Poonam Yadav, Leonardo Shoji Aota, Eric V Woods, Tim M Schwarz, Yug Joshi, Mahander Pratap Singh, Baptiste Gault
{"title":"Advancing Sodium-Ion Battery Cathode Analysis With Cryogenic Ag-coated APT Specimens.","authors":"Poonam Yadav, Leonardo Shoji Aota, Eric V Woods, Tim M Schwarz, Yug Joshi, Mahander Pratap Singh, Baptiste Gault","doi":"10.1093/mam/ozaf041","DOIUrl":"https://doi.org/10.1093/mam/ozaf041","url":null,"abstract":"<p><p>Layered oxide cathodes have attracted wide research interest due to their controllable synthesis, tuneability, and high energy density in sodium-ion batteries (SIBs). However, in layered oxide cathodes, capacity retention is unsatisfactory due to structural changes, and the severity of capacity fading increases at higher voltages. Chemical heterogeneity and concentration gradient lead to the co-existence of multiple phases with lattice mismatch and strain development. To achieve the practical usage of high-density and low-cost layered oxide cathodes for SIBs, it is very important to develop an atomic-scale understanding of the compositional changes in the multi-component cathode. Atom probe tomography (APT) is a very promising technique to analyze chemical composition and heterogeneity in three dimensions (3D) with high spatial resolution and brings insights into possible property- or lifetime-limiting factors. However, APT is underpinned by an intense electric field that can drive preferential alkali metal outward migration and cause in situ de-intercalation of alkali metals that makes APT analysis challenging. As a first report, we show that silver (Ag) coating on SIB cathode APT specimens, deposited inside the focused-ion beam (FIB) at cryogenic temperature, allows for analysis of the compositional heterogeneity in air-sensitive sodium-ion-layered oxide cathode material.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 4","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144699010","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Neil Mulcahy, James O Douglas, Michele Shelly Conroy
{"title":"Look What You Made Me Glue: SEMGlu™ Enabled Alternative Cryogenic Sample Preparation Process for Cryogenic Atom Probe Tomography Studies.","authors":"Neil Mulcahy, James O Douglas, Michele Shelly Conroy","doi":"10.1093/mam/ozaf063","DOIUrl":"https://doi.org/10.1093/mam/ozaf063","url":null,"abstract":"<p><p>Extensive efforts have been applied to develop workflows for sample preparation of specimens for atom probe tomography at cryogenic temperatures. This is primarily due to the difficulty involved in preparing site-specific lift-out samples at cryogenic temperatures without the assistance of the gas injection system (GIS) as using it under cryogenic conditions leads to nonuniform and difficult to control deposition. Building on the efforts of previously developed GIS-free workflows utilizing redeposition techniques, this work provides an alternative approach using SEMGlu™, which is an electron beam curing adhesive that remains usable at cryogenic temperatures, to both lift out cryogenically frozen samples and mount these samples to Si microarray posts for subsequent redeposition welding. This approach is applicable for a full cryogenic workflow but is particularly useful for nonfully cryogenic workflows such as beam-sensitive samples, samples that mill easily, and samples with challenging geometries. We demonstrate atom probe analysis of silicon samples in both laser pulsing and voltage mode prepared using this workflow, with comparable analytical performance to a presharpened microtip coupon. An application-based example, which directly benefits from this approach, correlative liquid cell transmission electron microscopy and cryogenic atom probe tomography sample preparation, is also shown.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 4","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144690928","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Revealing the Structural Organization of Starch From Native Potatoes Using Polarization-Resolved Second Harmonic Generation Microscopy.","authors":"Kiran Kumar Kolathur, Nandana Bijulal, Gagan Raju, Bhaswati Sarmah, Vishwa Jyoti Baruah, Ishita Chakraborty, Sib Sankar Mal, Hemanth Noothalapati, Ajeetkumar Patil, Guan-Yu Zhuo, Nirmal Mazumder","doi":"10.1093/mam/ozaf010","DOIUrl":"https://doi.org/10.1093/mam/ozaf010","url":null,"abstract":"<p><p>Starch from a single botanical source can exhibit variations in physicochemical properties in both its native and hydrolyzed forms. This study examined the structural and functional characteristics of starch from five potato varieties of India. In vitro enzymatic hydrolysis