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Depth sectioning using environmental and atomic-resolution STEM. 利用环境和原子分辨率 STEM 进行深度剖析。
Pub Date : 2024-04-08 DOI: 10.1093/jmicro/dfae005
Masaki Takeguchi, Ayako Hashimoto, Kazutaka Mitsuishi

(Scanning) transmission electron microscopy (TEM) images of samples in gas and liquid media are acquired with an environmental cell (EC) via silicon nitride membranes. The ratio of sample signal against the background is a significant factor for resolution. Depth-sectioning scanning TEM (STEM) is a promising technique that enhances the signal for a sample embedded in a matrix. It can increase the resolution to the atomic level, thereby enabling EC-STEM applications in important areas. This review introduces depth-sectioning STEM and its applications to high-resolution EC-STEM imaging of samples in gases and in liquids.

(通过氮化硅膜的环境电池(EC)获取气体和液体介质中样品的(扫描)透射电子显微镜(TEM)图像。样品信号与背景的比率是影响分辨率的重要因素。深度截面扫描 TEM(STEM)是一种很有前途的技术,它能增强嵌入基质中的样品的信号。它能将分辨率提高到原子水平,从而使 EC-STEM 应用于重要领域。本综述将介绍深度截面 STEM 及其在气体和液体样品高分辨率 EC-STEM 成像中的应用。
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引用次数: 0
In-situ TEM study from the perspective of holders. 持子视角下的原位透射电镜研究。
Pub Date : 2024-04-08 DOI: 10.1093/jmicro/dfad055
Toshie Yaguchi, Mia L San Gabriel, Ayako Hashimoto, Jane Y Howe

During the in situ transmission electron microscopy (TEM) observations, the diverse functionalities of different specimen holders play a crucial role. We hereby provide a comprehensive overview of the main types of holders, associated technologies and case studies pertaining to the widely employed heating and gas heating methods, from their initial developments to the latest advancement. In addition to the conventional approaches, we also discuss the emergence of holders that incorporate a micro-electro-mechanical system (MEMS) chip for in situ observations. The MEMS technology offers a multitude of functions within a single chip, thereby enhancing the capabilities and versatility of the holders. MEMS chips have been utilized in environmental-cell designs, enabling customized fabrication of diverse shapes. This innovation has facilitated their application in conducting in situ observations within gas and liquid environments, particularly in the investigation of catalytic and battery reactions. We summarize recent noteworthy studies conducted using in situ liquid TEM. These studies highlight significant advancements and provide valuable insights into the utilization of MEMS chips in environmental-cells, as well as the expanding capabilities of in situ liquid TEM in various research domains.

在原位透射电镜观察中,不同的试样支架的不同功能起着至关重要的作用。我们在此全面概述了主要类型的持有人,相关技术,以及与广泛使用的加热和气体加热方法有关的案例研究,从它们的最初发展到最新进展。除了传统的方法外,我们还讨论了采用微机电系统(MEMS)芯片进行现场观测的支架的出现。MEMS技术在单个芯片内提供多种功能,从而增强了支架的功能和多功能性。MEMS芯片已被应用于环境电池设计中,实现了不同形状的定制制造。这一创新促进了它们在气体和液体环境中进行现场观察的应用,特别是在催化和电池反应的研究中。我们总结了最近使用原位液体透射电镜进行的一些值得注意的研究。这些研究突出了重大进展,并为MEMS芯片在环境细胞中的应用提供了有价值的见解,以及原位液体TEM在各个研究领域的扩展能力。
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引用次数: 0
In-situ shearing process observation system for soft materials via transmission electron microscopy. 通过透射电子显微镜观察软材料原位剪切过程的系统。
Pub Date : 2024-04-08 DOI: 10.1093/jmicro/dfad045
Tomohiro Miyata, Hsiao-Fang Wang, Daisuke Watanabe, Yoshiaki Kawagoe, Tomonaga Okabe, Hiroshi Jinnai

