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Precise positional alignment of atom-resolved HAADF images of heteroepitaxial interface with low signal-to-noise ratio. 低信噪比异质外延界面原子分辨 HAADF 图像的精确定位。
Pub Date : 2024-08-23 DOI: 10.1093/jmicro/dfae038
Kohei Aso, Yoshifumi Oshima

Heteroepitaxial interfaces are important because they determine the performance of devices such that career mobility is sensitive to the distribution of roughness, strain and composition at the interface. High-angle annular dark field imaging in scanning transmission electron microscopy has been utilized to capture them at an atomic scale. For precise identification of atomic column positions, a technique has been proposed to average multiple image frames taken at a high scanning rate by their positional alignment for increasing signal-to-noise ratio. However, the positional alignment between frames is sometimes incorrectly estimated because of the almost perfect periodic structure at the interfaces. Here, we developed an approach for precise positional alignment, where the images are first aligned by two consecutive images and then are aligned more precisely against the integrated image of the first alignment. We demonstrated our method by applying it to the heterointerface of Si0.8Ge0.2 (Si: silicon, Ge: germanium) epitaxial thin films on a Si substrate.

异质外延界面非常重要,因为它们决定了器件的性能,例如职业迁移率对界面的粗糙度、应变和成分分布非常敏感。扫描透射电子显微镜中的高角度环形暗场成像技术可用于捕捉原子尺度的界面。为了精确识别原子柱的位置,有人提出了一种技术,通过位置对齐来平均以高扫描速率拍摄的多个图像帧,以提高信噪比。然而,由于界面上几乎完美的周期性结构,帧间的位置对齐有时会估计错误。在此,我们开发了一种精确位置对齐的方法,即首先通过两幅连续图像对齐图像,然后根据第一幅对齐图像的综合图像进行更精确的对齐。我们将这种方法应用于硅基底上的 Si0.8Ge0.2(Si:硅,Ge:锗)外延薄膜的异质界面,并对其进行了演示。
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引用次数: 0
Electron holography observation of electron spin polarization around charged insulating wire. 带电绝缘线周围电子自旋极化的电子全息观察。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfad056
Takafumi Sato, Keiko Shimada, Zentaro Akase, Hideyuki Magara, Takeshi Tomita, Daisuke Shindo

We report direct observation by electron holography of the spin polarization of electrons in a vacuum region around a charged SiO2 wire coated with Pt-Pd. Irradiating the SiO2 wire with 300 keV electrons caused the wire to become positively charged due to the emission of secondary electrons. The spin polarization of these electrons interacting with the charged wire was observed in situ using a phase reconstruction process under an external magnetic field. The magnetic field of the spin-polarized electrons was simulated taking into account the distribution of secondary electrons and the effect of the external magnetic field.

我们报道了用电子全息术直接观察到电子自旋极化在真空区周围的带电SiO2线包覆Pt-Pd。用300 kev的电子照射SiO2导线,由于二次电子的发射,使导线带正电。在外加磁场作用下,用相重构法原位观察了这些电子与带电导线相互作用的自旋极化。考虑二次电子的分布和外加磁场的影响,对自旋极化电子的磁场进行了模拟。
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引用次数: 0
Three-dimensional nanostructure analysis of non-stained Nafion in fuel-cell electrode by combined ADF-STEM tomography. 利用 ADF-STEM 层析成像技术对燃料电池电极中未染色的 Nafion 进行三维纳米结构分析。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfae002
Takuji Ube

The polymer electrolyte fuel cell (PEFC) is one of the strongest candidates for a next-generation power source for vehicles which do not emit CO2 gas as exhaust gas. The key factor in PEFCs is the nano-scaled electrochemical reactions that take place on the catalyst material and an ionomer supported by a carbon support. However, because the nano-scaled morphological features of the key materials in the catalyst compound cannot be observed clearly by transmission electron microscopy, improvement of PEFC performance had been approached by an imaginal schematic diagram based on an electrochemical analysis. In this study, we revealed the nano-scaled morphological features of the PEFC electrode in three dimensions and performed a quantitative analysis of the nanostructure by the newly developed 'Combined ADF-STEM tomography technique'. This method combines information from plural annular darkfield detectors with different electron collection angles and can emphasize the difference of the electron scattering intensity between the ionomer and carbon in the cross-sectional image of the reconstructed three-dimensional (3D) data. Therefore, this segmentation method utilizing image contrast does not require a high electron beam current like that used in energy dispersive X-ray analysis, and thus is suitable for electron beam damage-sensitive materials. By eliminating the process of manually determining the thresholds for obtaining classified component data from grayscale data, the obtained 3D structures have sufficient accuracy to allow quantitative analysis and specify the nano-scaled structural parameters directly related to power generation characteristics.

