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Improving the depth resolution of STEM-ADF sectioning by 3D deconvolution 利用三维反褶积提高STEM-ADF剖面的深度分辨率
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa056
A Ishizuka;K Ishizuka;R Ishikawa;N Shibata;Y Ikuhara;H Hashiguchi;R Sagawa
Although the possibility of locating single atom in three dimensions using the scanning transmission electron microscope (STEM) has been discussed with the advent of aberration correction technology, it is still a big challenge. In this report we have developed deconvolution routines based on maximum entropy method (MEM) and Richardson–Lucy algorithm (RLA), which are applicable to the STEM-annular dark-field (ADF) though-focus images to improve the depth resolution. The new three-dimensional (3D) deconvolution routines require a limited defocus-range of STEM-ADF images that covers a whole sample and some vacuum regions. Since the STEM-ADF probe is infinitely elongated along the optical axis, a 3D convolution is performed with a two-dimensional (2D) convolution over xy-plane using the 2D fast Fourier transform in reciprocal space, and a one-dimensional convolution along the z-direction in real space. Using our new deconvolution routines, we have processed simulated focal series of STEM-ADF images for single Ce dopants embedded in wurtzite-type AlN. Applying the MEM, the Ce peaks are clearly localized along the depth, and the peak width is reduced down to almost one half. We also applied the new deconvolution routines to experimental focal series of STEM-ADF images of a monolayer graphene. The RLA gives smooth and high-P/B ratio scattering distribution, and the graphene layer can be easily detected. Using our deconvolution algorithms, we can determine the depth locations of the heavy dopants and the graphene layer within the precision of 0.1 and 0.2 nm, respectively. Thus, the deconvolution must be extremely useful for the optical sectioning with 3D STEM-ADF images.
尽管随着像差校正技术的出现,人们已经讨论了使用扫描透射电子显微镜(STEM)在三维定位单个原子的可能性,但这仍然是一个巨大的挑战。在本报告中,我们开发了基于最大熵方法(MEM)和Richardson–Lucy算法(RLA)的去卷积例程,这些例程适用于STEM环形暗场(ADF),通过聚焦图像来提高深度分辨率。新的三维(3D)去卷积程序需要覆盖整个样本和一些真空区域的STEM-ADF图像的有限散焦范围。由于STEM-ADF探针沿光轴无限延长,因此使用倒数空间中的2D快速傅立叶变换在xy平面上进行二维(2D)卷积,并在真实空间中沿z方向进行一维卷积,从而执行3D卷积。使用我们新的去卷积程序,我们处理了嵌入纤锌矿型AlN中的单个Ce掺杂剂的STEM-ADF图像的模拟焦点序列。应用MEM,Ce峰沿深度明显局部化,并且峰宽度减小到几乎一半。我们还将新的去卷积例程应用于单层石墨烯的STEM-ADF图像的实验焦点序列。RLA给出了平滑且高P/B比的散射分布,并且可以容易地检测石墨烯层。使用我们的去卷积算法,我们可以分别在0.1和0.2nm的精度内确定重掺杂剂和石墨烯层的深度位置。因此,反褶积对于具有3D STEM-ADF图像的光学切片必须非常有用。
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引用次数: 1
Advances in cryo-EM and ED with a cold-field emission beam and energy filtration —Refinements of the CRYO ARM 300 system in RIKEN SPring-8 center— 冷场发射束和能量过滤低温EM和ED的研究进展——日本理工大学SPring-8中心cryo ARM 300系统的改进--
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa052
Saori Maki-Yonekura;Tasuku Hamaguchi;Hisashi Naitow;Kiyofumi Takaba;Koji Yonekura
We have designed and evaluated a cryo-electron microscopy (cryo-EM) system for higher-resolution single particle analysis and high-precision electron 3D crystallography. The system comprises a JEOL CRYO ARM 300 electron microscope—the first machine of this model—and a direct detection device camera, a scintillator-coupled camera, GPU clusters connected with a camera control computer and software for automated-data collection and efficient and accurate operation. The microscope provides parallel illumination of a highly coherent 300-kV electron beam to a sample from a cold-field emission gun and filters out energy-loss electrons through the sample with an in-column energy filter. The gun and filter are highly effective in improving imaging and diffraction, respectively, and have provided high quality data since July 2018. We here report on the characteristics of the cryo-EM system, updates, our progress and future plan for running such cryo-EM machines in RIKEN SPring-8 Center.