We developed an in-situ shear test system suitable for transmission electron microscopy (TEM) observations, which enabled us to examine the shear deformation behaviours inside soft materials at nanoscale resolutions. This study was conducted on a nanoparticle-filled rubber to investigate its nanoscale deformation behaviour under a large shear strain. First, the shear deformation process of a large area in the specimen was accurately examined and proven to exhibit an almost perfect simple shear. At the nanoscale, voids grew along the maximum principal strain during shear deformation. In addition, the nanoscale regions with rubber and silica aggregates exhibited deformation behaviours similar to the global shear deformation of the specimen. Although the silica aggregates exhibited displacement along the shearing directions, rotational motions were also observed owing to the torque generated by the local shear stress. This in-situ shear deformation system for TEM enabled us to understand the nanoscale origins of the mechanical properties of soft materials, particularly polymer composites. Graphical Abstract.

我们开发了一种适合透射电子显微镜(TEM)观察的原位剪切测试系统,使我们能够以纳米级分辨率研究软材料内部的剪切变形行为。本研究以纳米粒子填充橡胶为对象,研究其在大剪切应变下的纳米级变形行为。首先,对试样中大面积的剪切变形过程进行了精确检测,证明其表现出几乎完美的简单剪切。在纳米尺度上,剪切变形过程中的空隙沿着最大主应变生长。此外,带有橡胶和二氧化硅聚集体的纳米级区域表现出与试样整体剪切变形类似的变形行为。虽然二氧化硅聚集体沿剪切方向表现出位移,但由于局部剪切应力产生的扭矩,也观察到了旋转运动。这种用于 TEM 的原位剪切变形系统使我们能够了解软材料(尤其是聚合物复合材料)机械性能的纳米尺度起源。图表摘要。
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引用次数: 0
In situ microscopy techniques for understanding Li plating and stripping in solid-state batteries. 了解固态电池中锂电镀和剥离的原位显微镜技术。
Pub Date : 2024-04-08 DOI: 10.1093/jmicro/dfad058
Munekazu Motoyama

Solid-state batteries have potential to realize a rechargeable Li-metal anode. However, several challenges persist in the charging and discharging processes of the Li-metal anode, which require a fundamental understanding of Li plating and stripping across the interface of solid-state electrolytes (SEs) to address. This review overviews studies on Li-metal anodes in solid-state batteries using in situ observation techniques with an emphasis on Li electrodeposition and dissolution using scanning electron microscopy and SEs such as lithium phosphorus oxynitride and garnet-type compounds such as Li7La3Zr2O12. The previous research is categorized into three topics: (i) Li nucleation, growth and dissolution at the anode-free interface, (ii) electrochemical reduction of SE and (iii) short-circuit phenomena in SE. The current trends of each topic are summarized.

固态电池具有实现可充电锂金属阳极的潜力。然而,在锂金属阳极的充放电过程中仍然存在一些挑战,这需要对锂的电镀和剥离在固态电解质界面上的基本理解来解决。本文综述了利用原位观察技术对固态电池中锂金属阳极的研究,重点介绍了利用扫描电子显微镜(SEM)和固体电解质(SEs)如氮化磷锂(LiPON)和石榴石型化合物如Li7La3Zr2O12 (LLZ)对锂金属阳极的电沉积和溶解。目前的研究主要集中在三个方面:(1)无阳极界面上Li的成核、生长和溶解;(2)SE的电化学还原;(3)SE中的短路现象。总结了当前各课题的发展趋势。
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引用次数: 0
Bioimaging of glucose analogs labeled at the C-1 or C-2 position with a fluorescent dansylamino group. 在 C-1 或 C-2 位置用荧光丹酰氨基标记的葡萄糖类似物的生物成像。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad036
Mio Yanagida, Hirofumi Nakano, Hironori Ueno

