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In situ TEM and EELS analysis of Ni catalytic nanoparticles for dry reforming of methane Ni纳米颗粒催化甲烷干重整的原位TEM和EELS分析
IF 2.2 3区 工程技术
Micron Pub Date : 2025-08-12 DOI: 10.1016/j.micron.2025.103894
Yutain Han , Xiaobo Peng , Hideki Abe , Ayako Hashimoto
{"title":"In situ TEM and EELS analysis of Ni catalytic nanoparticles for dry reforming of methane","authors":"Yutain Han ,&nbsp;Xiaobo Peng ,&nbsp;Hideki Abe ,&nbsp;Ayako Hashimoto","doi":"10.1016/j.micron.2025.103894","DOIUrl":"10.1016/j.micron.2025.103894","url":null,"abstract":"<div><div>Dry reforming of methane (DRM, CH<sub>4</sub>+CO<sub>2</sub>→2CO+2H<sub>2</sub>) involves production of CO and H<sub>2</sub> using two kinds of greenhouse gases, CH<sub>4</sub> and CO<sub>2</sub>, without requiring an expensive and complicated gas separation process. Using a developed specimen holder, we observed the Ni nanoparticles on Al<sub>2</sub>O<sub>3</sub> supports during DRM catalysis through <em>in situ</em> transmission electron microscopy and electron energy loss spectroscopy by tracking each individual nanoparticle to elucidate the structural and chemical features of the working catalyst under practical conditions. The average value of the Ni L<sub>3</sub>/L<sub>2</sub> intensity ratio, which relates to the valence state (i.e., oxidation state), shows that the Ni nanoparticles were oxidized at 450 °C in the DRM gas and then slightly reduced at 650 °C as a whole. But the Ni nanoparticles actually exhibited a range of oxidation states under DRM conditions. In particular, some oxidized Ni nanoparticles were reduced at 550 °C and drastically changed in size, becoming much smaller. Compared with <em>in situ</em> observations under only CH<sub>4</sub> gas, without CO<sub>2</sub>, oxidation of the Ni surface was directly and locally observed, presumably due to the reaction with Al<sub>2</sub>O<sub>3</sub> and the decomposition of CO<sub>2</sub>. Additionally, the reduction of oxidized Ni was mainly due to hydrogen-containing gases. Furthermore, carbon deposition was observed at 350 °C, containing both amorphous carbon and graphene layers.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"199 ","pages":"Article 103894"},"PeriodicalIF":2.2,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144852742","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}
引用次数: 0
High-throughput determination of sample visibility in liquid-phase SEM via Monte Carlo simulations 通过蒙特卡罗模拟的液相扫描电镜样品可见性的高通量测定
IF 2.2 3区 工程技术
Micron Pub Date : 2025-08-12 DOI: 10.1016/j.micron.2025.103895
Dian Yu , Mia L. San Gabriel , Stas Dogel , Keryn Lian , Jane Y. Howe
{"title":"High-throughput determination of sample visibility in liquid-phase SEM via Monte Carlo simulations","authors":"Dian Yu ,&nbsp;Mia L. San Gabriel ,&nbsp;Stas Dogel ,&nbsp;Keryn Lian ,&nbsp;Jane Y. Howe","doi":"10.1016/j.micron.2025.103895","DOIUrl":"10.1016/j.micron.2025.103895","url":null,"abstract":"<div><div>We developed a Monte Carlo simulation workflow to investigate the effects of sample thickness, membrane thickness, sample composition, and incident electron energy on the visibility of samples in liquid-phase scanning electron microscopy based on electron-transparent Si<sub>3</sub>N<sub>4</sub> membranes. By using a thin wedge as the sample geometry and non-uniform spacing of the scan points, we avoided the need to generate numerous geometries for each configuration and reduced the computation time by up to 2 orders of magnitude. Quantitative analyses of the threshold current for visible contrast and the spatial resolution revealed that secondary electrons may visualize thin samples more effectively than BSEs at incident electron energies down to 3 keV when aided by efficient in-lens detectors and Si<sub>3</sub>N<sub>4</sub> membranes with a thickness of 20 nm or lower. The simulations also supported the trends of decreasing spatial resolution with the thickness of both the membrane and the sample material.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"199 ","pages":"Article 103895"},"PeriodicalIF":2.2,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144863331","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}
引用次数: 0
Anther and pollen development and their relevance in delimiting the Neotropical species of the Malveae tribe (Malvaceae) 花药和花粉的发育及其与新热带马尔科马尔科种划分的关系
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-23 DOI: 10.1016/j.micron.2025.103892
Jefferson Freitas de Oliveira , Mariana Ferreira Alves , Massimo Giuseppe Bovini , Karen L.G. De Toni