我们设计并评估了一种用于更高分辨率单粒子分析和高精度电子3D结晶学的冷冻电子显微镜(cryo-EM)系统。该系统包括一台JEOL CRYO ARM 300电子显微镜——该型号的第一台机器——以及一台直接检测设备相机、一台闪烁体耦合相机、与相机控制计算机连接的GPU集群和用于自动数据收集和高效准确操作的软件。该显微镜从冷场发射枪向样品提供高度相干的300kV电子束的平行照明,并用柱内能量过滤器过滤掉通过样品的能量损失电子。该枪和滤波器分别在改善成像和衍射方面非常有效,自2018年7月以来提供了高质量的数据。我们在这里报道了冷冻电镜系统的特点、更新、我们的进展以及在理研SPring-8中心运行这种冷冻电镜机器的未来计划。
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引用次数: 14
Recent advances in small-angle electron diffraction and Lorentz microscopy 小角度电子衍射和洛伦兹显微术的最新进展
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa048
Shigeo Mori;Hiroshi Nakajima;Atsuhiro Kotani;Ken Harada
We describe small-angle electron diffraction (SmAED) and Lorentz microscopy using a conventional transmission electron microscope. In SmAED, electron diffraction patterns with a wide-angular range on the order of 1 × 10−2 rad to 1 × 10−7 rad can be obtained. It is demonstrated that magnetic information of nanoscale magnetic microstructures can be obtained by Fresnel imaging, Foucault imaging and SmAED. In particular, we report magnetic microstructures associated with magnetic stripes and magnetic skyrmions revealed by Lorentz microscopy with SmAED. SmAED can be applied to the analysis of microstructures in functional materials such as dielectric, ferromagnetic and multiferroic materials.
我们描述了使用传统透射电子显微镜的小角度电子衍射(SmAED)和洛伦兹显微镜。在SmAED中,具有1量级的宽角度范围的电子衍射图案 × 10−2 rad至1 × 可以获得10−7 rad。结果表明,利用菲涅耳成像、福柯成像和SmAED可以获得纳米磁性微结构的磁信息。特别是,我们报道了通过SmAED的洛伦兹显微镜揭示的与磁条和磁性skyrmions相关的磁性微观结构。SmAED可应用于功能材料(如电介质、铁磁材料和多铁性材料)的微观结构分析。
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引用次数: 2
Transport of intensity equation method and its applications 强度方程输运法及其应用
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa053
Masanori Mitome
A phase retrieval technique based on a transport of intensity equation (TIE) is one of the defocus series reconstruction techniques in microscopy. Since it does not require any dedicated devices like a biprism, and only three defocus images are enough to retrieve phase information, it has been applied to observe magnetic fields, magnetic domains, electrostatic potentials and strains. It is also used to improve image resolution by correcting spherical aberration. This technique is simple and easy to use, but some artifacts often appear in the retrieved phase map. One should pay careful attention to the experimental conditions and the algorithms and boundary conditions used to solve the TIE. This paper reviews the principle of the TIE method, the algorithms used to solve it and application results in materials science.
基于强度输运方程(TIE)的相位恢复技术是显微镜中散焦序列重建技术之一。由于它不需要任何像双棱镜这样的专用设备,并且只有三个散焦图像就足以检索相位信息,因此它已被应用于观察磁场、磁畴、静电势和应变。它还用于通过校正球面像差来提高图像分辨率。这种技术简单易用,但在检索到的相位图中经常会出现一些伪影。应该仔细注意实验条件以及用于求解TIE的算法和边界条件。本文综述了TIE方法的原理、求解算法以及在材料科学中的应用结果。
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引用次数: 8
Practical implementation of high-resolution electron ptychography and comparison with off-axis electron holography 高分辨率电子ptychography的实际实现及其与离轴电子全息术的比较
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa055
Arthur M Blackburn;Robert A McLeod
Ptychography is a coherent diffractive imaging technique that can determine how an electron wave is transmitted through an object by probing it in many small overlapping regions and processing the diffraction data obtained at each point. The resulting electron transmission model describes both phase and amplitude changes to the electron wave. Ptychography has been adopted in transmission electron microscopy in recent years following advances in high-speed direct electron detectors and computer algorithms which now make the technique suitable for practical applications. Its ability to retrieve quantitative phase information at high spatial resolution makes it a plausible alternative or complement to electron holography. Furthermore, unlike off-axis electron holography, it can provide phase information without an electron bi-prism assembly or the requirement of a minimally structured region adjacent to the region of interest in the object. However, it does require a well-calibrated scanning transmission electron microscope and a well-managed workflow to manage the calibration, data acquisition and reconstruction process to yield a practical technique. Here we detail this workflow and highlight how this is greatly assisted by acquisition management software. Through experimental data and modelling we also explore the similarities and differences between high-resolution ptychography and electron holography. Both techniques show a dependence of the recovered phase on the crystalline orientation of the material which is attributable to dynamical scattering. However, the exact nature of the variation differs reflecting fundamental expectations, but nonetheless equally useful information is obtained from electron holography and the ptychographically determined object transmission function.