Glucose is the most important energy source in all organisms; however, our understanding of the pathways and mechanisms underlying glucose transportation and localization in living cells is incomplete. Here, we prepared two glucose analogs labeled with a dansylamino group at the C-1 (1-Dansyl) or C-2 (2-Dansyl) position; the dansyl group is a highly fluorescent moiety that is characterized by a large Stokes shift between its excitation and emission wavelengths. We then examined the cytotoxicity of the two glucose analogs in mammalian fibroblast cells and in the ciliated protozoan Tetrahymena thermophila. In both cell types, 2-Dansyl had no negative effects on cell growth. The specificity of cellular uptake of glucose analogs was confirmed using an inhibitor of glucose transporter in NIH3T3 cells. In NIH3T3 cells and T. thermophila, fluorescence microscopy revealed that the glucose analogs localized throughout the cytoplasm, but especially at the periphery of the nucleus. In T. thermophila, we also found that swimming speed was comparable in media containing non-labeled glucose or one of the glucose analogs, which provided more evidence not only that the analogs were not cytotoxic in these cells but also that the analogs had no negative effect on the ciliary motion. Together, the present results suggest that the glucose analogs have low toxicity and will be useful for bioimaging of glucose-related systems.

葡萄糖是所有生物体内最重要的能量来源;然而,我们对葡萄糖在活细胞内运输和定位的途径和机制的了解并不全面。在这里,我们制备了两种在 C-1 (1-丹酰)或 C-2 (2-丹酰)位置标记了丹酰氨基的葡萄糖类似物;丹酰基是一种高荧光分子,其特点是激发波长和发射波长之间存在较大的斯托克斯偏移。我们随后研究了这两种葡萄糖类似物在哺乳动物成纤维细胞和纤毛原生动物嗜热四膜虫中的细胞毒性。在这两种细胞中,2-丹酰对细胞生长都没有负面影响。在 NIH3T3 细胞中使用葡萄糖转运体抑制剂证实了细胞摄取葡萄糖类似物的特异性。在 NIH3T3 细胞和嗜热菌中,荧光显微镜显示葡萄糖类似物定位于整个细胞质,尤其是细胞核外围。我们还发现,在含有非标记葡萄糖或其中一种葡萄糖类似物的培养基中,嗜热菌的游动速度相当,这不仅进一步证明了类似物在这些细胞中没有细胞毒性,还证明了类似物对纤毛运动没有负面影响。这些结果表明,葡萄糖类似物的毒性很低,可用于葡萄糖相关系统的生物成像。
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引用次数: 0
Structural and electronic characterization of fluorine-doped La0.5Sr0.5CoO3-δ using electron energy-loss spectroscopy. 利用电子能损耗谱分析掺氟 La0.5Sr0.5CoO3-δ 的结构和电子特性。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad031
Ryotaro Aso, Takuya Katsumata, Takashi Nakamura, Yusuke Watase, Koji Amezawa, Yasukazu Murakami

Perovskite oxides, ABO3, are potential catalysts for the oxygen evolution reaction, which is important in the production of hydrogen as a sustainable energy resource. Optimizing the chemical composition of such oxides by substitution or doping with additional elements is an effective approach to improving the activity of such catalysts. Here, we characterized the crystal and electronic structures of fluorine-doped La0.5Sr0.5CoO3-δ particles using scanning transmission electron microscopy (STEM) and electron energy-loss spectroscopy (EELS). High-resolution STEM imaging demonstrated the formation of a disordered surface phase caused by fluorine doping. In addition, spatially resolved EELS data showed that fluorine anions were introduced into the interiors of the particles and that Co ions near the surfaces were slightly reduced by fluorine doping in conjunction with the loss of oxygen ions. Peak fitting of energy-loss near-edge structure data demonstrated an unexpected nanostructure in the vicinity of the surface. An EELS characterization comprising elemental mapping together with an energy-loss near-edge structure analysis indicated that this nanostructure could not be assigned to Co-based materials but rather to the solid electrolyte BaF2. Complementary structural and electronic characterizations using STEM and EELS as demonstrated herein evidently have the potential to play an increasingly important role in elucidating the nanostructures of functional materials.