聚合物电解质燃料电池(PEFC)是不排放二氧化碳(CO2)废气的汽车下一代动力源的最有力候选者之一。PEFC 的关键因素是催化剂材料和由碳支撑物支撑的离子体上发生的纳米级电化学反应。然而,由于透射电子显微镜无法清晰地观察到催化剂化合物中关键材料的纳米级形态特征,因此人们一直通过基于电化学分析的想象示意图来提高 PEFC 的性能。在本研究中,我们通过新开发的 "ADF-STEM 层析成像组合技术 "揭示了 PEFC 电极的三维纳米尺度形态特征,并对纳米结构进行了定量分析。该方法结合了多个具有不同电子收集角度的 ADF 探测器的信息,可以在重建的三维数据的横截面图像中强调离子体和碳之间电子散射强度的差异。因此,这种利用图像对比度的分割方法不需要像 EDX 分析那样的高电子束电流,因此适用于对电子束损伤敏感的材料。由于省去了从灰度数据中获取分类成分数据的人工确定阈值的过程,所获得的三维结构具有足够的准确性,可以进行定量分析,并明确与发电特性直接相关的纳米级结构参数。
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引用次数: 0
Observation and quantitative analysis of dislocations in steel using electron channeling contrast imaging method with precise control of electron beam incident direction. 利用精确控制电子束入射方向的电子通道对比成像方法观测和定量分析钢中的位错。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfad061
Takashige Mori, Takafumi Amino, Chie Yokoyama, Shunsuke Taniguchi, Takayuki Yonezawa, Akira Taniyama

Electron channeling contrast imaging (ECCI) was applied by precisely controlling the primary electron beam incident direction of the crystal plane in scanning electron microscope (SEM), and the dislocation contrast in steel materials was investigated in detail via SEM/ECCI. The dislocation contrast was observed near a channeling condition, where the incident electron beam direction of the crystal plane varied, and the backscattered electron intensity reached a local minimum. Comparing the dislocation contrasts in the visualized electron channeling contrast (ECC) images and transmission electron microscope (TEM) images, the positions of all dislocation lines were coincident. During the SEM/ECCI observation, the dislocation contrast varied depending on the incident electron beam direction of the crystal plane and accelerating voltages, and optimal conditions existed. When the diffraction condition g and the Burgers vector b of dislocation satisfied the condition g⸱b = 0, the screw dislocation contrast in the ECC image disappeared. An edge dislocation line was wider than a screw dislocation line. Thus, the SEM/ECCI method can be used for dislocation characterization and the strain field evaluation around dislocation, like the TEM method. The depth information of SEM/ECCI, where the channeling condition is strictly satisfied, can be obtained from dislocation contrast deeper than 5ξg, typically used for depth of SEM/ECCI.

通过精确控制扫描电子显微镜(SEM)中晶体平面的主电子束入射方向,应用电子沟道对比成像(ECCI)技术,通过 SEM/ECCI 详细研究了钢铁材料中的位错对比。在晶面入射电子束方向变化的沟道条件附近观察到了位错对比,反向散射电子强度达到了局部最小值。对比可视化电子扫描对比(ECC)图像和透射电子显微镜(TEM)图像中的位错对比,所有位错线的位置都是重合的。在 SEM/ECCI 观察过程中,位错对比度随晶体平面入射电子束方向和加速电压的不同而变化,并存在最佳条件。当衍射条件 g 和位错的布尔矢量 b 满足 g b = 0 条件时,ECC 图像中的螺旋位错对比度消失。边缘位错线比螺旋位错线宽。因此,与 TEM 方法一样,SEM/ECCI 方法可用于位错表征和位错周围的应变场评估。在严格满足沟道条件的情况下,SEM/ECCI 的深度信息可从通常用于 SEM/ECCI 深度的 5ξg 以上的位错对比中获得。
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引用次数: 0
Artifactual atomic displacements on surfaces using annular dark-field images with image simulation. 利用环形暗视野图像和图像模拟在表面上伪造原子位移。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfae001
Shunsuke Kobayashi, Kousuke Ooe, Kei Nakayama, Akihide Kuwabara

We investigated artifactual atomic displacements on a Pt (111) surface using annular dark-field (ADF) scanning transmission electron microscopy images under ideal conditions with multi-slice image simulation. Pt atomic columns on the surface exhibited artifact displacement. The bright spots shifted slightly toward the interior of the crystal, indicating that ADF imaging underestimates atomic distance measurements on the crystal surface. Multiple peak fitting is an effective method for determining the positions of bright spots and obtaining more accurate atomic positions while reducing the impact of surface-related artifacts. This is important for the measurement of interatomic distances on crystal surfaces, particularly for catalyst particles.

