{"title":"Light Element (C, N, O) Quantification by EDXS: Application to Meteorite Water Content and Organic Composition.","authors":"Corentin Le Guillou, Pierre-Marie Zanetta, Hugues Leroux, Anne-Marie Blanchenet, Maya Marinova","doi":"10.1093/mam/ozae071","DOIUrl":"10.1093/mam/ozae071","url":null,"abstract":"<p><p>Quantifying light elements such as carbon, nitrogen, and oxygen in a transmission electron microscope (TEM) is a challenging however essential task in biology, materials, or earth and planetary sciences. We have developed an approach that allows precise quantification by energy-dispersive X-ray spectroscopy (EDXS), using sensitive windowless silicon drift detectors and homemade Python routines for hyperspectral data processing. K-factors were determined using wedge-shaped focused ion beam sections. To correct for X-ray absorption within the sample, the sample mass thickness is determined by the-revisited-two-lines method (Morris, 1980). No beam current measurement is required. Applying this method to the K and L lines of iron, we found that the tabulated mass absorption coefficient at the energy of the iron L lines was too low. This is due to X-ray self-absorption at the iron edge. Using reference material, we experimentally determined an absorption coefficient that gave the expected results. We then analyzed the complex phyllosilicate mixture of the Orgueil meteorite. We show that the N/C ratio of organics can be obtained with an accuracy better than 5 at.% and that oxygen can be quantified accurately enough to infer the hydroxyl content of phyllosilicates.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"660-670"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141897778","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}
Yan-Ru Lin, Yao Li, Steven J Zinkle, Jose' D Arregui-Mena, M Grace Burke
{"title":"Application of Weak-Beam Dark-Field STEM for Dislocation Loop Analysis†.","authors":"Yan-Ru Lin, Yao Li, Steven J Zinkle, Jose' D Arregui-Mena, M Grace Burke","doi":"10.1093/mam/ozae067","DOIUrl":"10.1093/mam/ozae067","url":null,"abstract":"<p><p>Nanoscale dislocation loops formed by irradiation can significantly contribute to both irradiation hardening and embrittlement of materials when subjected to extreme nuclear reactor environments. This study explores the application of weak-beam dark-field (WBDF) scanning transmission electron microscopy (STEM) methods for quantitative irradiation-induced defect analysis in crystalline materials, with a specific focus on dislocation loop imaging and analysis. A high-purity Fe-5 wt% Cr model alloy was irradiated with 8 MeV Fe2+ ions at 450°C to a fluence of 8.8 × 1019 m-2, inducing dislocation loops for analysis. While transmission electron microscopy (TEM) has traditionally been the primary tool for dislocation imaging, recent advancements in STEM technology have reignited interest in using STEM for defect imaging. This study introduces and compares three WBDF STEM methods, demonstrating their effectiveness in suppressing background contrasts, isolating defect information for dislocation loop type classification, providing finer dislocation line images for small loop analysis, and presenting inside-outside contrast for identifying loop nature. Experimental findings indicate that WBDF STEM methods surpass traditional TEM approaches, yielding clearer and more detailed images of dislocation loops. The study concludes by discussing the potential applications of WBDF STEM techniques in defect analysis, emphasizing their adaptability across various material systems beyond nuclear materials.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"681-691"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141616805","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}
Sima Aslan Faal, Hamid Reza Esmaeili, Azad Teimori
{"title":"Scale Characteristics of Six Fish Species of the Genus Cyprinion (Teleostei: Cypriniformes): A Microscopic Analysis.","authors":"Sima Aslan Faal, Hamid Reza Esmaeili, Azad Teimori","doi":"10.1093/mam/ozae065","DOIUrl":"10.1093/mam/ozae065","url":null,"abstract":"<p><p>This study investigated the morphological characteristics of scales in six Cyprinion species, using light and scanning electron microscopy focusing on key features such as scale type, key scales, lateral line scales, radius/radii, rostral margin, focus, circuli, lepidonts, tubercles, and scale indices. The research analyzed the scales using ultramicroscopy and light microscopy imaging, categorizing them based on size classes and body regions. The morphological variations in scale characteristics were examined across different species, regions, and size classes. Notable findings included the tetra-sectioned form of scales, representing a unique characteristic of the Cyprinion genus. Morphological changes in scale features were observed with fish growth, particularly in the overall shape, focus shape, and size. Quantitative analysis revealed variations in average relative scale length and width among different species, regions, and size classes. The study utilized canonical discriminant analysis for multivariate assessment, classifying the species into distinct groups based on morphometric indices. The findings contribute to the understanding of scale morphology in Cyprinion species and exploring morphological variation between the examined species.