mn>0</mn><mo>.</mo><mn>5</mn></mrow></math></span> already with 100 solutions allowing to determine with high confidence and low statistical error realistic average shapes also for nano particles of a few thousand atoms. These particles typically exhibit a well defined core covered by a layer of sites that are not occupied in each solution. It is further demonstrated that sites with high probability to contain a vacancy can be identified <em>assuming</em> the presence of a vacancy. If a vacancy is actually present in a particle its position can be identified with rather high fidelity. Finally, it is shown that the procedure can cope with the statistical error or ambiguities inherent in atom counting data based on noisy, low dose electron microscopy images.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"275 ","pages":"Article 114139"},"PeriodicalIF":2.1,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144123527","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 : 2025-04-29DOI: 10.1016/j.ultramic.2025.114134
Shengkai Guo , Zihe Xu , Xinyan Li , Zhidong Yang , Chenjie Feng , Renmin Han
{"title":"Robust projection parameter calibration in cryo-ET with L1-norm optimization","authors":"Shengkai Guo , Zihe Xu , Xinyan Li , Zhidong Yang , Chenjie Feng , Renmin Han","doi":"10.1016/j.ultramic.2025.114134","DOIUrl":"10.1016/j.ultramic.2025.114134","url":null,"abstract":"<div><div>Fiducial marker-based alignment in cryo-electron tomography (cryo-ET) has been extensively studied over a long period. The calibration of projection parameters using nonlinear least squares technique methodologies stands as the ultimate and pivotal stage in the alignment procedure. The efficacy of calibration is substantially impacted by noise and outliers in the marker data obtained from previous steps. Several robust fitting methods have been explored and implemented to address this issue by improving marker data or assigning weights to markers. However, these methods have their own limitations and often assume general Gaussian noise assumption, which may not accurately represent the distribution of noise and outliers in the marker data. In this work, we propose a robust projection parameter calibration model based on <span><math><msub><mrow><mi>L</mi></mrow><mrow><mn>1</mn></mrow></msub></math></span>-norm optimization under Laplace noise assumption in order to overcome the limitations of existing methods. To efficiently solve the problem, we also design a faster and stabler first-order non-sparse method based on smooth approximation strategy. Additionally, we introduce subgradient and subdifferential for mathematical analysis. The accuracy, robustness, and efficacy of our approach are demonstrated through both simulated and real-world experiments.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"274 ","pages":"Article 114134"},"PeriodicalIF":2.1,"publicationDate":"2025-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143907639","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 : 2025-04-26DOI: 10.1016/j.ultramic.2025.114153
BG Mendis
{"title":"On the impulse approximation in electron Compton scattering","authors":"BG Mendis","doi":"10.1016/j.ultramic.2025.114153","DOIUrl":"10.1016/j.ultramic.2025.114153","url":null,"abstract":"<div><div>Electronic structure measurement via Compton scattering requires the impulse approximation to be satisfied. This states that the inelastic collision time is short, so that the ‘secondary’ electron ejected out of the atom is effectively free of the crystal potential. The robustness of the impulse approximation is tested for boron nitride and aluminium using momentum-resolved electron energy loss spectroscopy. Reliable (with respect to impulse approximation) electronic structure information is obtained for Compton peak energies at ∼250 eV energy loss or higher. These experimental results are validated using a simple Kronig-Penney model of the secondary electron travelling through the crystal. For loosely bound valence electrons the impulse approximation is satisfied when the Compton peak energy is significantly larger than the mean inner potential of the crystal. This criterion provides a straightforward estimate of the experimental conditions required for extracting reliable Compton data from any given material.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114153"},"PeriodicalIF":2.1,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143895965","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 : 2025-04-18DOI: 10.1016/j.ultramic.2025.114150
Sarah Schroeder , Koen Dewettinck , Volker Heinz , Ute Bindrich , Dana Middendorf , Knut Franke
