The crystallization process of the eutectic composition of GdAlO_3-Al_2O_3 from the amorphous phase prepared by rapid-quenching of melt that leads to the formation of a cantaloupe skin-like microstructure was investig...The crystallization process of the eutectic composition of GdAlO_3-Al_2O_3 from the amorphous phase prepared by rapid-quenching of melt that leads to the formation of a cantaloupe skin-like microstructure was investigated using focused ion-beam scanning electron microscopy (FIB-SEM) and high-resolution transmission electron microscopy (HR-TEM).The amorphous films were heat-treated at temperatures between 1000 °C and 1500 °C for up to 30min to form the eutectic phases of GdAlO_3 and Al_2O_3.The GdAlO_3 and Al_2O_3 crystal phases that formed from the amorphous phase were identified by FIB-SEM and HR-TEM.Both components began to crystallize and grow from the amorphous phase separately at different temperatures.The formation process of these crystal phases was different from that of the ordinary eutectic microstructure solidified from the GdAlO_3-Al_2O_3 system.Therefore,the observed structure is termed "eutectic-like" for distinction.The microstructures formed from the amorphous phases at sufficiently high temperatures consisted of ultra-fine microstructures of individually crystallized components and were similar to ordinary eutectic microstructures.By heat-treating the amorphous films at 1500 °C for either 2 min,8min or 30min,the ultra-fine components of GdAlO_3 and Al_2O_3 were found to crystallize following a eutectic-like stage after 8min of heat treatment.展开更多
FIB-SEM(Focused Ion Beam-Scanning Electron Microscope)双束系统是集聚焦离子束和扫描电子显微镜与一体的系统,其最大的优势是可以实现离子束切割或微加工的同时用电子束实时观察的功能。主要介绍FIB-SEM双束系统在PCB及IC载板缺陷...FIB-SEM(Focused Ion Beam-Scanning Electron Microscope)双束系统是集聚焦离子束和扫描电子显微镜与一体的系统,其最大的优势是可以实现离子束切割或微加工的同时用电子束实时观察的功能。主要介绍FIB-SEM双束系统在PCB及IC载板缺陷检测中的常见应用,如盲孔孔底分析、杂物失效分析和晶体结构分析。展开更多
The three-dimensional(3D)morphology,anatomy,and in-situ chemical composition analysis of fossils are crucial for systematic paleontology and determining their phylogenetic positions.Scanning electron microscopy(SEM)co...The three-dimensional(3D)morphology,anatomy,and in-situ chemical composition analysis of fossils are crucial for systematic paleontology and determining their phylogenetic positions.Scanning electron microscopy(SEM)coupled with energy-dispersive X-ray spectroscopy(EDS),offers valuable structural and chemical information for the analysis of fossils.However,its primary limitation is the restriction to two-dimensional surface data,which limits the exploration of fossils’3D complexities.Conversely,3D X-ray microscopy(3D-XRM),also known as a novel form of micro-computed tomography(micro-CT)facilitates the non-destructive 3D reconstruction of fossil specimens.Nevertheless,it lacks the capability to provide in-situ compositional data.Acknowledging the constraints inherent in these individual techniques,and in response to the evolving requirements of paleontological research,this study introduces an integrated approach that combines 3D-XRM with EDS-coupled focused ion beam scanning electron microscopy(FIB-SEM).This innovative strategy is designed to synergize the advantages of both techniques,thereby addressing challenges that conventional methods cannot.It enables the rapid identification of regions of interest(ROI)within fossil specimens at micrometer resolution.Subsequently,this method collects detailed data on both 3D structures and chemical compositions at the nanometer scale for the identified ROI.This integrated approach represents a significant advancement in paleontological and geological research methodologies,promising to meet the increasing demands of these fields.展开更多
聚焦离子束扫描电子显微镜(Focused Ion Beam Scanning Electron Microscope,FIB-SEM)双束系统结合了扫描电子显微镜与聚焦离子束系统的优势。基于该系统的高分辨率、原位加工及观测的特点,研究了它在缺陷与像元解剖分析、透射电镜样品...聚焦离子束扫描电子显微镜(Focused Ion Beam Scanning Electron Microscope,FIB-SEM)双束系统结合了扫描电子显微镜与聚焦离子束系统的优势。基于该系统的高分辨率、原位加工及观测的特点,研究了它在缺陷与像元解剖分析、透射电镜样品制备以及电路修复等方面的应用。详细介绍了用FIB-SEM系统定位问题像元的方法和修复电路的具体过程,并阐明了它对红外焦平面探测器研制的重要作用。该系统是高性能红外探测器研制过程中不可或缺的重要表征手段。展开更多
