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Simultaneous observation of multiple interferograms with Mach-Zehnder type electron interferometer on a 1.2-MV field-emission transmission electron microscope. 在 1.2-MV 场发射透射电子显微镜上使用马赫-泽恩德型电子干涉仪同时观测多个干涉图。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae030
Tetsuya Akashi, Yoshio Takahashi, Ken Harada

We developed a Mach-Zehnder type electron interferometer (MZ-EI) that enables simultaneous observation of interferograms created at multiple output locations on a 1.2-MV field-emission transmission electron microscope. This MZ-EI is composed of two single-crystal thin films, a lens located between the single-crystal thin films and imaging lenses. By comparing interferograms created by electron waves travelling through different beam paths, we found that the relative phase difference was caused by phase modulation passing through the single crystals and by aberrations and defocus values of the lenses. We also confirmed that the relative phase difference can be controlled using the tilted illumination method.

我们开发了一种马赫-泽恩德型电子干涉仪(MZ-EI),可以同时观测 1.2-MV 场发射透射电子显微镜上多个输出位置产生的干涉图。这种 MZ-EI 由两个单晶薄膜、位于单晶薄膜之间的透镜和成像透镜组成。通过比较电子波通过不同光束路径产生的干涉图,我们发现相对相位差是由通过单晶的相位调制以及透镜的像差和散焦值造成的。我们还证实,相对相位差可以用倾斜照明法来控制。
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引用次数: 0
Total third-degree variation for noise reduction in atomic-resolution STEM images. 用于原子分辨率 STEM 图像降噪的总三度变异。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae031
Kazuaki Kawahara, Ryo Ishikawa, Shun Sasano, Naoya Shibata, Yuichi Ikuhara

Scanning Transmission Electron Microscopy (STEM) enables direct determination of atomic arrangements in materials and devices. However, materials such as battery components are weak for electron beam irradiation, and low electron doses are required to prevent beam-induced damages. Noise removal is thus essential for precise structural analysis of electron-beam-sensitive materials at atomic resolution. Total square variation (TSV) regularization is an algorithm that exhibits high noise removal performance. However, the use of the TSV regularization term leads to significant image blurring and intensity reduction. To address these problems, we here propose a new approach adopting L2 norm regularization based on higher-order total variation. An atomic-resolution STEM image can be approximated as a set of smooth curves represented by quadratic functions. Since the third-degree derivative of any quadratic function is 0, total third-degree variation (TTDV) is suitable for a regularization term. The application of TTDV for denoising the atomic-resolution STEM image of CaF2 observed along the [001] zone axis is shown, where we can clearly see the Ca and F atomic columns without compromising image quality.

扫描透射电子显微镜(STEM)可直接测定材料和设备中的原子排列。然而,电池组件等材料对电子束辐照的耐受性较弱,需要较低的电子剂量以防止电子束引起的损坏。因此,要以原子分辨率对电子束敏感材料进行精确的结构分析,必须去除噪声。总平方变异(TSV)正则化是一种具有高去噪性能的算法。然而,使用 TSV 正则化项会导致图像严重模糊和强度降低。为了解决这些问题,我们在此提出了一种基于高阶总变化的 L2 规范正则化新方法。原子分辨率 STEM 图像可近似为一组由二次函数表示的平滑曲线。由于任何二次函数的三阶导数都是 0,因此总三阶变异(TTDV)适合作为正则化项。图中显示了应用 TTDV 对沿 [001] 区轴线观察到的 CaF2 原子分辨率 STEM 图像进行去噪的情况,在不影响图像质量的情况下,我们可以清楚地看到 Ca 和 F 原子列。
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引用次数: 0
Near-field electron ptychography using full-field structured illumination. 使用全场结构照明的近场电子层析成像技术。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae035
Hirokazu Tamaki, Koh Saitoh

A new configuration for near-field ptychography using a full-field illumination with a structured electron beam is proposed. A structured electron beam illuminating the entire field of view is scanned over the specimen, and a series of in-line holograms formed in the near-field region below the specimen are collected. The structured beam is generated by a conductive film with random openings, which ensures high stability and coherence of the beam. Observation in the near-field region reduces the beam concentration that occurs in the far-field region, which contributes to accurate recording of the beam intensity with a finite dynamic range of the detectors. The use of full-field illumination prevents the accumulation of errors caused by concatenating the local structures, which is the method used in conventional reconstruction. Since all holograms are obtained from the entire field of view, they have uniform multiplicity in terms of specimen information within the field of view. This contributes to robust and efficient reconstruction for a large field of view. The proposed method was tested using both simulated and experimental holograms. For the simulated holograms, the reconstruction of the specimen transmission function was achieved with an error less than 1/3485 of the wavelength. The method was further validated using experimental holograms obtained from MgO particles. The reconstructed phase transmission function of the specimen was consistent with the specimen structure and was equivalent to a mean inner potential of 13.53±0.16 V on the MgO particle, which is in close agreement with previously reported values.