{"title":"Anther and pollen development and their relevance in delimiting the Neotropical species of the Malveae tribe (Malvaceae)","authors":"Jefferson Freitas de Oliveira ,&nbsp;Mariana Ferreira Alves ,&nbsp;Massimo Giuseppe Bovini ,&nbsp;Karen L.G. De Toni","doi":"10.1016/j.micron.2025.103892","DOIUrl":"10.1016/j.micron.2025.103892","url":null,"abstract":"<div><div>Recent phylogenetic studies support the monophyly of the tribe Malveae, with floral morphology providing the main basis for clade delimitation. However, embryological data remain underexplored despite their potential contribution to phylogenetic inference. In this study, we analyzed the embryological development of 12 Neotropical Malveae species to investigate anther ontogeny, microsporogenesis, and microgametogenesis. Floral buds and flowers at different stages of development were collected, and standard methodologies for optical microscopy and confocal laser scanning microscopy were employed. The anther wall pattern corresponds to the dicotyledonous type, with unistratified epidermis, endothecium with ring thickening, an ephemeral middle layer, and a binuclear tapetum of the nonsyncytial invasive type. Microsporogenesis involves simultaneous meiosis, resulting in tetrahedral tetrads. After microspore maturation, microgametogenesis begins, with microspore undergoing asymmetric mitosis, giving rise to vegetative and generative cells. Mature pollen grains are bicellular and contain an abundance of starch. The uniformity in the developmental patterns observed among the analyzed species suggests the presence of shared characteristics that may serve as phylogenetic markers. This strengthens the evidence of a close evolutionary relationship among members of the Malveae tribe and highlights the importance of ontogeny in understanding phylogenetic relationships and delimiting clades in Malvaceae.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103892"},"PeriodicalIF":2.5,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144704249","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}
引用次数: 0
Performance verification of the "ghost"-free tomographic reconstruction method QURT 无虚影层析重建方法QURT的性能验证
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-20 DOI: 10.1016/j.micron.2025.103889
Norio Baba , Hiroyuki Ishikawa , Miki Ito
{"title":"Performance verification of the \"ghost\"-free tomographic reconstruction method QURT","authors":"Norio Baba ,&nbsp;Hiroyuki Ishikawa ,&nbsp;Miki Ito","doi":"10.1016/j.micron.2025.103889","DOIUrl":"10.1016/j.micron.2025.103889","url":null,"abstract":"<div><div>We recently proposed a novel tomographic reconstruction method called the quantisation unit reconstruction technique (QURT) that reconstructs a tomogram by arranging grey-level quantisation units in three-dimensional image space through unique discrete processing. QURT significantly reduces artificial image “ghost” generation caused by the “missing-wedge” and the number of projection images, which are common limitations of conventional methods. Unlike other recently developed advanced methods, such as compressed sensing, QURT does not require any parameter adjustments or modeling based on prior knowledge but requires only a series of projection images and tilt-angle data. It does not select the processing target because it exploits the inherent constraints of projection theory. In this study, the practical performance and resolution of QURT were quantitatively evaluated in both real and frequency domains using Fourier ring correlation and other metrics in simulations with fine test patterns. Even in the presence of the missing-wedge, QURT generated almost no ghost image outside the test pattern region, considerably suppressing the artifacts. This advanced property was experimentally validated by applying HAADF-STEM tomography to analyse a catalyst sample (Pd/CeO<sub>2</sub>–ZrO<sub>2</sub>–Al<sub>2</sub>O<sub>3</sub>), which was particularly sensitive to ghost image generation inside pores. QURT clearly revealed the pore structure without compromising the low-contrast Al regions and without generating ghost images, even at a tilt step angle of up to 4°. In EDXS tomography, QURT also reconstructed a 3D elemental map even from a small number of 22 tilt series signal maps with the missing-wedges.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103889"},"PeriodicalIF":2.5,"publicationDate":"2025-07-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144703448","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}
引用次数: 0
Optimizing sample preparation for In situ TEM heating studies of aluminum alloys 铝合金原位TEM加热研究中样品制备的优化
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-20 DOI: 10.1016/j.micron.2025.103891
Longhui Chen , Chunhui Liu , Jianshi Yang , Peipei Ma , Jun He
