Ultramicroscopy最新文献

英文中文

Sensitivity of multislice electron ptychography to point defects: A case study in SiC 多层电子平面摄影对点缺陷的灵敏度：以碳化硅为例

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-24 DOI: 10.1016/j.ultramic.2025.114282

Aaditya Bhat, Colin Gilgenbach, Junghwa Kim, Michael Xu, Menglin Zhu, James M. LeBeau

Here, we evaluate multislice electron ptychography as a tool for depth-resolved atomic-resolution characterization of point defects, using silicon carbide as a case study. Through multislice electron scattering simulations and multislice ptychographic reconstructions, we investigate the phase contrast arising from individual silicon vacancies, antisite defects, and a wide range of substitutional transition metal dopants (V_Si to W_Si), as well as their potential detectability. Simulating defect types, positions, and microscope conditions, we show that isolated point defects can be located within a unit cell along the sample’s depth. The influence of electron energy, dose, defocus, and convergence semi-angle is also explored to determine their role in governing defect contrast. These results guide experiments aimed at analyzing point defects using multislice electron ptychography.

在这里，我们以碳化硅为例，评估了多层电子平面摄影作为深度分辨原子分辨率表征点缺陷的工具。通过多层电子散射模拟和多层平面重建，我们研究了由单个硅空位、反位缺陷和广泛的取代过渡金属掺杂剂（VSi到WSi）引起的相衬，以及它们的潜在可探测性。模拟缺陷类型、位置和显微镜条件，我们显示孤立的点缺陷可以沿着样品的深度定位在一个单元胞内。还探讨了电子能量、剂量、离焦和会聚半角的影响，以确定它们在控制缺陷对比度中的作用。这些结果指导了用多层电子平面摄影技术分析点缺陷的实验。

引用次数: 0

On the Edge: In situ Kelvin probe AFM on InP nanowire arrays 边缘：在InP纳米线阵列上的原位开尔文探针AFM。

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-24 DOI: 10.1016/j.ultramic.2025.114284

Austin Irish , Lukas Hrachowina , David Alcer , Magnus Borgström , Rainer Timm

Surface physics play an outsized role in nanostructured electronic devices such as solar cells. Semiconductor nanowires are perfect candidates for advanced solar cells due to their outstanding light absorption properties and their flexibility in axially stacking materials of different doping and band gap. Due to nanowire geometry, however, their surfaces dominate device performance and at the same time are challenging to investigate. Kelvin probe force microscopy (KPFM), an atomic force microscopy (AFM)-based method, provides a unique structural and electrical characterization even in unconventional 3D geometries. We demonstrate a high-resolution, non-destructive AFM technique for directly measuring nanowires within an array and still on their growth substrate. This in situ approach ensures measurement integrity and relevance while preserving the structures for subsequent measurement and processing. When compared with electron beam-induced current, cross-sectional KPFM is both more surface sensitive and less destructive. Utilizing such a cross-sectional approach facilitates rapid and comprehensive characterization of nanoelectronic surfaces.

表面物理在太阳能电池等纳米结构电子器件中发挥着巨大的作用。半导体纳米线具有优异的光吸收性能和在不同掺杂和带隙的轴向堆叠材料中的灵活性，是先进太阳能电池的理想候选者。然而，由于纳米线的几何形状，它们的表面决定了器件的性能，同时也具有挑战性。开尔文探针力显微镜（KPFM）是一种基于原子力显微镜（AFM）的方法，即使在非常规的3D几何形状中也能提供独特的结构和电学表征。我们展示了一种高分辨率，非破坏性的原子力显微镜技术，用于直接测量阵列内的纳米线，并且仍然在其生长衬底上。这种原位方法确保了测量的完整性和相关性，同时保留了后续测量和处理的结构。与电子束感应电流相比，截面KPFM具有更高的表面敏感性和更小的破坏性。利用这种横截面方法有助于纳米电子表面的快速和全面表征。

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引用次数: 0

Neural field enhanced phase retrieval of atomic-scale structural dynamics in radiation sensitive materials 辐射敏感材料原子尺度结构动力学的神经场增强相位反演

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-24 DOI: 10.1016/j.ultramic.2025.114283

Yang Liu , Hongsheng Shi , Siyuan Shen , Yuan Lu , Shuchen Zhang , Jingyi Yu , Yi Yu