本文提出了一种利用结构电子束全场照明的近场全息成像新结构。照射整个视场的结构电子束在试样上扫描,收集试样下方近场区域形成的一系列在线全息图。结构光束由带有随机开口的导电薄膜产生,这确保了光束的高稳定性和相干性。在近场区域进行观测可减少远场区域出现的光束集中现象,从而有助于在探测器有限的动态范围内精确记录光束强度。使用全场照明可防止因串联局部结构而导致的误差累积,而串联局部结构是传统重建中使用的方法。由于所有全息图都是从整个视场获得的,因此视场内的样本信息具有统一的多重性。这有助于对大视场进行稳健高效的重建。我们使用模拟全息图和实验全息图对所提出的方法进行了测试。在模拟全息图中,试样传输函数的重建误差小于波长的 1/3485。使用氧化镁颗粒获得的实验全息图进一步验证了该方法。重建后的试样相透射函数与试样结构一致,相当于氧化镁颗粒上的平均内电势为 V,这与之前报道的数值非常接近。
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引用次数: 0
Surface sensitivity of atomic-resolution secondary electron imaging. 原子分辨率二次电子成像的表面灵敏度。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae041
Koh Saitoh, Teppei Oyobe, Keisuke Igarashi, Takeshi Sato, Hiroaki Matsumoto, Hiromi Inada, Takahiko Endo, Yasumitsu Miyata, Rei Usami, Taishi Takenobu

The surface sensitivity of high-resolution secondary electron (SE) imaging is examined using twisted bilayers of MoS2 stacked at an angle of 30°. High-resolution SE images of the twisted bilayer MoS2 show a honeycomb structure composed of Mo and S atoms, elucidating the monolayer structure of MoS2. Simultaneously captured annular dark-field scanning transmission electron microscope images from the same region show the projected structure of the two layers. That is, the SE images from the bilayer MoS2 selectively visualize the surface monolayer. It is noted that the SE yields from the surface monolayer are approximately three times higher than those from the second monolayer, likely attributable to attenuation when SEs emitted from the second layer traverse the surface layer. The surface sensitivity of high-resolution SE imaging is examined using twisted bilayers of MoS2 stacked at an angle of 30°. It was found that the SE images of the MoS2 bilayer visualize the surface monolayer approximately three times more intensely than the second monolayer.

利用以 30 度角堆叠的扭曲双层 MoS2,研究了高分辨率二次电子(SE)成像的表面灵敏度。扭曲双层 MoS2 的高分辨率 SE 图像显示了由 Mo 原子和 S 原子组成的蜂巢结构,从而阐明了 MoS2 的单层结构。从同一区域同时拍摄的环形暗场扫描透射电子显微镜图像显示了两层的投影结构。也就是说,双层 MoS2 的 SE 图像可选择性地观察到表面单层。值得注意的是,来自表面单层的 SE 产率大约是来自第二单层的 SE 产率的 3 倍,这可能是由于从第二层发射的 SE 穿过表面层时产生了衰减。小摘要:本研究利用由表层和基底组成的最薄系统--MoS2 双层膜,对原子分辨率二次电子成像的表面灵敏度进行了研究。研究发现,二次电子对表面单层原子排列的观察强度是第二层的三倍。
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引用次数: 0
Surface potential distribution of resist exposed by electron beam and the non-charging exposure conditions. 电子束和非充电曝光条件下光刻胶的表面电位分布。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae044
Masatoshi Kotera, Yoshinobu Kono

In this study, we experimentally analyzed the charging phenomenon when an insulating resist film on a conductive layer formed on bulk glass is irradiated by electron beams (EBs). To quantify the charging potential induced, an electrostatic force microscope device was installed in the scanning electron microscope sample chamber, and potential distributions formed under various exposure conditions were obtained. Based on the results obtained, a model for charge accumulation within the sample, explaining positive and negative charging and their transitions, was developed. At an EB acceleration voltage of 30 kV, the following observations were made: 'global charging' could be avoided by applying -5 V to the sample. Regarding 'local charging' near the exposure area of the EB, at low exposure doses, emission of secondary electrons from the sample surface induced positive charging, while the accumulation of incident electrons within the sample induced negative charging. At exposure doses where the effects of both are balanced, the sample exhibited zero potential, revealing the appearance of the 'first zero-cross exposure dose'. At higher exposure doses, the sample transitions from negative to positive as the exposure dose increases due to the electron-beam-induced conduction, resulting in the so-called second zero-cross exposure dose. The exposure dose dependence of the charging potential distribution at various acceleration voltages was obtained. In particular, we found that at an acceleration voltage of 0.6 kV, the sample surface is not charged even when exposed to small to very large doses of EBs.