Ptychography是一种相干衍射成像技术,它可以通过在许多小的重叠区域中探测电子波并处理在每个点获得的衍射数据来确定电子波是如何通过物体传输的。由此产生的电子传输模型描述了电子波的相位和振幅变化。近年来,随着高速直接电子探测器和计算机算法的进步,Ptychography已被用于透射电子显微镜,这使得该技术适合实际应用。它能够以高空间分辨率检索定量相位信息,这使它成为电子全息术的一种可行的替代或补充。此外,与离轴电子全息术不同,它可以在没有电子双棱镜组件或与物体中感兴趣区域相邻的最小结构区域的要求的情况下提供相位信息。然而,它确实需要一台校准良好的扫描透射电子显微镜和一个管理良好的工作流程来管理校准、数据采集和重建过程,以产生一种实用的技术。在这里,我们详细介绍了这一工作流程,并强调了采购管理软件如何在很大程度上帮助实现这一点。通过实验数据和建模,我们还探索了高分辨率ptychography和电子全息术之间的异同。这两种技术都显示出回收相对材料晶体取向的依赖性,这可归因于动态散射。然而,变化的确切性质不同,反映了基本的预期,但从电子全息术和物理摄影确定的物体传输函数中获得了同样有用的信息。
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引用次数: 0
Local structure analysis of amorphous materials by angstrom-beam electron diffraction 用埃束电子衍射分析非晶材料的局域结构
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa075
Akihiko Hirata
The structure analysis of amorphous materials still leaves much room for improvement. Owing to the lack of translational or rotational symmetry of amorphous materials, it is important to develop a different approach from that used for crystals for the structure analysis of amorphous materials. Here, the angstrom-beam electron diffraction method was used to obtain the local structure information of amorphous materials at a sub-nanometre scale. In addition, we discussed the relationship between the global and local diffraction intensities of amorphous structures, and verified the effectiveness of the proposed method through basic diffraction simulations. Finally, some applications of the proposed method to structural and functional amorphous materials are summarized.
非晶态材料的结构分析仍有很大的改进空间。由于非晶材料缺乏平移或旋转对称性,开发一种不同于晶体的方法来分析非晶材料的结构是很重要的。这里,使用埃束电子衍射方法来获得亚纳米尺度上非晶材料的局部结构信息。此外,我们还讨论了非晶结构的全局衍射强度和局部衍射强度之间的关系,并通过基本的衍射模拟验证了所提出方法的有效性。最后,总结了该方法在结构和功能非晶材料中的一些应用。
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引用次数: 9
Novel −75°C SEM cooling stage: application for martensitic transformation in steel 新型−75°C SEM冷却阶段:在钢中马氏体相变中的应用
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa051
Kaneaki Tsuzazki;Motomichi Koyama;Ryosuke Sasaki;Keiichiro Nakafuji;Kazushi Oie;Akinobu Shibata;Takashi Gondo;Hiroya Miyazaki;Hiroshi Akamine;Minoru Nishida
Microstructural changes during the martensitic transformation from face-centred cubic (FCC) to body-centred cubic (BCC) in an Fe-31Ni alloy were observed by scanning electron microscopy (SEM) with a newly developed Peltier stage available at temperatures to  −75°C. Electron channelling contrast imaging (ECCI) was utilized for the in situ observation during cooling. Electron backscatter diffraction analysis at ambient temperature (20°C) after the transformation was performed for the crystallographic characterization. A uniform dislocation slip in the FCC matrix associated with the transformation was detected at −57°C. Gradual growth of a BCC martensite was recognized upon cooling from −57°C to −63°C.
通过扫描电子显微镜(SEM)观察了Fe-31Ni合金从面心立方(FCC)到体心立方(BCC)马氏体转变过程中的微观结构变化,新开发的Peltier阶段在 −75°C。利用电子通道对比成像(ECCI)在冷却过程中进行原位观察。在转变后的环境温度(20°C)下进行电子背散射衍射分析以进行晶体表征。在FCC基体中检测到与转变相关的均匀位错滑移 −57°C。BCC马氏体在从 −57°C至 −63°C。
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引用次数: 1
Magnetic flux density measurements from narrow grain boundaries produced in sintered permanent magnets 烧结永磁体中产生的窄晶界磁通密度测量
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa032
Youngji Cho;Sujin Lee;Yasukazu Murakami
This review examines methods of magnetic flux density measurements from the narrow grain boundary (GB) regions, the thickness of which is of the order of nanometers, produced in Nd–Fe–B-based sintered magnets. Despite of the complex crystallographic microstructure and the significant stray magnetic field of the sintered magnet, recent progress in electron holography allowed for the determination of the intrinsic magnetic flux density due to the GB which is embedded in the polycrystalline thin-foil. The methods appear to be useful as well for intensive studies about interface magnetism in a variety of systems.