was employed to determine the dextrose equivalent profile of each starch type. The amylose content among the five potato varieties ranged from 17.5 and 25%. Optical microscopy revealed that the native starch granules were ovoid or elliptical in shape. X-ray diffraction analysis confirmed the presence of starch crystallinity and identified spectral peaks characteristic of A-type starch crystals in the native form. Fourier transform infrared spectra indicated common stretching and deformation of bonds in all native starches. Differential scanning calorimeter endotherms showed the highest and lowest gelatinization peak temperatures among the starch varieties. Additionally, polarization-resolved second harmonic generation microscopy was employed to image the starch granules and obtain high-resolution structural insights, revealing distinctive patterns of starch crystallinity. The findings of this study can help to optimize the usage of potato starch in food and nonfood industries. Additionally, understanding the control points of starch digestion and genetically tailoring potato varieties with different digestibility profiles could be beneficial for nutraceutical applications.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 4","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144699011","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Kayla Lynne Haberman, Jelena Danilovic Lukovic, Snezana Kovacevic, Xinyi Zhang, Bessie Kebaara, Joseph Taube, Debora Berti, Bernd Zechmann
{"title":"Comprehensive Comparison Between STEM-HAADF and TEM Bright-field Mode for Imaging Resin Embedded Biological Samples.","authors":"Kayla Lynne Haberman, Jelena Danilovic Lukovic, Snezana Kovacevic, Xinyi Zhang, Bessie Kebaara, Joseph Taube, Debora Berti, Bernd Zechmann","doi":"10.1093/mam/ozaf038","DOIUrl":"10.1093/mam/ozaf038","url":null,"abstract":"<p><p>Most investigations of resin embedded biological samples by transmission electron microscopy (TEM) have been performed in TEM bright-field mode where the electron beam transmits through the sample. Modern TEMs can also be used in scanning TEM mode (STEM) where the beam scans across the sample. The preferred detector for STEM mode is the high-angle annular dark-field (HAADF) detector. The aim of this study was to compare image quality of resin embedded biological samples such as yeast (Saccharomyces), algae (Chlorella, Haematococcus), plant leaves (Nicotiana), human cells (MCF7), and animal tissue (mouse liver and brain) between TEM bright-field and STEM-HAADF mode. Generally, images taken in STEM-HAADF mode showed better image quality in terms of contrast, brightness, and signal-to-noise ratio. Samples of sections that did not receive postcontrasting with uranyl acetate or lead citrate appeared significantly less grainy. Specifically, STEM-HAADF mode resulted in significantly better image quality of algae cells, MCF7, and liver cells that did not receive postcontrasting. Artifacts visible in TEM mode were absent in STEM-HAADF mode. Thus, we can conclude that STEM-HAADF mode has significant advantages when investigating resin embedded biological samples that have little contrast or sections that did not receive postcontrasting rendering postcontrasting of sections unnecessary.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144120110","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Aidar Zakirov, Yann Le Bouar, Frédéric Fossard, Williams Lefebvre
{"title":"A Reference Hydride Ratio Method for the Resolution of Al/Fe Peak Overlapping in Atom Probe Tomography Experiments.","authors":"Aidar Zakirov, Yann Le Bouar, Frédéric Fossard, Williams Lefebvre","doi":"10.1093/mam/ozaf030","DOIUrl":"https://doi.org/10.1093/mam/ozaf030","url":null,"abstract":"<p><p>Precise Fe concentration measurements are essential to understand the kinetics of precipitation and evolution of mechanical properties in Al-Fe alloys. Moreover, with the increasing proportion of recycled metals, it is mandatory to rely on techniques capable of tracking impurities in Al-alloys to elucidate their effects on microstructure and properties. Atom Probe Tomography (APT) is a powerful material analysis tool capable of precise composition measurements. As it relies on time-of-flight mass spectrometry, the quality of the composition measurements is highly dependent on the proper peak identification and solving peak overlapping. The complexity of peak decomposition multiplies if molecular ions such as hydrides or oxides are present in the mass spectrum. Al-Fe is one of these systems, where three out of four peaks of Fe isotopes are overlapping with Al, AlH, and AlH2 mass intervals. To solve this complex peak overlapping case, an approach has been developed here. It is based on acquiring the Al-hydride formation ratio from APT analyses of standard materials, where no overlap with Fe peaks is observed. This simple method aims to improve the precision of Fe concentration measurements in Al-Fe system.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144032914","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Kerui Wei, Matthew Lindley, Xuzhao Liu, Sarah J Haigh, Ping Xiao, Philip J Withers, Anamul Haq Mir, Graeme Greaves, João P Martins, Junquan Lao, Xiangli Zhong