我们利用环形暗场(ADF)扫描透射电子显微镜(STEM)图像,在理想条件下进行多片图像模拟,研究了铂(111)表面上的人造原子位移。表面上的铂原子柱出现了人工位移。亮点略微向晶体内部移动,表明 ADF 成像低估了晶体表面原子距离的测量值。多峰拟合是确定亮点位置和获得更精确原子位置的有效方法,同时还能减少表面相关伪影的影响。这对于测量晶体表面的原子间距离,尤其是催化剂颗粒的原子间距离非常重要。
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引用次数: 0
A simple coordinate transformation method for quickly locating the features of interest in TEM samples. 在 TEM 样品中快速定位相关特征的简单坐标转换方法。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfae009
Mingzhi Zeng, Wenzhao Wang, Yang Yin, Changlin Zheng

We developed a simple coordinate transformation method for quickly locating features of interest (FOIs) of samples in transmission electron microscope (TEM). The method is well suited for conducting sample searches in aberration-corrected scanning/transmission electron microscopes (S/TEM), where the survey can be very time-consuming because of the limited field of view imposed by the highly excited objective lens after fine-tuning the aberration correctors. For implementation, a digital image of the sample and the TEM holder was captured using a simple stereo-optical microscope. Naturally presented geometric patterns on the holder were referenced to construct a projective transformation between the electron and optical coordinate systems. The test results demonstrated that the method was accurate and required no electron microscope or specimen holder modifications. Additionally, it eliminated the need to mount the sample onto specific patterned TEM grids or deposit markers, resulting in universal applications for most TEM samples, holders and electron microscopes for fast FOI identification. Furthermore, we implemented the method into a Gatan script for graphical-user-interface-based step-by-step instructions. Through online communication, the script enabled real-time navigation and tracking of the motion of samples in TEM on enlarged optical images with a panoramic view.

我们开发了一种简单的坐标变换方法,用于快速定位透射电子显微镜(TEM)中样品的感兴趣特征(FOI)。该方法非常适合在像差校正扫描/透射电子显微镜(S/TEM)中进行样品搜索,由于微调像差校正器后高度激发的物镜会造成有限的视场,因此在这种显微镜中进行样品搜索非常耗时。在实施过程中,使用简单的立体光学显微镜捕捉样品和 TEM 支架的数字图像。以支架上自然呈现的几何图形为参照,构建电子坐标系和光学坐标系之间的投影变换。测试结果表明,该方法准确无误,且无需改装电子显微镜或试样架。此外,该方法无需将样品安装到特定图案的 TEM 网格或沉积标记上,因此可普遍应用于大多数 TEM 样品、支架和电子显微镜,从而实现快速 FOI 识别。此外,我们还将该方法应用到了基于图形用户界面的分步指导 Gatan 脚本中。通过在线交流,该脚本可在放大的全景光学图像上实时导航和跟踪 TEM 中样品的运动。
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引用次数: 0
High-precision charge analysis in a catalytic nanoparticle by electron holography. 利用电子全息技术对催化纳米粒子进行高精度电荷分析。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfae018
Ryotaro Aso, Yoshihiro Midoh, Toshiaki Tanigaki, Yasukazu Murakami

The charge state of supported metal catalysts is the key to understand the elementary processes involved in catalytic reactions. However, high-precision charge analysis of the metal catalysts at the atomic level is experimentally challenging. To address this critical challenge, high-sensitivity electron holography has recently been successfully applied for precisely measuring the elementary charges on individual platinum nanoparticles supported on a titanium dioxide surface. In this review, we introduce the latest advancements in high-precision charge analysis and discuss the mechanisms of charge transfer at the metal-support interface. The development of charge measurements is entering a new era, and charge analyses under conditions closer to practical working environments, such as real-time, real-space, and reactive gas environments, are expected to be realized in the near future.

支撑金属催化剂的电荷状态是了解催化反应基本过程的关键。然而,在原子水平上对金属催化剂进行高精度电荷分析在实验上具有挑战性。为了应对这一重大挑战,最近成功应用高灵敏度电子全息技术精确测量了二氧化钛表面支撑的单个铂纳米粒子上的基本电荷。在这篇综述中,我们将介绍高精度电荷分析的最新进展,并讨论金属-支撑界面的电荷转移机制。电荷测量的发展正进入一个新时代,在更接近实际工作环境的条件下,如实时、真实空间和反应气体环境下的电荷分析有望在不久的将来实现。
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引用次数: 0
Development of an integrated high-voltage electron microscope-gas chromatograph-quadrupole mass spectrometer system for the operando analysis of catalytic gas reactions. 开发用于催化气体反应操作分析的高压电子显微镜-气相色谱仪-四极杆质谱仪集成系统。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfae010
Longshu Tang, Tetsuo Higuchi, Shigeo Arai, Hiromochi Tanaka, Shunsuke Muto