Copper extraction from chalcopyrite is challenging,because acid dissolution is slow,occurring incongruently via a complex three-step reaction mechanism.Silver has been known to catalyse copper extraction from chalcopy...Copper extraction from chalcopyrite is challenging,because acid dissolution is slow,occurring incongruently via a complex three-step reaction mechanism.Silver has been known to catalyse copper extraction from chalcopyrite since the 1970's;yet the mechanism remains controversial.Microcharacterisation of experimental products obtained under optimal leaching conditions(50-150μm chalcopyrite grains in ferric/ferrous-sulfate solution with a redox potential around 500 mV vs.Ag/AgCl,approximately 1ppm Ag;[Ag]6.4×10^(−6)mol/L;70℃;4 days)highlights the heterogeneity of the reaction:µm-thick layers of a porous copper-sulfide with variable composition formed both in cracks within,and on the surface of the chalcopyrite grains.There is no evidence for formation of Ag-rich phases(Ag_(2)S_((s)),Ag_((s)^(0))).The fundamental three-step reaction mechanism remains the same with or without added silver;silver merely accelerates the initial dissolution step.An integrated model for the catalytic effect of silver is proposed that incorporates recent advances in the reactivity of sulfide minerals.The initial reaction follows a‘Fluid-Induced Solid State Diffusion Mechanism’,where diffusion of Fe in the chalcopyrite lattice is driven towards the surface by its rapid removal into solution,resulting in a Fe-deficient surface layer.The large Ag+ion,relative to Cu+/Fe3+,diffuses into this Fe-deficient surface layer and accelerates chalcopyrite dissolution in the subsequent step,whereby chalcopyrite is replaced by copper sulfides via an interface coupled dissolution reprecipitation reaction as a consequence of the sulfide-rich micro-environment at the mineral surface.Effective Ag+recycling is key to the catalytic effect of silver,and occurs as a result of the strong affinity of Ag+for bisulfide ligands accumulating at the surface of dissolving chalcopyrite.展开更多
Understanding the degradation phenomenon of proton exchange membrane fuel cells under electrochemical cycling requires an analysis of the porous carbon support structure.Key factors contributing to this phenomenon inc...Understanding the degradation phenomenon of proton exchange membrane fuel cells under electrochemical cycling requires an analysis of the porous carbon support structure.Key factors contributing to this phenomenon include changes in the total porosity and viable surface area for electrochemical reactions.Electron tomography-based serial section imaging using focused ion beam-scanning electron microscopy(FIB-SEM)can elucidate this phenomenon at a nanoscale resolution.However,this highresolution tomographic analysis requires a huge image dataset and manual inputs in rule-based workflows;these requirements are time-consuming and often cause experimental difficulties and unreliable interpretations.We propose a deep learning-empowered approach comprising a two-step automated process for image interpolation and semantic segmentation to address the practical issues encountered in FIB-SEM electron tomography.An optimally trained interpolation model can reduce the image data requirement by more than 95%to analyze the structural degradation of carbon supports after electrochemical cycling while maintaining the reliability obtained in conventional tomographic analysis with several hundred images.Because the subsequent image segmentation model excludes a complicated manual filtering process,the relevant structural parameters can be reliably measured without human bias.Our sparse-section imaging-based deep learning process can allow cost-efficient analysis and reliable measurement of the degree of cycling-induced carbon corrosion.展开更多
基金part of the study under the "Human Resource Development Center for Economic Region Leading Industry" Projectsupported by the Ministry of Education,Science & Technology(MEST)by the National Research Foundation of Korea(NRF)