Atomic-scale imaging of radiation-sensitive materials has been a challenge for both materials science and life science. While low-dose transmission electron microscopy (TEM) is particularly useful for minimizing the radiation damage, the noisy images with poor resolution make it extremely difficult for the purpose of fine structure analysis. Here, this work presents a phase retrieval method to achieve high-quality atomic-scale imaging of radiation-sensitive materials under low-dose TEM conditions. By integrating neural fields (NF) with traditional exit wave reconstruction (EWR), it is able to reveal atomic details from limited low-dose experimental data. Taking the radiation-sensitive organic–inorganic hybrid halide perovskite CH

_{3}

_{3}

PbI

_{3}

(MAPbI

_{3}

) as an example, the EWR-NF method demonstrates superior performance in reconstructing the pristine atomic structure using as few as just three low-dose images, which is beyond the limits of conventional methods. In this manner, EWR-NF enables higher temporal resolution to reveal intermediate states during irradiation-induced decomposition. An example of stacking of MAPbI

_{3}

with its as-decomposed product is shown. EWR-NF offers a promising tool for atomic-level structure analysis of sensitive halide perovskites and understanding irradiation-induced structure changes, with implications for a wide range of applications in materials science and beyond.

辐射敏感材料的原子尺度成像一直是材料科学和生命科学面临的挑战。虽然低剂量透射电子显微镜（TEM）在最大限度地减少辐射损伤方面特别有用，但低分辨率的噪声图像使精细结构分析变得极其困难。本文提出了一种在低剂量透射电镜条件下实现高质量辐射敏感材料原子尺度成像的相位检索方法。通过将神经场（NF）与传统的出口波重建（EWR）相结合，可以从有限的低剂量实验数据中揭示原子细节。以辐射敏感型有机-无机杂化卤化物钙钛矿CH3NH3PbI3 （MAPbI3）为例，EWR-NF方法在只需三张低剂量图像即可重建原始原子结构方面表现出优越的性能，这超出了传统方法的限制。通过这种方式，EWR-NF能够提供更高的时间分辨率来揭示辐射诱导分解期间的中间状态。给出了MAPbI3与其分解产物的叠加示例。EWR-NF为敏感卤化物钙钛矿的原子水平结构分析和理解辐照引起的结构变化提供了一个有前途的工具，在材料科学和其他领域具有广泛的应用前景。

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引用次数: 0

Secondary electron topographical contrast formation in scanning transmission electron microscopy 扫描透射电子显微镜中二次电子地形对比的形成

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-11 DOI: 10.1016/j.ultramic.2025.114278

Evgenii Vlasov, Wouter Heyvaert, Tom Stoops, Sandra Van Aert, Johan Verbeeck, Sara Bals

Secondary electron (SE) imaging offers a powerful complementary capabilities to conventional scanning transmission electron microscopy (STEM) by providing surface-sensitive, pseudo-3D topographic information. However, contrast interpretation of such images remains empirical due to complex interactions of emitted SE with the magnetic field in the objective field of TEM. Here, we propose an analytical physical model that takes into account the physics of SE emission and interaction of the emitted SEs with magnetic field. This enables more reliable image interpretation and potentially lay the foundation for novel 3D surface reconstruction algorithms.

二次电子（SE）成像通过提供表面敏感的伪三维地形信息，为传统的扫描透射电子显微镜（STEM）提供了强大的补充能力。然而，由于在TEM的目标场中发射的SE与磁场的复杂相互作用，这种图像的对比解释仍然是经验的。在这里，我们提出了一个考虑SE发射物理和发射的SE与磁场相互作用的解析物理模型。这可以实现更可靠的图像解释，并可能为新的3D表面重建算法奠定基础。

引用次数: 0

Reflected and transmitted secondary electron images of thin Si3N4 window Si3N4薄窗的反射和透射二次电子图像。

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-09 DOI: 10.1016/j.ultramic.2025.114277

Yanli Li , Yichen Ping , Yue Wu , Yao Liu , Huibin Zhao , Li Han

Reflected and transmitted secondary electron images of Si₃N₄ window are obtained in scanning electron microscopy (SEM) by using SEM and scanning transmission electron microscopy (STEM) holders. The figure of Si₃N₄ window becomes distinguishable as the accelerating voltage increases. However, the brightness of Si₃N₄ window relative to the surroundings in images for SEM and STEM holders is completely opposite. It changes from dark to bright, which means the number of detected secondary electron increases. The difference of the two kinds of image is caused by the fact that secondary electrons emitted from the bottom surface can also be detected when using STEM holder. The images are consistent with Monte Carlo simulation results. Image figures are sensitive to accelerating voltages and sample thicknesses. Therefore, more characteristics of thin sample could be analyzed via combining the two kinds of image.

