{"title":"An empirical-parameter-free approach toward quantitative in situ electron tomography data analysis: in situ observation of metal nanoparticle sintering","authors":"Shiro Ihara , Shunsuke Sato , Mizumo Yoshinaga , Mitsuhiro Murayama","doi":"10.1016/j.micron.2025.103872","DOIUrl":"10.1016/j.micron.2025.103872","url":null,"abstract":"<div><div>Metal nanoparticles (NPs) exhibit multiple unique technological characteristics compared to their bulk or micrometer counterparts, such as coalescing or sintering at lower temperatures. This enables low-cost manufacturing of electronic products by using NPs as nano pastes. Three-dimensional (3D) observation of their dynamic sintering process is an emerging approach to deepen our scientific and technological understanding of the different pathways underlying sintering phenomena at the nanoscale. However, quantitatively evaluating the details of NP ensembles, including measurements of neck length, relative geometrical features of the NPs, initial dispersion, and their relative positions, from 3D data remains labor-intense and error prone so far due to the non-uniformity of both NP shape and their distribution, as well as the large volume of data. Here, we developed an empirical-parameter-free scheme for the quantitative evaluation of microstructural parameters in 3D that characterize neck growth and densification. The developed scheme was based only on a few relatively simple mathematical assumptions, such as the center point of any geometry being the farthest from the outside of the geometry, and the neck being a flat plane formed between NPs. This paper demonstrates the successful extraction of both the neck and the connectivity of NP ensembles from in situ scanning transmission electron microscopy (STEM) tomography data, providing a quantitative description of NPs’ coalescing/sintering behavior.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103872"},"PeriodicalIF":2.5,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144588086","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}
MicronPub Date : 2025-07-02DOI: 10.1016/j.micron.2025.103873
Ehsan Nikbin , Dian Yu , Ilya Gourevich , Stas Dogel , R.J. Dwayne Miller , Jane Y. Howe
{"title":"Design and evaluation of a novel Faraday cup for easy and accurate beam current measurement in a transmission electron microscope","authors":"Ehsan Nikbin , Dian Yu , Ilya Gourevich , Stas Dogel , R.J. Dwayne Miller , Jane Y. Howe","doi":"10.1016/j.micron.2025.103873","DOIUrl":"10.1016/j.micron.2025.103873","url":null,"abstract":"<div><div>Beam current measurement is a crucial step in estimating the electron dose when studying beam-sensitive samples in electron microscopy. A Faraday cup is a standard tool for measuring beam current; however, commercially available Faraday cups for transmission electron microscopes (TEM) are limited, expensive, and often difficult to use as the cup itself is invisible in the TEM. We herein present a new Faraday cup design that fits into an insulated TEM holder of Hitachi HT7700 and HT7800 series and can be easily located using four symmetrical through holes around the cup. This design also accommodates the 3 mm TEM mesh grid in the holder and allows both sample imaging and access to the Faraday cup within the TEM stage movement range. We evaluated the effectiveness of our Faraday cup in capturing the electron beam by varying the diameter to depth ratio and material of the Faraday cup through experimental measurements and Monte Carlo simulations, demonstrating an accuracy better than 1–2 %. The preferred configuration is an aluminum cup with a diameter of 0.2 mm and a depth of 0.8 mm. Monte Carlo simulations also suggest that this Faraday cup provides accurate beam current measurement at different electron energies. Our novel Faraday cup design provides a practical, simple, and cost-effective solution for beam current measurement in a TEM.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103873"},"PeriodicalIF":2.5,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144569960","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}
MicronPub Date : 2025-06-20DOI: 10.1016/j.micron.2025.103868
Shusuke Kanomi , Tomohiro Miyata , Hiroshi Jinnai
{"title":"Identification of phase-separated structures and polymer crystals inside polyolefin blends","authors":"Shusuke Kanomi , Tomohiro Miyata , Hiroshi Jinnai","doi":"10.1016/j.micron.2025.103868","DOIUrl":"10.1016/j.micron.2025.103868","url":null,"abstract":"<div><div>Polyolefins, including polyethylene (PE) and isotactic polypropylene (iPP), constitute approximately half of all plastic production and consumption. However, recycled PE/iPP mixtures tend to be brittle, necessitating modifications to enhance their physical properties for practical applications. A comprehensive understanding of the internal structure of PE/iPP blends, which is influenced by phase separation and crystallization, is essential for improving their physical properties. Conventional electron microscopy techniques face limitations in distinguishing phases and observing crystal morphology. In this study, we