This paper describes the development of a gas chromatography-quadrupole mass spectrometry system attached to a differential-pumping-type environmental cell of the reaction science high-voltage electron microscopy instrument at Nagoya University to distinguish unambiguously between different gas species with the same mass-to-charge ratio. Several model experiments were used to verify the efficacy of the newly proposed system, confirming its ability to analyse the atomic-level structural changes during heterogeneous catalysts and the associated gas-reaction kinetics simultaneously, providing new insights into operando measurements in the field of environmental transmission electron microscopy. Graphical Abstract.

本文介绍了与名古屋大学反应科学高压电子显微镜仪器的差分泵式环境池相连接的气相色谱-四极杆质谱系统的开发情况,该系统能够明确区分具有相同质量电荷比的不同气体种类。通过几个模型实验验证了新系统的功效,证实它能够同时分析异相催化剂过程中的原子级结构变化和相关的气体反应动力学,为环境透射电子显微镜领域的操作测量提供了新的见解。
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引用次数: 0
Removal of phase residues in electron holography. 去除电子全息摄影中的相位残留。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfad062
Yoshio Takahashi, Tetsuya Akashi, Toshiaki Tanigaki

Electron holography provides quantitative phase information regarding the electromagnetic fields and the morphology of micro- to nano-scale samples. A phase image reconstructed numerically from an electron hologram sometimes includes phase residues, i.e. origins of unremovable phase discontinuities, which make it much more difficult to quantitatively analyze local phase values. We developed a method to remove the residues in a phase image by a combination of patching local areas of a hologram and denoising based on machine learning. The small patches for a hologram, which were generated using the spatial frequency information of the own fringe patterns, were pasted at each residue point by an algorithm based on sparse modeling. After successive phase reconstruction, the phase components with no dependency on the vicinity were filtered out by Gaussian process regression. We determined that the phase discontinuities that appeared around phase residues were removed and the phase distributions of an atomic resolution phase image of a Pt nanoparticle were sufficiently restored.

电子全息技术可提供有关电磁场和微米至纳米级样品形态的定量相位信息。从电子全息图中以数字方式重建的相位图像有时会包含相位残留,即不可移动的相位不连续的起源,这使得定量分析局部相位值变得更加困难。我们开发了一种方法,通过对全息图的局部区域进行修补和基于机器学习的去噪相结合的方法来去除相位图像中的残留物。全息图的小补丁是利用自身条纹图案的空间频率信息生成的,通过基于稀疏建模的算法将其粘贴到每个残差点上。在连续的相位重建之后,通过高斯过程回归滤除与附近区域无关的相位成分。我们确定,相位残基周围出现的相位不连续性已被消除,铂纳米粒子原子分辨率相位图像的相位分布得到了充分恢复。
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引用次数: 0
Magnetic field observation in a magnetic tunnel junction by scanning transmission electron microscopy. 用扫描透射电子显微镜观察磁隧道结中的磁场。
Pub Date : 2024-07-30 DOI: 10.1093/jmicro/dfad063
Yuji Kohno, Takehito Seki, Shun Tsuruoka, Shinobu Ohya, Naoya Shibata

A magnetic tunnel junction (MTJ) consists of two ferromagnetic layers separated by a thin insulating layer. MTJs show tunnel magnetoresistance effect, where the resistance in the direction perpendicular to the insulator layer drastically changes depending on the magnetization directions (parallel or antiparallel) in the ferromagnetic layers. However, direct observation of local magnetizations inside MTJs has been challenging. In this study, we demonstrate direct observation of magnetic flux density distribution inside epitaxially grown Fe/MgO/Fe layers using differential phase contrast scanning transmission electron microscopy. By utilizing newly developed tilt-scan averaging system for suppressing diffraction contrasts, we clearly visualize parallel and antiparallel states of ferromagnetic layers at nanometer resolution.

磁隧道结(MTJ)由两个被薄绝缘层隔开的铁磁层组成。MTJ 具有隧道磁阻效应,在垂直于绝缘层的方向上,电阻会根据铁磁层的磁化方向(平行或反平行)发生急剧变化。然而,直接观察 MTJ 内部的局部磁化一直是个挑战。在本研究中,我们展示了利用差分相衬扫描透射电子显微镜直接观察外延生长的铁/氧化镁/铁层内部磁通密度分布的方法。通过利用新开发的倾斜扫描平均系统抑制衍射对比,我们以纳米分辨率清晰地观察到了铁磁层的平行和反平行状态。
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引用次数: 0
期刊
Microscopy (Oxford, England)
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