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"771-792"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141727502","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":"Parameter Optimization in Cluster Identification Algorithms for Characterizing Nanoclusters in Al-Mg-Si-Cu Alloys.","authors":"MinYoung Song, Equo Kobayashi, JaeHwang Kim","doi":"10.1093/mam/ozae053","DOIUrl":"10.1093/mam/ozae053","url":null,"abstract":"<p><p>Optimization of user-defined parameters (Dmax, Nmin, order (K)) in the Density-based Spatial Clustering of Applications with Noise (DBSCAN) algorithm, used to characterize nanoclusters in Al-0.9% Mg-1.0% Si-0.3% Cu (mass %), was conducted. Ten combinations of parameters with a given K were considered for samples naturally aged (NA) and preaged (PA) at 100°C. We confirmed four types of unphysical clusters, artificially formed, by analyzing composition with size, atomic density, and atomic arrangement inside clusters. The optimum combinations minimizing those unphysical clusters were obtained for both NA and PA samples. Meanwhile, to evaluate the reliability of the optimum combination, volume rendering and isosurfacing were performed. As a result, regions of high solute concentration were confirmed, and those regions are in good agreement with the position of the clusters obtained by applying the optimum combination in DBSCAN. Furthermore, by comparing the optimum combinations with the fixed parameters widely used until now, we showed that for each dataset, considering independent parameters obtained in the same method is desirable rather than using fixed parameters. Consequently, an idea of determining the algorithm parameters for characterizing the nanoclusters in Al-Mg-Si(-Cu) alloys was introduced.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"635-649"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141446551","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}
Marko Radulović, Xingyu Li, Goran J Djuričić, Jelena Milovanović, Nataša Todorović Raković, Tijana Vujasinović, Dušan Banovac, Ksenija Kanjer
{"title":"Bridging Histopathology and Radiomics Toward Prognosis of Metastasis in Early Breast Cancer.","authors":"Marko Radulović, Xingyu Li, Goran J Djuričić, Jelena Milovanović, Nataša Todorović Raković, Tijana Vujasinović, Dušan Banovac, Ksenija Kanjer","doi":"10.1093/mam/ozae057","DOIUrl":"10.1093/mam/ozae057","url":null,"abstract":"<p><p>Tumor histomorphology is crucial for the prognostication of breast cancer outcomes because it contains histological, cellular, and molecular tumor heterogeneity related to metastatic potential. To enhance breast cancer prognosis, we aimed to apply radiomics analysis-traditionally used in 3D scans-to 2D histopathology slides. This study tested radiomics analysis in a cohort of 92 breast tumor specimens for outcome prognosis, addressing -omics dimensionality by comparing models with moderate and high feature counts, using least absolute shrinkage and selection operator for feature selection and machine learning for prognostic modeling. In the test folds, models with radiomics features [area under the curves (AUCs) range 0.799-0.823] significantly outperformed the benchmark model, which only included clinicopathological (CP) parameters (AUC = 0.584). The moderate-dimensionality model with 11 CP + 93 radiomics features matched the performance of the highly dimensional models with 1,208 radiomics or 11 CP + 1,208 radiomics features, showing average AUCs of 0.823, 0.799, and 0.807 and accuracies of 79.8, 79.3, and 76.6%, respectively. In conclusion, our application of deep texture radiomics analysis to 2D histopathology showed strong prognostic performance with a moderate-dimensionality model, surpassing a benchmark based on standard CP parameters, indicating that this deep texture histomics approach could potentially become a valuable prognostic tool.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"751-758"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141555180","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":"Application of the EBSD Technique in the Study of Porosity and Permeability in Deformation Bands in Sandstone.","authors":"Flávia Priscila Souza Afonso, Leonardo Lagoeiro, Haakon Fossen, Paola Ferreira Barbosa, Celeste Bertassoni Pinto, Camila Gomes Peçanha de Souza","doi":"10.1093/mam/ozae070","DOIUrl":"10.1093/mam/ozae070","url":null,"abstract":"<p><p>Deformation bands are common constituents of porous clastic fluid reservoirs. Various techniques have been used to study deformation band structure and the associated changes in porosity and permeability. However, the use of electron backscatter diffraction technique is limited. Thus, more information is needed regarding the crystallographic relationships between detrital crystals, which can significantly impact reservoir rock quality. We employ microscopic and microstructural investigation techniques to analyze the influence of cataclastic deformation bands on pore space. Porosity measurements of the Cretaceous Ilhas Group sandstone in NE Brazil, obtained through computerized microtomography, indicate that the undeformed domains exhibit a total porosity of up to 13%. In contrast, this porosity is slightly over 1% in the deformation bands. Scanning electron microscopy analyses revealed the presence of grain fragmentation and dissolution microstructures, along with cement-filling pre-existing pores. The electron backscatter diffraction analyses indicated extensive grain fragmentation and minimal contribution from intracrystalline plasticity as a deformation mechanism. However, the c axes of quartz crystals roughly align parallel to the orientation of the deformation band. In summary, we have confirmed and quantified the internal changes in a deformation band cluster, with grain size reduction and associated compaction as the main mechanism supported by quartz cementation.