这篇综述研究了在Nd–Fe–B基烧结磁体中产生的厚度为纳米量级的窄晶界(GB)区域的磁通密度测量方法。尽管烧结磁体具有复杂的晶体微观结构和显著的杂散磁场,但由于嵌入多晶薄箔中的GB,电子全息术的最新进展允许测定本征磁通密度。这些方法似乎对深入研究各种系统中的界面磁性也很有用。
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引用次数: 1
Visualization of microstructural change affected by mechanical stimulation in tendon healing with a novel tensionless model 用一种新的无张力模型可视化肌腱愈合过程中受机械刺激影响的微观结构变化
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa043
Junya Oshima;Kaoru Sasaki;Naoto Yamamoto;Tomoharu Kiyosawa;Mitsuru Sekido
Since the majority of a tendon’s dry weight is collagen fibers, tendon healing consists mainly of collagen repair and observing three-dimensional networks of collagen fibers with scanning electron microscopy (SEM) is optimal for investigating this process. In this report, a cell-maceration/SEM method was used to investigate extrasynovial tendon (unwrapped tendon in synovial tissue such as the tendon sheath) healing of an injured Achilles tendon in a rat model. In addition, since mechanical stimulation is important for tendon healing, a novel, tensionless, rat lower leg tendon injury model was established and verified by visualizing the structural change of collagen fibers under tensionless conditions by SEM. This new model was created by transplanting the leg of a rat with a tendon laceration to the back, removing mechanical stimulation. We then compared the process of tendon healing with and without tension using SEM. Under tension, collagen at the tendon stump shows axial alignment and repair that subsequently demarcates the paratenon (connective tissue on the surface of an extrasynovial tendon) border. In contrast, under tensionless conditions, the collagen remains randomly arranged. Our findings demonstrate that mechanical stimulation contributes to axial arrangement and reinforces the importance of tendon tension in wound healing.
由于肌腱干重的大部分是胶原纤维,肌腱愈合主要由胶原修复组成,用扫描电子显微镜(SEM)观察胶原纤维的三维网络是研究这一过程的最佳方法。在本报告中,使用细胞浸渍/SEM方法来研究大鼠模型中受伤跟腱的滑膜外肌腱(滑膜组织如腱鞘中未包裹的肌腱)愈合。此外,由于机械刺激对肌腱愈合很重要,因此建立了一种新型的无张力大鼠小腿肌腱损伤模型,并通过扫描电镜观察无张力条件下胶原纤维的结构变化进行了验证。该模型是通过将肌腱撕裂伤大鼠的腿移植到背部,去除机械刺激而建立的。然后,我们使用SEM比较了有张力和无张力的肌腱愈合过程。在张力下,肌腱残端的胶原蛋白显示出轴向排列和修复,随后划定了副腱(滑膜外肌腱表面的结缔组织)边界。相反,在无张力条件下,胶原保持随机排列。我们的研究结果表明,机械刺激有助于轴向排列,并加强肌腱张力在伤口愈合中的重要性。
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引用次数: 0
Phase plates in the transmission electron microscope: operating principles and applications 透射电子显微镜中的相位板:工作原理和应用
IF 1.8 4区 工程技术 Pub Date : 2020-11-01 DOI: 10.1093/jmicro/dfaa070
Marek Malac;Simon Hettler;Misa Hayashida;Emi Kano;Ray F Egerton;Marco Beleggia
In this paper, we review the current state of phase plate imaging in a transmission electron microscope. We focus especially on the hole-free phase plate design, also referred to as the Volta phase plate. We discuss the implementation, operating principles and applications of phase plate imaging. We provide an imaging theory that accounts for inelastic scattering in both the sample and in the hole-free phase plate.
本文综述了透射电子显微镜相位板成像的现状。我们特别关注无孔相位板的设计,也称为Volta相位板。我们讨论了相位板成像的实现、工作原理和应用。我们提供了一种成像理论,该理论解释了样品和无孔相板中的非弹性散射。
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引用次数: 21
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