在这项研究中,我们通过实验分析了在大块玻璃上形成的导电层上的绝缘抗蚀膜在电子束照射下的充电现象。为了量化引起的充电电势,我们在扫描电子显微镜样品室中安装了静电力显微镜装置,并获得了在不同照射条件下形成的电势分布。根据所获得的结果,建立了样品内部的电荷积累模型,解释了正负电荷及其转换。在 30 千伏的电子束加速电压下,得出了以下结论:对样品施加 -5V 电压可避免 "整体充电"。至于电子束照射区域附近的 "局部充电",在低照射剂量下,样品表面发射的二次电子会引起正充电,而入射电子在样品内部的积累则会引起负充电。在两者影响平衡的曝光剂量下,样品显示出零电位,出现了 "第一个零交叉曝光剂量"。在较高的曝光剂量下,由于电子束诱导传导,随着曝光剂量的增加,样品会从负电位转变为正电位,这就是所谓的 "第二次零交叉曝光剂量"。我们获得了不同加速电压下充电电势分布的曝光剂量依赖性。我们特别发现,在加速电压为0.6千伏时,即使暴露在小剂量到超大剂量的电子束中,样品表面也不会带电。
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引用次数: 0
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 : 2025-01-30 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
Development of a localized surface plasmon-enhanced electron beam-pumped nanoscale light source for electron beam excitation-assisted optical microscopy. 开发用于电子束激发辅助光学显微镜的局部表面等离子体增强电子束泵浦纳米级光源。
Pub Date : 2025-01-30 DOI: 10.1093/jmicro/dfae043
Atsushi Nakamura, Shunpei Shiba, Kei Hosomi, Atsushi Ono, Yoshimasa Kawata, Wataru Inami

We have demonstrated localized surface plasmon (LSP)-enhanced cathodoluminescence (CL) from an atomic layer deposition-grown Al2O3/ZnO/Al2O3 heterostructure to develop a bright nanometer-scale light source for an electron beam excitation-assisted optical microscope. Three types of metals, Ag, Al and Au, were compared, and an 181-fold enhancement of CL emission was achieved with Ag nanoparticles, with the plasmon resonance wavelength close to the emission wavelength energy of ZnO. The enhanced emission is plausibly attributed to LSP/exciton coupling. However, it is also attributed to an increase in coupling efficiency with penetration depth and also to an increase in light extraction efficiency by grading the refractive indices at the heterostructure.

我们展示了原子层沉积(ALD)生长的 Al2O3/ZnO/Al2O3 异质结构的局部表面等离子体(LSP)增强阴极荧光(CL),为电子束激发辅助(EXA)光学显微镜开发了一种明亮的纳米级光源。通过对 Ag、Al 和 Au 三种金属进行比较,Ag 纳米粒子(NPs)的 CL 发射增强了 181 倍,等离子共振波长接近 ZnO 的发射波长能量。发射增强可能归因于 LSP/激子耦合。不过,这也归因于耦合效率随穿透深度的增加而提高,以及异质结构的折射率分级提高了光萃取效率。
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引用次数: 0
Momentum-resolved EELS and CL study on 1D-plasmonic crystal prepared by FIB method. 用 FIB 方法制备的一维等离子晶体的动量分辨 EELS 和 CL 研究。
Pub Date : 2024-12-05 DOI: 10.1093/jmicro/dfae022
Akira Yasuhara, Masateru Shibata, Wakaba Yamamoto, Izzah Machfuudzoh, Sotatsu Yanagimoto, Takumi Sannomiya

We investigate a one-dimensional plasmonic crystal using momentum-resolved electron energy-loss spectroscopy (EELS) and cathodoluminescence (CL) techniques, which are complementary in terms of available optical information. The plasmonic crystal sample is fabricated from large aluminum grains through the focused ion beam method. This approach allows curving nanostructures with high crystallinity, providing platforms for detailed analysis of plasmonic nanostructures using both EELS and CL. The momentum-resolved EELS visualizes dispersion curves outside the light cone, confirming the existence of the surface plasmon polaritons and local modes, while the momentum-resolved CL mapping analysis identified these surface plasmon polaritons and local modes. Such synergetic approach of two electron-beam techniques offers full insights into both radiative and non-radiative optical properties in plasmonic or photonic structures.