利用扫描电子显微镜（SEM）和扫描透射电子显微镜（STEM）支架在扫描电子显微镜（SEM）下获得了Si3N4窗口的反射和透射二次电子图像。随着加速电压的增加，氮化硅窗口的图形变得清晰。然而，SEM和STEM持有者的图像中Si3N4窗口相对于周围环境的亮度完全相反。它由暗变亮，这意味着检测到的二次电子数量增加。两种图像的差异是由于使用STEM支架时也可以检测到从底面发射的二次电子。所得图像与蒙特卡罗模拟结果吻合较好。图像数据对加速电压和样品厚度敏感。因此，通过两种图像的结合，可以分析薄样品的更多特征。

引用次数: 0

Evaluation of electron threshold energy for predicting radiation damage in transmission electron microscopy 透射电镜中预测辐射损伤的电子阈值能的评价。

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-09 DOI: 10.1016/j.ultramic.2025.114279

Yupeng Yin , Ruiqi Zhan , Yufeng Du , Chi Xu , Somei Ohnuki , Farong Wan , Wentuo Han

The electron threshold energy (E_t) of a material is a critical parameter for anyone conducting research using transmission electron microscopy (TEM). For studies involving irradiation damage, the electron beam energy must exceed the material’s E_t to enable in-situ electron irradiation experiments. In contrast, for researchers focused on microstructural characterization, it is essential to ensure that the beam energy remains below E_t to avoid electron-beam-induced radiation damage, which could compromise the accuracy and reliability of the TEM analysis. This study revisits the commonly used formula for calculating E_t, originally cited in the textbook by Williams and Carter, and identifies significant discrepancies when compared with experimental observations and the original formulation. A corrected formula is proposed and applied to compute E_t values for 81 elements using their minimum displacement energies (E_{d min}). The results are presented in a periodic-table-based diagram, providing practical reference for selecting appropriate TEM accelerating voltages to either induce or avoid irradiation damage.

材料的电子阈值能（Et）对于任何使用透射电子显微镜（TEM）进行研究的人来说都是一个关键参数。对于涉及辐照损伤的研究，电子束能量必须超过材料的Et才能进行原位电子辐照实验。相比之下，对于专注于微观结构表征的研究人员来说，确保光束能量保持在Et以下是必不可少的，以避免电子束引起的辐射损伤，这可能会影响TEM分析的准确性和可靠性。本研究重新审视了Williams和Carter在教科书中最初引用的计算Et的常用公式，并与实验观察和原始公式进行了比较，发现了显著的差异。提出了一个修正公式，并应用于用最小位移能（edmin）计算81个元素的Et值。结果以周期表的形式给出，为选择合适的瞬变电磁法加速电压以诱导或避免辐照损伤提供了实用参考。

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引用次数: 0

Development of precession Lorentz transmission electron microscopy 进动洛伦兹透射电镜的发展

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-08 DOI: 10.1016/j.ultramic.2025.114276

Shunsuke Hayashi , Dongxue Han , Hidenori Tsuji , Kyoko Ishizaka , Asuka Nakamura

Lorentz transmission electron microscopy (LTEM) is a powerful tool for high-resolution imaging of magnetic textures, including their dynamics under external stimuli and ultrafast nonequilibrium conditions. However, magnetic imaging is often hindered by non-magnetic diffraction contrast arising from inhomogeneous sample deformation or a non-parallel electron beam. In this study, we develop a precession LTEM system that can suppress diffraction contrast by changing the incident angle of the electron beam relative to the sample in a precessional manner. By comparing LTEM images acquired at different precession angles (

θ

), we show that diffraction contrast is significantly reduced with increasing

θ

. However, large

θ

values lead to an undesired broadening of the magnetic contrast, highlighting the importance of optimizing

θ

. Furthermore, defocus-dependent measurements reveal that magnetic contrast is particularly improved at small defocus values. These findings demonstrate the potential of precession LTEM as a powerful technique for studying magnetic dynamics.