{"title":"Optimizing sample preparation for In situ TEM heating studies of aluminum alloys","authors":"Longhui Chen ,&nbsp;Chunhui Liu ,&nbsp;Jianshi Yang ,&nbsp;Peipei Ma ,&nbsp;Jun He","doi":"10.1016/j.micron.2025.103891","DOIUrl":"10.1016/j.micron.2025.103891","url":null,"abstract":"<div><div>Aluminum-copper-lithium (Al-Cu-Li) alloy is a key structural material in the aerospace field. Its mechanical properties are closely related to the dynamic evolution of T<sub>1</sub> phase during the aging process. To accurately capture this dynamic process, the <em>in situ</em> transmission electron microscope (TEM) combined with the microelectromechanical system (MEMS) heating chip was used to observe the T<sub>1</sub> precipitation behavior in an Al-Cu-Li alloy in real time. All experimental samples were solution treated at 510 °C for 30 min and water quenched externally, and then heated to 180 °C on a MEMS heater chip at a heating rate of 1 °C/s. This study presents an improved sample preparation and transfer protocol to mitigate Ga infiltration. High-angle annular dark-field scanning TEM (HAADF-STEM) and energy-dispersive X-ray spectroscopy (EDS) were used to evaluate the effects of preparation methods, transfer techniques, and sample thickness (80–300 nm) on gallium (Ga) and platinum (Pt) contamination and precipitation behavior. The results show that Ga segregation, in the form of ∼10 nm intragranular particles and grain boundary enrichment, significantly distorts the intrinsic precipitation of T<sub>1</sub> phases. However, combining an external transfer method with low-energy ion milling at an accelerating voltage of 3 kV effectively suppresses Ga/Pt contamination. Furthermore, sample thickness critically influences precipitation kinetics in Al-Cu-Li alloys: sub-100 nm samples exhibit surface-driven abnormal coarsening of T<sub>1</sub> precipitates, while samples exceeding 250 nm suffer from reduced imaging resolution due to limited electron transparency. A thickness range of 150–200 nm optimally balances resolution fidelity with representative precipitation dynamics.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103891"},"PeriodicalIF":2.5,"publicationDate":"2025-07-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144695356","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}
引用次数: 0
Electron beam-induced damage in tellurium dioxide 电子束致二氧化碲损伤
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-19 DOI: 10.1016/j.micron.2025.103875
Cathal Cassidy
{"title":"Electron beam-induced damage in tellurium dioxide","authors":"Cathal Cassidy","doi":"10.1016/j.micron.2025.103875","DOIUrl":"10.1016/j.micron.2025.103875","url":null,"abstract":"<div><div>In this work, structural and compositional changes in <span><math><mi>α</mi></math></span>-TeO<sub>2</sub>, also known as paratellurite, were studied as function of 300 kV electron beam exposure. Firstly, the mean free path for electron scattering in <span><math><mi>α</mi></math></span>-TeO<sub>2</sub> was measured, to enable local specimen thickness measurement and estimation of scattering probabilities. A value of <span><math><mi>λ</mi></math></span> = 155 nm <span><math><mo>±</mo></math></span> 6 nm was obtained, for the specific experimental conditions as detailed in the text. Then, high resolution TEM images and EEL spectra were acquired as a function of electron beam exposure, and the material changes were recorded. Differing behaviors, ranging from complete specimen etching, reduction to elemental tellurium, or no effect, were observed depending on the specific specimen and illumination conditions that were employed. Markedly different material changes were observed under broad illumination (TEM mode) and focused probe illumination (STEM mode). In STEM mode, a threshold effect in the applied electron dose rate was observed. For the conditions employed, with a beam current of 45 pA or less, there was no significant damage to the specimen. In TEM mode, it was observed that specimen damage was enhanced at the periphery of the illuminating electron beam area, and proceeded more rapidly in thicker regions of the specimen. Under certain illumination conditions, a stable network of tellurium oxide and elemental tellurium was formed. While only a small fraction of the parameter space governing electron-beam induced damage has been investigated, the results to date indicate that specimen charging and induced electric fields are the dominant mechanism of damage in this insulating material.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103875"},"PeriodicalIF":2.5,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144713075","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}
引用次数: 0
Modeling the partially detected backside reflectance of transparent substrates in reflectance microspectroscopy 在反射微光谱学中对透明衬底部分检测的背面反射率进行建模
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-19 DOI: 10.1016/j.micron.2025.103878
Julian Schwarz , Jan Dick , Susanne Beuer , Mathias Rommel , Andreas Hutzler