{"title":"Novel Focused Ion Beam Techniques for Enhanced Sample Preparation for In Situ Transmission Electron Microscopy Heating and Irradiation Experiments.","authors":"Kerui Wei, Matthew Lindley, Xuzhao Liu, Sarah J Haigh, Ping Xiao, Philip J Withers, Anamul Haq Mir, Graeme Greaves, João P Martins, Junquan Lao, Xiangli Zhong","doi":"10.1093/mam/ozaf029","DOIUrl":"https://doi.org/10.1093/mam/ozaf029","url":null,"abstract":"<p><p>Focused ion beam (FIB) systems have revolutionized sample preparation for transmission electron microscopy (TEM), enabling precise and site-specific material analysis. However, the conventional ion beam-induced deposition (IBID) approach to preparing FIB samples can lead to contamination effects that can compromise the quality of TEM data acquisition. This study introduces an innovative FIB method for connecting TEM lamellae to support grids via redeposition, avoiding the contamination issue. We demonstrate the effectiveness of this technique through observations of a SiC phase within tristructural-isotropic particles during in situ high-temperature and irradiation TEM experiments, establishing an improved process for characterizing material behaviors during exposure to their industrially relevant environmental conditions.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144033479","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Morphology of Mouthparts and Distribution of Sensilla in Immature Stages and Adults of Parthenium Beetles.","authors":"Priyanka Yadav, Arvind Kumar Patel, Desh Deepak Chaudhary, Bhupendra Kumar","doi":"10.1093/mam/ozaf035","DOIUrl":"https://doi.org/10.1093/mam/ozaf035","url":null,"abstract":"<p><p>The Parthenium beetle, Zygogramma bicolorata Pallister (Coleoptera: Chrysomelidae) is a notable biocontrol agent against invasive Parthenium weed in Australia, South Africa, and the Indian subcontinent. While larvae consume both inflorescences and leaves, and adults feed exclusively on leaves, no prior study has compared the mouthparts of Z. bicolorata larvae and adults. Present study utilized scanning electron microscopy to investigate the morphology and distribution of sensilla on mouthparts of fourth-instar larvae, pupae, and adults. Our results revealed that fourth-instar larvae had 9-different sensillum types: sensilla chaetica (Sch I-III), sensilla basiconica (Sb I-V), and sensilla digitiformia (Ds) on their mouthparts, whereas pupal sensilla were fewer and less distinct. In adults, 13-different sensillum types were present: sensilla chaetica (Sch I-III) on labrum, labium, mandibles, and maxillae; sensilla basiconica (Sb I-VI) on labium, epipharyx, lacinia, maxillary palps, and labial palps; sensilla digitiformia (Ds) on maxillary palps; and sensilla campaniformia (Sca), and sensilla coeloconica (Sco I-II) on epipharyx. These sensilla likely play vital roles in feeding behavior, sensory perception, and host plant detection. Our findings provide a microscopic morphological foundation for further research on food recognition mechanisms and local adaptations in specialist phytophagous insects.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143993106","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dal-Jae Yun, Junhyeong Park, Youngkwon Haam, Hee-Seok Kweon, Hwan Hur, Jisoo Kim, In-Yong Park, Ha Rim Lee, Haewon Jung
{"title":"Three-Dimensional Reconstruction of Serial Block-Face Scanning Electron Microscopy Using Semantic Segmentation based on Semi-Supervised Deep Learning.","authors":"Dal-Jae Yun, Junhyeong Park, Youngkwon Haam, Hee-Seok Kweon, Hwan Hur, Jisoo Kim, In-Yong Park, Ha Rim Lee, Haewon Jung","doi":"10.1093/mam/ozaf047","DOIUrl":"https://doi.org/10.1093/mam/ozaf047","url":null,"abstract":"<p><p>Serial block-face scanning electron microscopy (SBF-SEM) is employed to achieve high-resolution volume reconstructions and detailed ultrastructural analyses of complex organelles. The performance of SBF-SEM is evaluated according to the accuracy of segmentation. Our study introduces a semi-supervised learning approach using a segment interpolation method to mitigate the costs