文摘The crystallization process of the eutectic composition of GdAlO_3-Al_2O_3 from the amorphous phase prepared by rapid-quenching of melt that leads to the formation of a cantaloupe skin-like microstructure was investigated using focused ion-beam scanning electron microscopy (FIB-SEM) and high-resolution transmission electron microscopy (HR-TEM).The amorphous films were heat-treated at temperatures between 1000 °C and 1500 °C for up to 30min to form the eutectic phases of GdAlO_3 and Al_2O_3.The GdAlO_3 and Al_2O_3 crystal phases that formed from the amorphous phase were identified by FIB-SEM and HR-TEM.Both components began to crystallize and grow from the amorphous phase separately at different temperatures.The formation process of these crystal phases was different from that of the ordinary eutectic microstructure solidified from the GdAlO_3-Al_2O_3 system.Therefore,the observed structure is termed "eutectic-like" for distinction.The microstructures formed from the amorphous phases at sufficiently high temperatures consisted of ultra-fine microstructures of individually crystallized components and were similar to ordinary eutectic microstructures.By heat-treating the amorphous films at 1500 °C for either 2 min,8min or 30min,the ultra-fine components of GdAlO_3 and Al_2O_3 were found to crystallize following a eutectic-like stage after 8min of heat treatment.
文摘FIB-SEM(Focused Ion Beam-Scanning Electron Microscope)双束系统是集聚焦离子束和扫描电子显微镜与一体的系统,其最大的优势是可以实现离子束切割或微加工的同时用电子束实时观察的功能。主要介绍FIB-SEM双束系统在PCB及IC载板缺陷检测中的常见应用,如盲孔孔底分析、杂物失效分析和晶体结构分析。
基金founded by the National Natural Science Foundation of China(No.42022010)the National Key Research and Development Program of China(No.2022YFF0800100)the CAS Interdisciplinary Innovation Team(No.JCTD-2020-18)and the Youth Innovation Promotion Association.
文摘The three-dimensional(3D)morphology,anatomy,and in-situ chemical composition analysis of fossils are crucial for systematic paleontology and determining their phylogenetic positions.Scanning electron microscopy(SEM)coupled with energy-dispersive X-ray spectroscopy(EDS),offers valuable structural and chemical information for the analysis of fossils.However,its primary limitation is the restriction to two-dimensional surface data,which limits the exploration of fossils’3D complexities.Conversely,3D X-ray microscopy(3D-XRM),also known as a novel form of micro-computed tomography(micro-CT)facilitates the non-destructive 3D reconstruction of fossil specimens.Nevertheless,it lacks the capability to provide in-situ compositional data.Acknowledging the constraints inherent in these individual techniques,and in response to the evolving requirements of paleontological research,this study introduces an integrated approach that combines 3D-XRM with EDS-coupled focused ion beam scanning electron microscopy(FIB-SEM).This innovative strategy is designed to synergize the advantages of both techniques,thereby addressing challenges that conventional methods cannot.It enables the rapid identification of regions of interest(ROI)within fossil specimens at micrometer resolution.Subsequently,this method collects detailed data on both 3D structures and chemical compositions at the nanometer scale for the identified ROI.This integrated approach represents a significant advancement in paleontological and geological research methodologies,promising to meet the increasing demands of these fields.
文摘聚焦离子束扫描电子显微镜(Focused Ion Beam Scanning Electron Microscope,FIB-SEM)双束系统结合了扫描电子显微镜与聚焦离子束系统的优势。基于该系统的高分辨率、原位加工及观测的特点,研究了它在缺陷与像元解剖分析、透射电镜样品制备以及电路修复等方面的应用。详细介绍了用FIB-SEM系统定位问题像元的方法和修复电路的具体过程,并阐明了它对红外焦平面探测器研制的重要作用。该系统是高性能红外探测器研制过程中不可或缺的重要表征手段。
基金supporting this work through an ARC linkage grant(LP190101230)Part of this work was funded by ARC DP220100500+2 种基金The authors acknowledge the use of the instruments and scientific and technical assistance at the Monash Centre for Electron Microscopy,Monash University,a Microscopy Australia(ROR:042mm0k03)facility supported by NCRISThis research used equipment funded by Australian Research Council grant(s)(LE200100132,LE110100223).