{"title":"Modeling the partially detected backside reflectance of transparent substrates in reflectance microspectroscopy","authors":"Julian Schwarz ,&nbsp;Jan Dick ,&nbsp;Susanne Beuer ,&nbsp;Mathias Rommel ,&nbsp;Andreas Hutzler","doi":"10.1016/j.micron.2025.103878","DOIUrl":"10.1016/j.micron.2025.103878","url":null,"abstract":"<div><div>Thick transparent substrates are a key component for transmissive thin film optical filters and optoelectronics. In optical characterization of such substrates, light reflected from the backside — whether fully or partially detected — interferes with light directly reflected from the substrate’s front side. Herein, we introduce a straightforward approach for microspectroscopic measurements, with lateral dimensions in the micrometer range, to reliably assess the amount of measured backside reflectance. Therefore, geometric calculations based on micrographs, substrate thickness and refractive index, as well as magnification of the applied objective lens are utilized as input parameters. Additionally, we account for the influence of the numerical aperture, which is essential for accurate determination of the properties of thin films coated on thick transparent substrates. Compared to simulations completely incorporating or entirely neglecting the backside reflectance, our approach significantly reduces the mean squared error between measurement and model in the case of partially detected backside reflectance. After demonstrating the capabilities of our approach to accurately identify the amount of backside reflectance detected for a variety of bare transparent substrate materials, thicknesses, and objective lenses, we prove the capacity to determine the thickness of silicon nitride and silicon nitride/silicon oxide layers on glass substrates with high consistency to complementary STEM/EDX measurements even for large numerical apertures.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103878"},"PeriodicalIF":2.5,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144694305","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}
引用次数: 0
Accessible and thorough magnetic field mapping of TEMs using a commercial Hall-sensor and TEM automation for in situ magnetic experiments 使用商用霍尔传感器和TEM自动化进行原位磁实验的TEM易于访问和彻底的磁场测绘
IF 2.2 3区 工程技术
Micron Pub Date : 2025-07-19 DOI: 10.1016/j.micron.2025.103877
Sivert Dagenborg, Kristian Tveitstøl, Iryna Zelenina, Gregory Nordahl , Magnus Nord
{"title":"Accessible and thorough magnetic field mapping of TEMs using a commercial Hall-sensor and TEM automation for in situ magnetic experiments","authors":"Sivert Dagenborg,&nbsp;Kristian Tveitstøl,&nbsp;Iryna Zelenina,&nbsp;Gregory Nordahl ,&nbsp;Magnus Nord","doi":"10.1016/j.micron.2025.103877","DOIUrl":"10.1016/j.micron.2025.103877","url":null,"abstract":"<div><div>For imaging and quantitative <em>in situ</em> experiments of magnetic materials in the transmission electron microscope (TEM), knowing the external magnetic field over the sample position and the parameters affecting it is crucial. Calibrating this thoroughly also requires an efficient method for sampling a large set of parameters. This work presents accessible solutions to both these problems, using a commercial Hall-sensor soldered onto a custom printed circuit board then inserted into a TEM biasing holder. This is enhanced by TEM automation using open-source Python scripting, enabling thorough and effective experimental measurements. The magnetic field in the sample position was measured over a range of positions, tilts and lens excitations for three different TEMs: The JEOL JEM-2100F. JEOL JEM 2100,and JEOL JEM-ARM200F. In objective lens-off mode these have remnant fields of up to respectively 19.19<!--> <!-->mT, 15.24<!--> <!-->mT and 8.95<!--> <!-->mT, all oriented downwards in the column. The magnetic fields had a strong decay in x- and y-positions of up to 13.1%. The objective lens gave a highly linear response to lens excitation up to 27.5% of max excitation. For the 2100F and 2100, fully exciting the objective lens caused a significant change in remnant field of above 4<!--> <!-->mT which was counteracted with lens relaxation. The image aberration corrector lenses in the ARM200F caused changes of 0.2<!--> <!-->mT. This magnetic field mapping enables quantitative <em>in situ</em> experiments with magnetic fields up to 2<!--> <!-->T.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103877"},"PeriodicalIF":2.2,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144780031","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}
引用次数: 0
Application of scanning electron microscopy and energy-dispersive x-ray spectroscopy in the study of bronze disease on ancient copper-based artifacts 扫描电子显微镜和能量色散x射线光谱学在古代铜制品青铜病研究中的应用
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-18 DOI: 10.1016/j.micron.2025.103890
Laura A. Battista , Maryam Golozar , Ehsan Nikbin , Dian Yu , Masha Stanko , Laura Lipcsei , Jane Howe , Doug Perovic