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"692-702"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141897776","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":"Employing Constrained Nonnegative Matrix Factorization for Microstructure Segmentation.","authors":"Ashish Chauniyal, Pascal Thome, Markus Stricker","doi":"10.1093/mam/ozae056","DOIUrl":"10.1093/mam/ozae056","url":null,"abstract":"<p><p>Materials characterization using electron backscatter diffraction (EBSD) requires indexing the orientation of the measured region from Kikuchi patterns. The quality of Kikuchi patterns can degrade due to pattern overlaps arising from two or more orientations, in the presence of defects or grain boundaries. In this work, we employ constrained nonnegative matrix factorization to segment a microstructure with small grain misorientations, (<1∘), and predict the amount of pattern overlap. First, we implement the method on mixed simulated patterns-that replicates a pattern overlap scenario, and demonstrate the resolution limit of pattern mixing or factorization resolution using a weight metric. Subsequently, we segment a single-crystal dendritic microstructure and compare the results with high-resolution EBSD. By utilizing weight metrics across a low-angle grain boundary, we demonstrate how very small misorientations/low-angle grain boundaries can be resolved at a pixel level. Our approach constitutes a versatile and robust tool, complementing other fast indexing methods for microstructure characterization.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"712-723"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141559122","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":"Probing Defectivity Beneath the Hydrocarbon Blanket in 2D hBN Using TEM-EELS.","authors":"Dana O Byrne, Jim Ciston, Frances I Allen","doi":"10.1093/mam/ozae064","DOIUrl":"10.1093/mam/ozae064","url":null,"abstract":"<p><p>The controlled creation and manipulation of defects in 2D materials has become increasingly popular as a means to design and tune new material functionalities. However, defect characterization by direct atomic-scale imaging is often severely limited by surface contamination due to a blanket of hydrocarbons. Thus, analysis techniques that can characterize atomic-scale defects despite the contamination layer are advantageous. In this work, we take inspiration from X-ray absorption spectroscopy and use broad-beam electron energy loss spectroscopy (EELS) to characterize defect structures in 2D hexagonal boron nitride (hBN) based on averaged fine structure in the boron K-edge. Since EELS is performed in a transmission electron microscope (TEM), imaging can be performed in-situ to assess contamination levels and other factors such as tears in the fragile 2D sheets, which can affect the spectroscopic analysis. We demonstrate the TEM-EELS technique for 2D hBN samples irradiated with different ion types and doses, finding spectral signatures indicative of boron-oxygen bonding that can be used as a measure of sample defectiveness depending on the ion beam treatment. We propose that even in cases where surface contamination has been mitigated, the averaging-based TEM-EELS technique can be useful for efficient sample surveys to support atomically resolved EELS experiments.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"650-659"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141727431","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}
Jasmine Eshun, Natalie C Lamar, Sinan G Aksoy, Sarah Akers, Benjamin Garcia, Heather Cunningham, George Chin, Jenna A Bilbrey
{"title":"Identifying Sample Provenance From SEM/EDS Automated Particle Analysis via Few-Shot Learning Coupled With Similarity Graph Clustering.","authors":"Jasmine Eshun, Natalie C Lamar, Sinan G Aksoy, Sarah Akers, Benjamin Garcia, Heather Cunningham, George Chin, Jenna A Bilbrey","doi":"10.1093/mam/ozae068","DOIUrl":"10.1093/mam/ozae068","url":null,"abstract":"<p><p>Automated particle analysis (APA) provides a vast amount of compositional data via energy-dispersive X-ray spectroscopy along with size and shape data via scanning electron microscopy for individual particles in a sample. In many instances, APA data are leveraged to support identification of the source of a sample based on the detection of particles of a specific composition. Often, the particles that provide context make up a minuscule portion of the sample. Additionally, the interpretation of complex samples can be difficult due to the diversity of compositions both in the mixture and within a particle. In this work, we demonstrate a method to compute and cluster similarity graphs that describe inter-particle relationships within a sample using a multi-modal few-shot learning neural network. As a proof-of-concept, we show that samples known to have been exposed to gunshot residue can be distinguished from samples occasionally mistaken for gunshot residue. Our workflow builds upon standard APA techniques and data processing methods to unveil additional information in a readily interpretable and quantitatively comparable format.</p>","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"741-750"},"PeriodicalIF":2.9,"publicationDate":"2024-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141860221","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":"Correction to: Low-Temperature X-ray Microanalysis Sheds New Light on Mineral Nutrition Aspects of Insect Leaf Galling.","authors":"","doi":"10.1093/mam/ozae030","DOIUrl":"10.1093/mam/ozae030","url":null,"abstract":"","PeriodicalId":18625,"journal":{"name":"Microscopy and Microanalysis","volume":" ","pages":"633"},"PeriodicalIF":2.9,"publicationDate":"2024-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140892493","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}