introduce a four-dimensional scanning transmission electron microscopy technique known as nanodiffraction imaging (NDI) to analyze the internal structure of polyolefin blends. Scanning a 1.4 nm-diameter electron beam at 5 nm intervals, we examined a high-density PE (HDPE)/iPP blend specimen with a 10:90 wt composition. Based on scattering vectors and azimuthal angles of the diffraction peaks, NDI effectively identifies phases inside the HDPE/iPP blend, maps the spatial distribution of HDPE and iPP crystals, and facilitates the orientation mapping of their molecular chains. Additionally, it enables analysis of the relationship between HDPE and iPP crystals near the interface. The demonstrated effectiveness of NDI in structural analysis represents a significant advancement in understanding how the internal structure of polyolefin blends correlates with their physical properties.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103868"},"PeriodicalIF":2.5,"publicationDate":"2025-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365936","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}
MicronPub Date : 2025-06-16DOI: 10.1016/j.micron.2025.103866
Martin Couillard
{"title":"Unmixing system-wide and geometry-specific plasmon modes in faceted nanoparticle trimers using a two-step matrix factorization","authors":"Martin Couillard","doi":"10.1016/j.micron.2025.103866","DOIUrl":"10.1016/j.micron.2025.103866","url":null,"abstract":"<div><div>Plasmonic modes in coupled nanoparticle systems are shaped by both interparticle interactions and geometry-specific features, such as facets and vertices. However, standard decomposition techniques, such as non-negative matrix factorization (NMF), often fail to individually isolate modes that are localized. This limitation arises because the factorization process relies solely on spectral data, without incorporating spatial context. To address this, we apply factorization in two steps. First, NMF identifies bulk and coupled system-wide contributions, that can then be removed in spectral reconstruction to isolate localized geometry-specific modes. Then, we perform region-based NMF on spatially-selected areas of a silica-shelled silver-nanoparticle trimer to identify subtle energy shifts between vertex and facet modes at different locations on the nanoparticles. Our approach thus enables the identification of global plasmonic modes extending across the entire dimer or trimer system, as well as geometry-specific modes arising from the faceted structure of individual nanoparticles. By reintroducing spatial context, we further distinguish between different localized modes, even within the same nanoparticle, revealing the influence of subtle geometric variations on plasmonic resonances and the potential for partial coupling between geometry-specific modes.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103866"},"PeriodicalIF":2.5,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365937","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}
MicronPub Date : 2025-06-14DOI: 10.1016/j.micron.2025.103867
E. Stai , V. Constantoudis , A. Kaidatzis , V. Singh , M.K. Tiwari , E. Gogolides
{"title":"Generative resolution-enhanced microscopy based on computational stitching of Fourier spectra","authors":"E. Stai , V. Constantoudis , A. Kaidatzis , V. Singh , M.K. Tiwari , E. Gogolides","doi":"10.1016/j.micron.2025.103867","DOIUrl":"10.1016/j.micron.2025.103867","url":null,"abstract":"<div><div>Scanning Microscopies such as Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) are widely used in nanotechnology to display (<span><span>Kalinin et al., 2023</span></span>) and quantify surface nanoroughness. However, their measurements suffer from scale and spatial limitations which hinder their full exploitation in the optimization of nanostructure fabrication and performance. The aim of this work is to overcome these limitations by proposing a computational method which enables the generation of multiple surface measurements (overcome spatial limitation) with enhanced scale content and increased resolution (overcome scale limitation) successfully mimicking the real surfaces. The method exploits the benefits of Fourier transform and is easily implemented based on Fourier spectra stitching. It can provide astonishing increase of resolution (>10 times) in a large variety of image textures and, is fast with no requirements for training with large data sets. The so-called generative Fourier Spectra Stitching (gFSS) method is validated in synthesized rough surfaces and applied in real experimental AFM and SEM images of magnetic and metal surfaces with very promising results.