包晶氧化物 ABO3 是氧进化反应的潜在催化剂,而氧进化反应对作为可持续能源的氢气生产非常重要。通过替代或掺杂额外元素来优化此类氧化物的化学成分,是提高此类催化剂活性的有效方法。在此,我们利用扫描透射电子显微镜(STEM)和电子能量损失光谱(EELS)对掺氟 La0.5Sr0.5CoO3-δ 颗粒的晶体和电子结构进行了表征。高分辨率 STEM 成像显示,氟掺杂导致无序表面相的形成。此外,空间分辨 EELS 数据显示,氟阴离子被引入颗粒内部,表面附近的钴离子因掺氟而略有减少,同时氧离子也有所损失。能量损失近缘结构数据的峰值拟合显示,表面附近出现了意想不到的纳米结构。由元素图谱和能损近边结构分析组成的电子能谱表征表明,这种纳米结构不能归属于钴基材料,而是归属于固体电解质 BaF2。本文所展示的 STEM 和 EELS 互补结构和电子特性分析,显然有可能在阐明功能材料的纳米结构方面发挥越来越重要的作用。
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引用次数: 0
Transmission electron microscopy study on the phase transformation of metastable precipitates to stable phases. 透射电子显微镜研究析出物向稳定相的相变。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad043
T T T Trang, Yoon-Uk Heo

Nanosized precipitates play a critical role in increasing the strength of metallic alloys. There are many reports that the initial precipitates are metastable phases holding a different composition and crystal structure from the equilibrium precipitate. The metastable precipitate transforms to its stable phase during heat treatment. A transmission electron microscope enables researchers to study the phase transition of metastable precipitates to stable phases due to its fine resolution in identifying crystal structures and chemical compositions. This review introduces the various phase transformation mechanisms of metastable precipitates to stable phases obtained from the analysis using a transmission electron microscope. The role of dislocation movement in the phase transition is further discussed.

纳米沉淀物在提高金属合金强度方面发挥着关键作用。有许多报告指出,初始沉淀物是与平衡沉淀物具有不同成分和晶体结构的析出相。在热处理过程中,析出物会转变为稳定相。透射电子显微镜在确定晶体结构和化学成分方面具有高分辨率,因此研究人员可以利用透射电子显微镜研究析出物向稳定相的相变。本综述介绍了利用透射电子显微镜分析获得的可转移析出物向稳定相转变的各种相变机制。还进一步讨论了位错运动在相变中的作用。
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引用次数: 0
Nondestructive initial-profile-free 3D elemental mapping in multilayer thin film structures based on EDX and a quadratic programming problem. 基于 EDX 和二次编程问题的多层薄膜结构无损初始剖面三维元素图谱。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad041
Yutaka Hoshina, Yugo Kubo, Yojiro Nakayama

We have demonstrated a new data analysis method that enables nondestructive depth profiling of a multilayer thin-film sample from energy-dispersive X-ray spectroscopy (EDX) data without the assumption of initial profiles. This method is based on a quadratic programming problem and allows for three-dimensional elemental mapping in the sample without destroying it, by performing depth profiling for all the pixels in the EDX two-dimensional mapping data. In this paper, first nondestructive depth profiling of two samples with different multilayer structures was performed using the proposed method. The results were compared with those obtained by cross-sectional observation to validate the accuracy and usefulness of the proposed method. Next, an example of the three-dimensional elemental mapping based on the proposed method was demonstrated. This method allows us to nondestructively obtain three-dimensional elemental distribution within a sample over a wide area on the order of mm, which is impossible to obtain using other analytical methods. The way to determine the hyperparameters, which significantly affects the calculation results, is fully described in this paper.