洛伦兹透射电子显微镜（LTEM）是研究磁性织构在外部刺激和超快非平衡条件下动力学的高分辨率成像工具。然而，由于非均匀样品变形或非平行电子束引起的非磁性衍射对比，往往阻碍了磁成像。在本研究中，我们开发了一种进动LTEM系统，该系统可以通过以进动方式改变电子束相对于样品的入射角来抑制衍射对比。通过比较在不同进动角（θ）下获得的tem图像，我们发现随着θ的增大，衍射对比度明显降低。然而，较大的θ值会导致磁对比度的不希望的扩大，突出了优化θ的重要性。此外，离焦相关的测量表明，在小离焦值下，磁对比度得到了特别的提高。这些发现证明了进动LTEM作为研究磁动力学的一种强有力的技术的潜力。

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引用次数: 0

Femtosecond-laser-assisted focused ion beam method for the fabrication of tip specimens for atom probe tomography 飞秒激光辅助聚焦离子束制备原子探针层析成像尖端试样的方法

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-06 DOI: 10.1016/j.ultramic.2025.114268

Yu-Chen Yang , Tung-Huan Chou , Ya-Lan Hsu , Kun-Lin Lin , Zhiqiang Wang , Kuen-Hsing Lin

This study developed a simple femtosecond (fs)-laser-assisted focused ion beam (FIB) method for rapidly fabricating tip samples for atom probe tomography (APT). In this method, a microtip array is fabricated directly on a Si sample to avoid the use of conventional lift-out procedures. The proposed method comprises two steps: fs-laser ablation and Ga FIB annular milling. Fs-laser ablation results in the formation of a damaged amorphous layer; however, this layer is small, does not affect the results of APT, and can be removed through subsequent Ga FIB annular milling. APT analysis of a tip sample fabricated using the proposed approach confirmed the feasibility of the method. This method not only enhanced the stability of the tip sample but also had a considerably shorter sample preparation time compared with conventional Ga FIB and Xe FIB fabrication processes.

本研究开发了一种简单的飞秒激光辅助聚焦离子束（FIB）快速制备原子探针断层扫描（APT）尖端样品的方法。在这种方法中，微针尖阵列是直接在硅样品上制造的，以避免使用传统的提升程序。该方法包括两步：fs激光烧蚀和Ga FIB环空铣削。fs激光烧蚀导致非晶层的破坏；然而，该层很小，不影响APT的结果，可以通过后续的Ga FIB环铣去除。用该方法制备的针尖样品的APT分析证实了该方法的可行性。该方法不仅提高了尖端样品的稳定性，而且与传统的Ga FIB和Xe FIB制备工艺相比，样品制备时间大大缩短。

引用次数: 0

An electrostatic aberration corrector for improved Low-Voltage SEM imaging 一种改进低压扫描电镜成像的静电像差校正器

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-03 DOI: 10.1016/j.ultramic.2025.114267

Diederik Jan Maas

An electrostatic aberration corrector (AC), based on a quadrupole-octupole design, for a low voltage scanning electron microscope (LV-SEM) has been developed, integrated and tested in a modified commercial SEM for improving image quality. After quantitative assessment and adjustment of the chromatic aberration and qualitive adjustment of the spherical aberration, LV-SEM image resolution and contrast improved by almost a factor three. Some unavoidable electromagnetic interference (EMI) accounts for the difference between the experimentally demonstrated AC-SEM edge resolution of 3.0 nm at a beam energy of 1000 eV and the corresponding theoretical probe size of 2.2 nm. After cancelling the chromatic and spherical aberrations of the objective lens of a scanning electron microscope (SEM) the reachable image resolution is limited by spot blur due to EMI, higher order aberrations and, more fundamentally, by the interaction volume of the focused electron beam in a sample and beam-induced alterations to the sample. Furthermore, the practical performance of the purely electrostatic aberration corrector integrated into an AC-SEM is demonstrated on typical material and life science samples at a beam energy of 500 and 1000 eV. Whereas electro-magnetic aberration correctors struggle with re-alignment iterations after a beam energy change due to remanent magnetic fields, a purely electrostatic corrector is swiftly adjusted by proportional scaling of electrode voltages. In principle, an electrostatic corrector can also be applied to low-voltage ion microscopy.

Summarising, an easy-to-use purely electrostatic corrector has been developed which, after proper integration into a state-of-the-art SEM, is capable of delivering the ultimate low-voltage SEM images.