{"title":"Application of scanning electron microscopy and energy-dispersive x-ray spectroscopy in the study of bronze disease on ancient copper-based artifacts","authors":"Laura A. Battista ,&nbsp;Maryam Golozar ,&nbsp;Ehsan Nikbin ,&nbsp;Dian Yu ,&nbsp;Masha Stanko ,&nbsp;Laura Lipcsei ,&nbsp;Jane Howe ,&nbsp;Doug Perovic","doi":"10.1016/j.micron.2025.103890","DOIUrl":"10.1016/j.micron.2025.103890","url":null,"abstract":"<div><div>Bronze disease is a severe type of degradation in ancient copper-based artifacts and poses challenges to their preservation. This “disease” is an active cyclic corrosion process primarily caused by chlorine, oxygen and moisture. Products formed during this process, such as cuprous chloride (CuCl), continue to spread across the artifact’s surface until all available oxygen is consumed, resulting in irreversible destruction. Bronze disease is difficult to distinguish from other corrosion processes, leading to inaccurate assessments of the degradation mechanisms affecting the artifact. Combined scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS) is a viable method for analyzing bronze disease in ancient artifacts and for differentiating it from other forms of degradation. This study investigated suspected bronze disease on a Chinese cast bronze vessel dating from the 11th – 10th century BCE, part of the collection at the Royal Ontario Museum in Toronto, Canada. Corrosion product sampled from the vessel using two different methods, was chemically and topographically analyzed using SEM-EDS. The first method involved the removal of corrosion product using a scalpel, resulting in the collection of mixed particles. The second method, involving the creation of replicas, utilized an adhesive to directly remove the corrosion product, capturing the particles in their original locations. The sampled material contained copper and chlorine, consistent with the presence of bronze disease, though further work is required for confirmation. Although both techniques can investigate bronze disease, the replica technique offers a more promising approach, as it enables more precise, site-specific analysis of the corrosion product.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103890"},"PeriodicalIF":2.5,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144662404","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}
引用次数: 0
Chemical analysis of spherical and fiber structures on lithium-ion batteries anodes using SEM, EDS and SIMS 利用SEM、EDS和SIMS对锂离子电池阳极的球形结构和纤维结构进行化学分析
IF 2.5 3区 工程技术
Micron Pub Date : 2025-07-17 DOI: 10.1016/j.micron.2025.103886
Gudrun Wilhelm , Ute Golla-Schindler , Timo Bernthaler , Ute Kaiser , Gerhard Schneider
{"title":"Chemical analysis of spherical and fiber structures on lithium-ion batteries anodes using SEM, EDS and SIMS","authors":"Gudrun Wilhelm ,&nbsp;Ute Golla-Schindler ,&nbsp;Timo Bernthaler ,&nbsp;Ute Kaiser ,&nbsp;Gerhard Schneider","doi":"10.1016/j.micron.2025.103886","DOIUrl":"10.1016/j.micron.2025.103886","url":null,"abstract":"<div><div>Scanning electron microscopy (SEM), when combined with secondary ion mass spectrometry (SIMS) enables spatially resolved detection of lithium. The time-of-flight detector allows the precise identification of each fragment. Quantitative results are obtained through inductively coupled plasma optical emission spectrometry (ICP-OES). This innovative technique combination provides new insights into the chemical composition of three morphologies found on the anode surface in a long-term cycled lithium-ion battery, compared to a reference battery. The three morphologies are a) fine-grained precipitations, b) fiber structures and c) spherical particles. The fine-grained precipitations are inhomogeneous and composed of Li, F, O, P, Cu and S. Their thickness ranges from 50 to 100 nm. The fiber structures appear in three different shapes: round, helically twisted and flattened with a thicker rim. Their length spans from 1 to 14 µm and their width varies between 50 and 900 nm. The fibers contain the same elements as the fine-grained precipitations. The spherical particles predominantly range from 300 to 600 nm in size and have a fine-grained surface. They consist of Li, F, O, Si, Al and S. Also traces of Ni, Mn and Co are detected with ICP-OES. SIMS mappings and mass spectra of small regions of interest suggest that the fine-grained precipitations contain LiF, probably LiOH, Li- and Cu-oxides and phosphate compounds. The fiber structures contain no phosphate but additionally Li- and Cu-phosphides whereas the spherical particles consist of a silicate or aluminosilicate structure combined with LiF. Further studies are required to clarify the sequence of formation.</div></div>","PeriodicalId":18501,"journal":{"name":"Micron","volume":"198 ","pages":"Article 103886"},"PeriodicalIF":2.5,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144687541","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}
引用次数: 0
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