我们展示了一种新的数据分析方法,该方法可根据能量色散 X 射线光谱(EDX)数据对多层薄膜样品进行无损深度剖面分析,而无需假设初始剖面。该方法以二次编程问题为基础,通过对 EDX 二维绘图数据中的所有像素进行深度剖析,可在不破坏样品的情况下绘制样品的三维元素图谱。本文首次使用所提出的方法对两个具有不同多层结构的样品进行了无损深度剖析。结果与横截面观察结果进行了比较,从而验证了所提方法的准确性和实用性。接下来,演示了基于所提方法的三维元素图谱。通过这种方法,我们可以无损地获得样品内部在毫米量级的大范围内的三维元素分布,而这是其他分析方法无法获得的。超参数对计算结果有重大影响,本文全面介绍了确定超参数的方法。
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引用次数: 0
Spatial frequency-based correction of the spherical aberration in living brain imaging. 基于空间频率的活体脑成像球差校正。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad035
Aoi Gohma, Naoya Adachi, Yasuo Yonemaru, Daiki Horiba, Kaori Higuchi, Daisuke Nishiwaki, Eiji Yokoi, Yoshihiro Ue, Atsushi Miyawaki, Hiromu Monai

Optical errors, including spherical aberrations, hinder high-resolution imaging of biological samples due to biochemical components and physical properties. We developed the Deep-C microscope system to achieve aberration-free images, employing a motorized correction collar and contrast-based calculations. However, current contrast-maximization techniques, such as the Brenner gradient method, inadequately assess specific frequency bands. The Peak-C method addresses this issue, but its arbitrary neighbor selection and susceptibility to the noise limit its effectiveness. In this paper, we emphasize the importance of a broad spatial frequency range for accurate spherical aberration correction and propose Peak-F. This spatial frequency-based system utilizes a fast Fourier transform as a bandpass filter. This approach overcomes Peak-C's limitations and comprehensively covers the low-frequency domain of image spatial frequencies.

由于生物化学成分和物理特性的影响,包括球差在内的光学误差阻碍了生物样本的高分辨率成像。我们开发了 Deep-C 显微镜系统,利用电动校正环和基于对比度的计算来实现无像差成像。然而,目前的对比度最大化技术,如布伦纳梯度法,对特定频段的评估不足。Peak-C 方法解决了这一问题,但其任意选择邻域和易受噪声影响的特性限制了其有效性。在本文中,我们强调了宽广的空间频率范围对准确校正球差的重要性,并提出了 Peak-F。这种基于空间频率的系统利用快速傅立叶变换作为带通滤波器。这种方法克服了 Peak-C 的局限性,全面覆盖了图像空间频率的低频域。
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引用次数: 0
Measuring mechanical properties with high-speed atomic force microscopy. 用高速原子力显微镜测量机械性能。
Pub Date : 2024-02-07 DOI: 10.1093/jmicro/dfad051
Christian Ganser, Takayuki Uchihashi

High-speed atomic force microscopy (HS-AFM) is now a widely used technique to study the dynamics of single biomolecules and complex structures. In the past, it has mainly been used to capture surface topography as structural analysis, leading to important discoveries not attainable by other methods. Similar to conventional AFM, the scope of HS-AFM was recently expanded to encompass quantities beyond topography, such as the measurement of mechanical properties. This review delves into various methodologies for assessing mechanical properties, ranging from semi-quantitative approaches to precise force measurements and their corresponding sample responses. We will focus on the application to single proteins such as bridging integrator-1, ion channels such as Piezo1, complex structures such as microtubules and supramolecular fibers. In all these examples, the unique combination of quantifiable force application and high spatiotemporal resolution allows to unravel mechanisms that cannot be investigated by conventional means.

高速原子力显微镜是研究单个生物分子和复杂结构动力学的一种广泛应用的技术。过去,它主要用于捕捉表面地形作为结构分析,导致了其他方法无法实现的重要发现。与传统的原子力显微镜类似,高速原子力显微镜的范围最近扩大到包括形貌之外的量,例如机械性能的测量。这篇综述深入探讨了评估机械性能的各种方法,从半定量方法到精确的力测量及其相应的样品响应。我们将专注于应用于单一蛋白质,如BIN1,离子通道,如Piezo1,复杂结构,如微管和超分子纤维。在所有这些例子中,可量化的力施加和高时空分辨率的独特组合允许揭示传统方法无法研究的机制。
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引用次数: 0
期刊
Microscopy (Oxford, England)
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