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103867"},"PeriodicalIF":2.5,"publicationDate":"2025-06-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144290564","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":"Early stages of trunk muscles differentiation in small-spotted catshark (Scyliorhinus canicula): Ultrastructural studies","authors":"Damian Lewandowski , Magda Dubińska-Magiera , Marta Migocka-Patrzałek , Sylvie Mazan , Małgorzata Daczewska","doi":"10.1016/j.micron.2025.103865","DOIUrl":"10.1016/j.micron.2025.103865","url":null,"abstract":"<div><div>We report here a study of early trunk muscle differentiation in the catshark <em>S</em>. <em>canicula</em>, a representative of Chondrichthyes. Light and TEM investigations revealed that during <em>S</em>. <em>canicula</em> somitogenesis, the metameric cell segments (somites) are formed and their cell arrangement resembles the shape of a rosette. The somite structure shares similarities with those observed in lungfish and urodeles. As embryogenesis proceeds, somites differentiate into three compartments: the dermomyotome (with dorsomedial and ventrolateral lips), myotome, and sclerotome. In the developing myotome two, morphologically different classes of cells are distinguished: elongated cells with homogenous nuclei and bottle-shaped cells with condensed nuclei. Based on morphological studies, we hypothesize that in <em>S</em>. <em>canicula</em>, the second class of cells observed in the early myotome can be classified as muscle progenitor cells. Myogenesis in small-spotted catshark starts in the ventral part of the somite, as observed for the development of trunk muscles in teleosts. In summary, the structure of somites in <em>S</em>. <em>canicula</em> shares similarities with lungfish and urodeles, which could reflect plesiomorphic features of small-spotted catshark myogenesis. On the other hand, the myogenesis appear to be apomorphic feature. Many issues related to myogenesis in sharks, cartilaginous fish representatives, remain unresolved. These data provide new insights into myogenesis in Chondrichthyes, the closest outgroup to Osteichthyes, and contribute to a better understanding of ancestral features of this process and its diversification across vertebrates.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103865"},"PeriodicalIF":2.5,"publicationDate":"2025-06-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144279823","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}
MicronPub Date : 2025-06-07DOI: 10.1016/j.micron.2025.103864
Daniel L. Foley , Emily H. Mang , Yongqiang Wang , Douglas E. Spearot , Mitra L. Taheri
{"title":"Low frequency band pass Fourier filtering for irradiation damage analysis in the transmission electron microscope","authors":"Daniel L. Foley , Emily H. Mang , Yongqiang Wang , Douglas E. Spearot , Mitra L. Taheri","doi":"10.1016/j.micron.2025.103864","DOIUrl":"10.1016/j.micron.2025.103864","url":null,"abstract":"<div><div>We demonstrate a simple technique for improved imaging of non-crystallographic, irradiation-induced defects in the transmission electron microscope (TEM). By Fourier filtering bright-field TEM images to isolate relatively low-frequency fluctuations in intensity, it is possible to better resolve defects such as cavities caused by He-ion irradiation of iron. This analysis can be done with basic TEM imaging and most image processing software. This technique requires minimal defocus and can eliminate contrast mechanisms on both longer and short length scales. The resulting images are sensitive to filtering parameters, but clearly reveal the size, density, and distribution of cavities when compared with standard imaging techniques.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103864"},"PeriodicalIF":2.5,"publicationDate":"2025-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307045","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}
MicronPub Date : 2025-06-01DOI: 10.1016/j.micron.2025.103863
Haozhe Lu , Chuanhong Jin
{"title":"Self-aligned protective shield for preparing beam-sensitive MEMS-based chip samples using focused ion beam","authors":"Haozhe Lu , Chuanhong Jin","doi":"10.1016/j.micron.2025.103863","DOIUrl":"10.1016/j.micron.2025.103863","url":null,"abstract":"<div><div>Focused ion beam (FIB) preparation for transmission electron microscopy (TEM) specimens is widely used across various fields. However, in-situ micro-electro-mechanical systems-based (MEMS-based) chip specimen preparation presents unique challenges, particularly during the transfer stage, which involves transferring and attaching the sample to the MEMS-based chip. Attaching these chips often requires tilting the sample stage, which can cause the ion beam to strike the region of interest (ROI) at a steep, oblique angle. This leads to damage, redeposition, and contamination from ion beam-induced metal deposition. This issue becomes particularly critical for beam-sensitive nanostructures like aligned single-walled carbon nanotube arrays (A-CNTs). To address this, we developed a self-aligned protective shield method. This technique uses the inherent angular offset between the electron and ion beams in a dual-beam FIB system to shield the ROI during critical processing steps. Compatible with standard sampling techniques, our approach effectively mitigates ion beam-induced damage, redeposition and contamination. Controlled experiments on palladium (Pd)–A-CNT–silicon oxide (SiO<sub>2</sub>) multilayers, typical contact interface for A-CNT based devices, show enhanced interfacial integrity and structural clarity in scanning TEM (STEM) imaging. Ultimately, our method provides a robust and versatile solution for preparing high-quality cross-sectional TEM lamellae for in-situ MEMS-based chips, offering broad applicability to ion beam-sensitive materials.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103863"},"PeriodicalIF":2.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144230191","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}