of manual segmentation. The shapes and locations of individual segments between sparsely annotated label images are estimated using the proposed method. The proposed method is particularly well suited for SBF-SEM, where alignment and fine cutting of samples allow for accurate predictions with a minimal amount of labelled data. To validate the deep neural networks trained using the proposed method, the F-1 score metric and the K-fold technique were utilized. The results achieved an F-1 score of 0.89 for mouse brain cells and 0.84 for inverted images during the validation process for semi-supervised learning. Testing on an independently separated test dataset yielded scores of 0.84 for mouse brain cells and 0.80 for inverted cases. The automatically segmented results were then reconstructed in volume images using the marching cube algorithm. This allows for a three-dimensional (3-D) analysis of complex organelles, with potential applications in the fields of biology and medicine.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144266652","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Aurys Šilinga, András Kovács, Stephen McVitie, Rafal E Dunin-Borkowski, Kayla Fallon, Trevor P Almeida
{"title":"Model-Based Iterative Reconstruction of Three-Dimensional Magnetization in a Nanowire Structure Using Electron Holographic Vector Field Tomography.","authors":"Aurys Šilinga, András Kovács, Stephen McVitie, Rafal E Dunin-Borkowski, Kayla Fallon, Trevor P Almeida","doi":"10.1093/mam/ozaf043","DOIUrl":"https://doi.org/10.1093/mam/ozaf043","url":null,"abstract":"<p><p>Experimental techniques for the characterization of three-dimensional (3D) magnetic spin structures are required to advance the performance of nanoscale magnetic technologies. However, as component dimensions approach the nanometer range, it becomes ever more challenging to analyze 3D magnetic configurations quantitatively with the required spatial resolution and sensitivity. Here, we use off-axis electron holography and model-based iterative reconstruction to reconstruct the 3D magnetization distribution in an exemplary nanostructure comprising an L-shaped ferromagnetic cobalt nanowire fabricated using focused electron beam induced deposition. Our approach involves using off-axis electron holography to record tomographic tilt series of electron holograms, which are analyzed to reconstruct electron optical magnetic phase shifts about two axes with tilts of up to ±60∘. A 3D magnetization vector field that provides the best fit to the tomographic phase measurements is then reconstructed, revealing multiple magnetic domains in the nanowire. The reconstructed magnetization is shown to be accurate for magnetic domains that are larger than approximately 50 nm. Higher spatial resolution and improved signal-to-noise can be achieved in the future by using more specialized electron microscopes, improved reconstruction algorithms, and automation of data acquisition and analysis.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144275258","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Study of the Adhesive Organ and Associated Structures of Glyptothorax ngapang (Teleostei: Sisoridae) From Manipur, India Using Light and Scanning Electron Microscopy.","authors":"Linthoingambi Irengbam, Ningombam Shashibala, Catherine Ngangbam, Gitartha Kaushik","doi":"10.1093/mam/ozaf034","DOIUrl":"https://doi.org/10.1093/mam/ozaf034","url":null,"abstract":"<p><p>The current work represents the scanning electron microscopical study of the adhesive organ and its associated structures in the hill stream silurid Glyptothorax ngapang Vishwanath and Linthoingambi, 2007 from Manipur, India for the first time. The inverted \"U\"-shaped thoracic adhesive apparatus of the fish is located between the bases of its pectoral fins on the ventral side, just below the operculum. The apparatus had longitudinal ridges and grooves in the scanning electron microscopy picture, and the posterior base had a slightly concave triangular depression. The ridges were seen with spiny tubercular projections or the unculi of varying shapes and sizes. Grooves were devoid of any glands and such horny structures. Mucous gland openings were seen in the median depression of the apparatus as well as on the general body surface. Skin appeared rough due to the presence of numerous plaques. Tubercles, papillae, and receptor organs surrounded by numerous microvilli were seen around the snout region.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":"31 3","pages":""},"PeriodicalIF":2.9,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144528752","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}