{"title":"Opportunities and challenges to determine surface free energy of chocolates on microscopic scale from atomic force microscopy adhesion measurements","authors":"Sarah Schroeder , Koen Dewettinck , Volker Heinz , Ute Bindrich , Dana Middendorf , Knut Franke","doi":"10.1016/j.ultramic.2025.114150","DOIUrl":"10.1016/j.ultramic.2025.114150","url":null,"abstract":"<div><div>Surface free energy (SFE) is an important surface property in food processing as it determines the wettability of solid surfaces or the interaction of mould surfaces and chocolate during the moulding process. High-resolution information about SFE could be useful to understand gloss inhomogeneities of chocolates after de-moulding. SFE is connected with adhesion properties. Thus, Atomic force microscopy (AFM) adhesion measurements can be applied to determine SFE of a solid surface at microscopic scale. For this purpose, AFM tips were functionalized to modify their SFE and used for adhesion measurements at three different chocolate gloss areas (matt, glossy and homogenous) via AFM force maps. Influence of relevant parameters such as surface roughness, contact area, relative humidity, and SFE of functionalized tips was considered. Two different mathematical approaches based on Johnson-Kendall-Roberts theory were used to calculate SFE from adhesion values. The measured adhesion values showed variations depending on functionalized tip and chocolate gloss area. The results showed a difference in adhesion and, consequently, SFE in the different gloss areas with gloss > homogenous > matt. However, SFE obtained from adhesion forces were not decisive enough to enable a direct correlation with SFE data from contact angle measurements at the same area.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114150"},"PeriodicalIF":2.1,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143855695","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 : 2025-04-18DOI: 10.1016/j.ultramic.2025.114148
Ilya A. Morozov, Roman I. Izyumov
{"title":"Influence of experimental conditions on apparent AFM tip-surface contact in air","authors":"Ilya A. Morozov, Roman I. Izyumov","doi":"10.1016/j.ultramic.2025.114148","DOIUrl":"10.1016/j.ultramic.2025.114148","url":null,"abstract":"<div><div>Accurate determination of the onset of the contact between the atomic force microscope (AFM) tip and the surface in force measurements is necessary both for calculating the constants of non-contact interactions and for determining the structural and mechanical properties of the materials. In an air environment the contact is preceded by a rapid jump of the tip to the surface due to attractive forces. If a surface is not deformed by a probe of a given stiffness, the end of the jump (minimum of the deflection of the cantilever) is taken as the onset of the contact. In this work, it is shown that the tip contacts with the deformable surface before the completion of the jump. It is reasonable to use the point of the extreme deflection velocity as the onset of the contact. A dynamic mass-spring model of the interaction of the tip with the viscoelastic material has shown that the high deflection velocity and the low rate of data acquisition (bandwidth) are the reasons for significant errors in determining the contact from the experimental force curve. In the most cases, the observed contact point is lower than the actual one (under certain conditions, the opposite situation is also possible) and the measurement error is at least 50 % (depending on the experimental settings, the properties of the probe and the material).</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114148"},"PeriodicalIF":2.1,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143870563","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":"Capacitance compensation on a double-barrel nanopipette for improving current detection of scanning ion conductance microscopy","authors":"Futoshi Iwata , Naoto Fukuzawa , Hitoshi Inomata , Kenta Nakazawa , Toshi Nagata , Hideya Kawasaki , Osamu Hoshi","doi":"10.1016/j.ultramic.2025.114149","DOIUrl":"10.1016/j.ultramic.2025.114149","url":null,"abstract":"<div><div>We developed a method to improve the current-detection response of scanning ion conduction microscopy (SICM) using a double-barrel nanopipette. By detecting the difference between the two signals from each channel, capacitive currents can be canceled out, resulting in an improved ion current detection response and reduced imaging time in bias-modulated scanning ion conductance microscopy operated with AC bias voltages (BM-SICM). Furthermore, this method can reduce the synchronized capacitive current noise of two adjacent channels of a double-barrel nanopipette by canceling each other via a differential operation. Therefore, an improved detection signal was achieved even in the SICM operated with a DC bias voltage by reducing the noise from the piezoelectric scanner. As demonstrated by the proposed method, chromosomes that were difficult to observe owing to their strong negative charges were clearly imaged in the BM-SICM operated with an AC bias voltage without artifacts caused by surface charging. Additionally, in SICM operating with a DC bias voltage, dynamic interaction among an intracellular short rod, <em>Listeria monocytogenes</em>, and Caco-2 human enterocyte-like cells was successfully observed.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114149"},"PeriodicalIF":2.1,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143864533","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 : 2025-04-08DOI: 10.1016/j.ultramic.2025.114136
Pengfei Lin, Kuan Lu, ChaBum Lee