MicronPub Date : 2025-05-29DOI: 10.1016/j.micron.2025.103862
Smyan Sondur, Hugo E.A. Svenberg, Anton Johansson, Philip J.B. Koeck
{"title":"Simulating dynamic image formation in a Transmission Electron Microscope with a proposed electron beam phase plate","authors":"Smyan Sondur, Hugo E.A. Svenberg, Anton Johansson, Philip J.B. Koeck","doi":"10.1016/j.micron.2025.103862","DOIUrl":"10.1016/j.micron.2025.103862","url":null,"abstract":"<div><div>Imaging thin organic specimens with Transmission Electron Microscopy (TEM) presents a significant challenge due to their inherently weak contrast. An additional electron optical element, placed in a focal plane of the objective lens, such as a phase plate (PP) can improve the contrast by inducing a relative phase shift between scattered and unscattered electrons. However, any additional optical element can also lead to additional noise due to random and beam-induced variations. To address this problem we have, as a first example, simulated the dynamic image formation of a weak phase object in a TEM equipped with a proposed PP consisting of two electron beams orthogonal to the optical axis of the TEM. The random and beam-induced variation of the PP is simulated with particle dynamics including all pairwise interactions among the electrons of the PP and the TEM electron. The resulting three-dimensional PP potential, which now includes these variations, is then used in a variant of the multislice algorithm to compute the exit wave’s interaction with the PP. The quality of the simulation was validated against previous theoretical calculations and the simulated images were quantitatively compared to the projected potential of the specimen using Fourier ring correlation. These simulations indicate that a TEM equipped with this type of PP could produce images with consistent contrast in a resolution band up to about 4 Å. This range could be extended to higher resolutions by a modified CTF-correction including the effect of the PP. The underlying idea of dynamic simulations taking the variation of optical elements and maybe even the specimen into account could be generalized to many other imaging situations.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103862"},"PeriodicalIF":2.5,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144195773","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}
MicronPub Date : 2025-05-26DOI: 10.1016/j.micron.2025.103861
Mauricio da Silva Paulo , Paulo Henrique Rezende , Ana Clara Pereira Teixeira , Dayvson Ayala-Costa , José Lino-Neto , Glenda Dias
{"title":"New insights into aberrant sperm morphology: The structure of dimorphic spermatozoa in Edessa rufomarginata (De Geer, 1773) (Hemiptera: Pentatomidae)","authors":"Mauricio da Silva Paulo , Paulo Henrique Rezende , Ana Clara Pereira Teixeira , Dayvson Ayala-Costa , José Lino-Neto , Glenda Dias","doi":"10.1016/j.micron.2025.103861","DOIUrl":"10.1016/j.micron.2025.103861","url":null,"abstract":"<div><div>Male bugs of the Pentatomidae family can produce heteromorphic sperm during spermiogenesis, forming two or more distinct morphotypes. In <em>Edessa rufomarginata</em> (De Geer, 1773), this phenomenon culminates in the production of two specific sperm morphotypes: one typical (Type I) and the other aberrant (Type II). Using transmission electron microscopy techniques, we describe in detail the characteristics of these cells. Typical sperm have characteristics common to Heteroptera, including an acrosome positioned anteriorly to the nucleus, which later elongates laterally to it; two symmetrical mitochondrial derivatives in a “half-moon” shape connected to the axoneme by two bridges; and the absence of accessory bodies. In contrast, aberrant spermatozoa have a rounded acrosome that does not extend laterally to the nucleus until the nucleus-flagellum transition region. Furthermore, the mitochondrial derivatives of these spermatozoa are considerably thicker, reaching up to five times the diameter observed in typical spermatozoa. However, both morphotypes exhibit the synapomorphies of Heteroptera. These structural distinctions indicate a marked morphological variation that may be associated with specific functions or reproductive strategies of the species. These new morphological data are possibly specific to the genus <em>Edessa</em>, or perhaps to the Edessinae. They may be complementary tools for resolving taxonomic and phylogenetic questions for this diverse group.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"196 ","pages":"Article 103861"},"PeriodicalIF":2.5,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144137808","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}