为提高低电压扫描电子显微镜（LV-SEM）成像质量，研制了一种基于四极-八极设计的静电像差校正器（AC），并在改进的商用扫描电子显微镜（LV-SEM）上进行了集成和测试。经过色差的定量评估和调整，球差的定性调整，LV-SEM图像的分辨率和对比度提高了近三倍。一些不可避免的电磁干扰（EMI）造成了实验证明的在1000 eV束流下3.0 nm的AC-SEM边缘分辨率与相应的理论探针尺寸2.2 nm之间的差异。在消除扫描电子显微镜（SEM）物镜的色差和球差后，可达到的图像分辨率受到EMI引起的斑模糊，高阶像差，更根本的是，受到样品中聚焦电子束的相互作用体积和光束引起的样品变化的限制。此外，在典型的材料和生命科学样品上验证了集成在交流扫描电镜中的纯静电像差校正器在500和1000 eV束流能量下的实际性能。而电磁像差校正器在由于剩余磁场导致的光束能量变化后挣扎于重新对准迭代，纯静电校正器通过电极电压的比例缩放迅速调整。原则上，静电校正器也可以应用于低压离子显微镜。总之，已经开发出一种易于使用的纯静电校正器，经过适当集成到最先进的扫描电镜中，能够提供最终的低压扫描电镜图像。

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引用次数: 0

Evaporated amorphous Si protective coatings for dual FIB/SEM preparation of high-quality lamellae for S/TEM analysis 蒸发非晶硅双FIB/SEM保护涂层制备高质量片层进行S/TEM分析

IF 2 3区工程技术 Q2 MICROSCOPY

Ultramicroscopy

Pub Date : 2025-11-03 DOI: 10.1016/j.ultramic.2025.114266

N.G. Rudawski, M.A. Downing

Amorphous Si (a-Si) evaporated using electron beam physical vapor deposition (EBPVD) was investigated as a protective coating for dual focused ion beam/scanning electron microscope (FIB/SEM) preparation of lamellae for scanning/transmission electron microscopy (S/TEM) analysis. EBPVD a-Si films were evaporated on polished, undoped (001) SrTiO₃ substrates and then dual FIB/SEM was used to prepare lamellae for S/TEM analysis. It was revealed that the EBPVD a-Si coating suppressed charging-related instabilities during dual FIB/SEM preparation. Subsequent S/TEM analyses using TEM imaging, high-angle annular dark-field (HAADF) STEM imaging, and selected area electron diffraction revealed the EBPVD a-Si films deposit with a smooth surface, non-porous microstructure, and amorphous crystal structure, which ultimately results in high-quality lamellae with smooth, curtain-free sidewalls. High-resolution TEM and HAADF-STEM imaging also revealed that the EBPVD process did not damage the surface of the (001) SrTiO₃ substrates and that EBPVD a-Si is robust to both O₂-based plasma cleaning and typical high-dose electron irradiation performed during atomic-resolution elemental mapping using energy dispersive spectroscopy. It is thus demonstrated that EBPVD a-Si meets all requirements for an ideal protective coating for dual FIB/SEM preparation of high-quality lamellae for S/TEM analysis and is advantageous over all other coatings previously investigated in this capacity.

研究了电子束物理气相沉积（EBPVD）蒸发非晶硅（a-Si）作为双聚焦离子束/扫描电镜（FIB/SEM）制备片层的保护涂层，用于扫描/透射电镜（S/TEM）分析。将EBPVD a-Si薄膜蒸发在抛光、未掺杂的（001）SrTiO3衬底上，然后用FIB/SEM制备片层进行S/TEM分析。结果表明，在双FIB/SEM制备过程中，EBPVD a-Si涂层抑制了充电相关的不稳定性。随后的S/TEM分析使用TEM成像，高角度环形暗场（HAADF） STEM成像和选定区域电子衍射显示EBPVD a- si薄膜沉积具有光滑的表面，无孔微观结构和非晶态晶体结构，最终产生具有光滑，无幕侧壁的高质量片层。高分辨率TEM和HAADF-STEM成像还显示，EBPVD过程没有破坏（001）SrTiO3衬底的表面，并且EBPVD a-Si对基于o2的等离子体清洗和使用能量色散光谱进行原子分辨率元素映射时进行的典型高剂量电子照射都具有鲁棒性。因此，EBPVD a-Si满足了理想的双重FIB/SEM制备用于S/TEM分析的高质量片层的保护涂层的所有要求，并且优于之前研究过的所有其他涂层。

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