文摘Copper extraction from chalcopyrite is challenging,because acid dissolution is slow,occurring incongruently via a complex three-step reaction mechanism.Silver has been known to catalyse copper extraction from chalcopyrite since the 1970's;yet the mechanism remains controversial.Microcharacterisation of experimental products obtained under optimal leaching conditions(50-150μm chalcopyrite grains in ferric/ferrous-sulfate solution with a redox potential around 500 mV vs.Ag/AgCl,approximately 1ppm Ag;[Ag]6.4×10^(−6)mol/L;70℃;4 days)highlights the heterogeneity of the reaction:µm-thick layers of a porous copper-sulfide with variable composition formed both in cracks within,and on the surface of the chalcopyrite grains.There is no evidence for formation of Ag-rich phases(Ag_(2)S_((s)),Ag_((s)^(0))).The fundamental three-step reaction mechanism remains the same with or without added silver;silver merely accelerates the initial dissolution step.An integrated model for the catalytic effect of silver is proposed that incorporates recent advances in the reactivity of sulfide minerals.The initial reaction follows a‘Fluid-Induced Solid State Diffusion Mechanism’,where diffusion of Fe in the chalcopyrite lattice is driven towards the surface by its rapid removal into solution,resulting in a Fe-deficient surface layer.The large Ag+ion,relative to Cu+/Fe3+,diffuses into this Fe-deficient surface layer and accelerates chalcopyrite dissolution in the subsequent step,whereby chalcopyrite is replaced by copper sulfides via an interface coupled dissolution reprecipitation reaction as a consequence of the sulfide-rich micro-environment at the mineral surface.Effective Ag+recycling is key to the catalytic effect of silver,and occurs as a result of the strong affinity of Ag+for bisulfide ligands accumulating at the surface of dissolving chalcopyrite.
基金supported by the Technology Innovation Program(No.20011712)funded by the Ministry of Trade,Industry,and Energy(MOTIE,Korea)a National Research Foundation of Korea(NRF)grant funded by the Ministry of Science and ICT(MSIT)(No.2022M3J1A108538),Korea+2 种基金the support of the Nano&Material Technology Development Program through the National Research Foundation of Korea(NRF)funded by the Ministry of Science and ICT(RS-2024-00444986,50%)the Institute for Basic Science(IBS-R036-D1)。
文摘Understanding the degradation phenomenon of proton exchange membrane fuel cells under electrochemical cycling requires an analysis of the porous carbon support structure.Key factors contributing to this phenomenon include changes in the total porosity and viable surface area for electrochemical reactions.Electron tomography-based serial section imaging using focused ion beam-scanning electron microscopy(FIB-SEM)can elucidate this phenomenon at a nanoscale resolution.However,this highresolution tomographic analysis requires a huge image dataset and manual inputs in rule-based workflows;these requirements are time-consuming and often cause experimental difficulties and unreliable interpretations.We propose a deep learning-empowered approach comprising a two-step automated process for image interpolation and semantic segmentation to address the practical issues encountered in FIB-SEM electron tomography.An optimally trained interpolation model can reduce the image data requirement by more than 95%to analyze the structural degradation of carbon supports after electrochemical cycling while maintaining the reliability obtained in conventional tomographic analysis with several hundred images.Because the subsequent image segmentation model excludes a complicated manual filtering process,the relevant structural parameters can be reliably measured without human bias.Our sparse-section imaging-based deep learning process can allow cost-efficient analysis and reliable measurement of the degree of cycling-induced carbon corrosion.