{"title":"A novel method for through-silicon via characterization based on diffraction fringe analysis","authors":"Pengfei Lin, Kuan Lu, ChaBum Lee","doi":"10.1016/j.ultramic.2025.114136","DOIUrl":"10.1016/j.ultramic.2025.114136","url":null,"abstract":"<div><div>The precision metrology of through-hole silicon via (TSV) in the semiconductor industry has remained a critical challenge as its critical dimension (CD) reduces. In this letter, we report a novel method for TSV geometric feature measurement and characterization. By illuminating a collimated infrared laser beam to the TSV and then analyzing the TSV edge-induced diffraction interferometric fringe patterns, multiple geometric information of the TSV could be characterized, establishing its database. This computational approach to TSV characterization was validated by experiments. Being non-destructive and easy to deploy, this method provides a low cost and high efficiency solution for TSV metrology.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"272 ","pages":"Article 114136"},"PeriodicalIF":2.1,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143792586","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 : 2025-04-05DOI: 10.1016/j.ultramic.2025.114137
Desheng Ma , Steven E. Zeltmann , Chenyu Zhang , Zhaslan Baraissov , Yu-Tsun Shao , Cameron Duncan , Jared Maxson , Auralee Edelen , David A. Muller
{"title":"Emittance minimization for aberration correction I: Aberration correction of an electron microscope without knowing the aberration coefficients","authors":"Desheng Ma , Steven E. Zeltmann , Chenyu Zhang , Zhaslan Baraissov , Yu-Tsun Shao , Cameron Duncan , Jared Maxson , Auralee Edelen , David A. Muller","doi":"10.1016/j.ultramic.2025.114137","DOIUrl":"10.1016/j.ultramic.2025.114137","url":null,"abstract":"<div><div>Precise alignment of the electron beam is critical for successful application of scanning transmission electron microscopes (STEM) to understanding materials at atomic level. Despite the success of aberration correctors, aberration correction is still a complex process. Here we approach aberration correction from the perspective of accelerator physics and show it is equivalent to minimizing the emittance growth of the beam, the span of the phase space distribution of the probe. We train a deep learning model to predict emittance growth from experimentally accessible Ronchigrams. Both simulation and experimental results show the model can capture the emittance variation with aberration coefficients accurately. We further demonstrate the model can act as a fast-executing function for the global optimization of the lens parameters. Our approach enables new ways to quickly quantify and automate aberration correction that takes advantage of the rapid measurements possible with high-speed electron cameras. In part II of the paper, we demonstrate how the emittance metric enables rapid online tuning of the aberration corrector using Bayesian optimization.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114137"},"PeriodicalIF":2.1,"publicationDate":"2025-04-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143821413","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 : 2025-04-04DOI: 10.1016/j.ultramic.2025.114138
Desheng Ma , Steven E. Zeltmann , Chenyu Zhang , Zhaslan Baraissov , Yu-Tsun Shao , Cameron Duncan , Jared Maxson , Auralee Edelen , David A. Muller
{"title":"Emittance Minimization for Aberration Correction II: Physics-informed Bayesian Optimization of an Electron Microscope","authors":"Desheng Ma , Steven E. Zeltmann , Chenyu Zhang , Zhaslan Baraissov , Yu-Tsun Shao , Cameron Duncan , Jared Maxson , Auralee Edelen , David A. Muller","doi":"10.1016/j.ultramic.2025.114138","DOIUrl":"10.1016/j.ultramic.2025.114138","url":null,"abstract":"<div><div>Aberration-corrected Scanning Transmission Electron Microscopy (STEM) has become an essential tool in understanding materials at the atomic scale. However, tuning the aberration corrector to produce a sub-Ångström probe is a complex and time-costly procedure, largely due to the difficulty of precisely measuring the optical state of the system. When measurements are both costly and noisy, Bayesian methods provide rapid and efficient optimization. To this end, we develop a Bayesian approach to fully automate the process by minimizing a new quality metric, beam emittance, which is shown to be equivalent to performing aberration correction. In part I, we derived several important properties of the beam emittance metric and trained a deep neural network to predict beam emittance growth from a single Ronchigram. Here we use this as the black box function for Bayesian Optimization and demonstrate automated tuning of simulated and real electron microscopes. We explore different surrogate functions for the Bayesian optimizer and implement a deep neural network kernel to effectively learn the interactions between different control channels without the need to explicitly measure a full set of aberration coefficients. Both simulation and experimental results show the proposed method outperforms conventional approaches by achieving a better optical state with a higher convergence rate.</div></div>","PeriodicalId":23439,"journal":{"name":"Ultramicroscopy","volume":"273 ","pages":"Article 114138"},"PeriodicalIF":2.1,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143821412","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}