我们利用动量分辨电子能量损失光谱(EELS)和阴极发光(CL)技术研究了一种一维等离子晶体(1D PlC),这两种技术在可用光学信息方面具有互补性。PlC 样品是通过聚焦离子束 (FIB) 方法从大型铝晶粒中制造出来的。这种方法可实现具有高结晶度的弯曲纳米结构,为使用 EELS 和 CL 对等离子纳米结构进行详细分析提供了平台。动量分辨 EELS 可观察到光锥外的色散曲线,证实了表面等离子体极化子 (SPP) 和局部模式的存在,而动量分辨 CL 绘图分析则确定了这些 SPP 和局部模式。通过两种电子束技术的协同作用,可以全面了解等离子体或光子结构中的辐射和非辐射光学特性。
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引用次数: 0
Role of lipids in the organization of tight junction. 脂质在紧密连接组织中的作用。
Pub Date : 2024-12-05 DOI: 10.1093/jmicro/dfae039
Junichi Ikenouchi, Kenta Shigetomi

Cell membrane structures are supramolecular complexes that require the ordered assembly of membrane proteins and lipids. The morphology of various cell adhesion structures in multicellular organisms, such as those between epithelial cells, neural synapses and immune synapses, was initially described through electron microscopic analyses. Subsequent studies aimed to catalog their constituent proteins, which encompass transmembrane cell adhesion molecules, cytoskeletal proteins and scaffolding proteins that bind the two components. However, the diversity of plasma membrane lipids and their significance in the organization of cell adhesion structures were underappreciated until recently. It is now understood that phase separation of lipids and liquid-liquid phase separation of proteins are important driving forces for such self-assembly. In this review, we summarized recent findings on the role of lipids as scaffolds for supramolecular complexes using tight junctions in epithelial cells as an example.

细胞膜结构是一种超分子复合体,需要膜蛋白和脂质的有序组装。多细胞生物体中各种细胞粘附结构的形态,如上皮细胞之间、神经突触和免疫突触之间的粘附结构,最初是通过电子显微镜分析来描述的。随后的研究旨在对它们的组成蛋白进行编目,其中包括跨膜细胞粘附分子、细胞骨架蛋白和结合这两种成分的支架蛋白。然而,直到最近,人们才意识到质膜脂质的多样性及其在细胞粘附结构组织中的重要性。现在人们了解到,脂质的相分离和蛋白质的液-液相分离是这种自组装的重要驱动力。在这篇综述中,我们以上皮细胞的紧密连接为例,总结了有关脂质作为超分子复合物支架的作用的最新发现。
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引用次数: 0
Visualization of Bacillus subtilis spore structure and germination using quick-freeze deep-etch electron microscopy. 利用速冻深描电子显微镜观察枯草芽孢杆菌孢子的结构和萌发。
Pub Date : 2024-12-05 DOI: 10.1093/jmicro/dfae023
Kiran Jalil, Yuhei O Tahara, Makoto Miyata

Bacterial spores, known for their complex and resilient structures, have been the focus of visualization using various methodologies. In this study, we applied quick-freeze and replica electron microscopy techniques, allowing observation of Bacillus subtilis spores in high-contrast and three-dimensional detail. This method facilitated visualization of the spore structure with enhanced resolution and provided new insights into the spores and their germination processes. We identified and described five distinct structures: (i) hair-like structures on the spore surface, (ii) spike formation on the surface of lysozyme-treated spores, (iii) the fractured appearance of the spore cortex during germination, (iv) potential connections between small vesicles and the core membrane and (v) the evolving surface structure of nascent vegetative cells during germination.

细菌孢子以其复杂而富有弹性的结构而闻名,一直是使用各种方法进行可视化研究的重点。在这项研究中,我们应用了速冻和复制电子显微镜技术,从而观察到了枯草杆菌孢子的高对比度和三维细节。这种方法提高了孢子结构的可视化分辨率,为我们了解孢子及其萌发过程提供了新的视角。我们确定并描述了五种不同的结构:(i) 孢子表面的毛发状结构;(ii) 溶菌酶处理过的孢子表面形成的穗状结构;(iii) 孢子皮层在萌发过程中的断裂外观;(iv) 小囊泡与核心膜之间的潜在连接;(v) 新生无性细胞在萌发过程中不断演变的表面结构。
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引用次数: 0
期刊
Microscopy (Oxford, England)
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