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Parameter dependence of depth and lateral resolution of transmission Kikuchi diffraction 透射菊池衍射的深度和横向分辨率与参数有关。
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-10-18 DOI: 10.1016/j.ultramic.2024.114062
Glenn C. Sneddon , Patrick W. Trimby , Levi Tegg , Julie M. Cairney
The spatial resolution of transmission Kikuchi diffraction (TKD) depends on experimental parameters such as atomic number, accelerating voltage, sample backtilt and thickness. In this work, the dependence of spatial resolution on these parameters is explored by using bilayered coarse-grained/nanocrystalline samples to determine the depth resolution. Digital image correlation of the Kikuchi patterns across grain boundaries is used to measure the lateral resolution. The depth resolutions of TKD in aluminium, copper and platinum at 30 kV for an untilted sample were 80, 32 and 14 nm respectively. These worsened with increasing sample backtilt and slightly improved with decreasing accelerating voltage. The best physical lateral resolution obtained was 6 nm, at 30 keV in a 41 nm thick aluminium sample with no backtilt. The lateral resolution worsened with increasing sample thickness and backtilt, contrasting with some previous reports. Accelerating voltage and atomic number did not have a significant impact on the measured lateral resolution within the scatter in the data.
透射菊池衍射(TKD)的空间分辨率取决于原子序数、加速电压、样品后倾和厚度等实验参数。在这项工作中,通过使用双层粗粒/纳米晶样品来确定深度分辨率,从而探索空间分辨率对这些参数的依赖性。跨晶界菊池图案的数字图像相关性用于测量横向分辨率。在 30 千伏电压下,铝、铜和铂的 TKD 深度分辨率分别为 80、32 和 14 纳米。这些分辨率随着样品后倾的增加而降低,随着加速电压的降低而略有提高。在 30 千伏电压下,41 纳米厚的铝样品在没有后倾的情况下获得的最佳物理横向分辨率为 6 纳米。横向分辨率随着样品厚度和后倾角的增加而降低,这与之前的一些报道形成了鲜明对比。加速电压和原子序数对数据散射范围内测得的横向分辨率没有显著影响。
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引用次数: 0
The reference window for reduced perturbation of the reference wave in electrical biasing off-axis electron holography 减少电偏压离轴电子全息技术中参考波扰动的参考窗口
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-10-11 DOI: 10.1016/j.ultramic.2024.114060
Tolga Wagner , Robin Kraft , Franz Nowak , Dirk Berger , Christian M. Günther , Hüseyin Çelik , Christoph T. Koch , Michael Lehmann
The perturbation of the reference wave due to electric stray fields represents a major challenge in quantitative electron holographic investigations. By introducing a focused-ion-beam-milled rectangular hole, the reference window, in an area of nearly constant electrostatic potential of the sample, this perturbation can be significantly reduced. The edge of the window forms a closed conducting loop, acting similarly to a Faraday cage, shielding the influence of the stray field on the reference wave to some extent. In this work, the shielding effect of the reference window is systematically investigated by comparing electron holograms of an electrically biased coplanar capacitor, as a well-known reference sample, with finite element simulations. It is shown that the introduction of the reference window into electrical biasing samples both suppresses unknown lateral phase distortions substantially and in addition improves the agreement of the experimentally observed phase slope with that expected by simulation significantly, particularly for small object-reference wave distances. Consequently, a slight adjustment of the sample geometry results in an improved reproducibility of electron holographic electrical biasing experiments, which is a significant step towards quantitative evaluation.
电杂散场对参考波的扰动是定量电子全息研究的一大挑战。通过在样品静电电位几乎恒定的区域引入一个聚焦离子束铣制的矩形孔(即参考窗口),可以显著降低这种扰动。窗口的边缘形成一个封闭的导电环,其作用类似于法拉第笼,可在一定程度上屏蔽杂散场对参考波的影响。在这项工作中,通过比较电偏压共面电容器(众所周知的参考样品)的电子全息图和有限元模拟,系统地研究了参考窗口的屏蔽效应。结果表明,在电偏压样品中引入参考窗不仅能大大抑制未知的横向相位失真,还能显著改善实验观测到的相位斜率与模拟预期相位斜率的一致性,尤其是在物体与参考波距离较小的情况下。因此,只要对样品的几何形状稍作调整,就能提高电子全息电偏压实验的可重复性,这是向定量评估迈出的重要一步。
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引用次数: 0
Principle of TEM alignment using convolutional neural networks: Case study on condenser aperture alignment 利用卷积神经网络对准 TEM 的原理:聚光器孔径对准案例研究
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-10-09 DOI: 10.1016/j.ultramic.2024.114047
Loïc Grossetête , Cécile Marcelot , Christophe Gatel , Sylvain Pauchet , Martin Hytch
The possibility of automatically aligning the transmission electron microscope (TEM) is explored using an approach based on artificial intelligence (AI). After presenting the general concept, we test the method on the first step of the alignment process which involves centering the condenser aperture. We propose using a convolutional neural network (CNN) that learns to predict the x and y-shifts needed to realign the aperture in one step. The learning data sets were acquired automatically on the microscope by using a simplified digital twin. Different models were tested and analysed to choose the optimal design. We have developed a human-level estimator and intend to use it safely on all apertures. A similar process could be used for most steps of the alignment process with minimal changes, allowing microscopists to reduce the time and training required to perform this task. The method is also compatible with continuous correction of alignment drift during lengthy experiments or to ensure uniformity of illumination conditions during data acquisition.
我们采用一种基于人工智能(AI)的方法,探讨了自动对准透射电子显微镜(TEM)的可能性。在介绍了总体概念之后,我们在对准过程的第一步对该方法进行了测试,这一步涉及将聚光器光圈对准中心。我们建议使用卷积神经网络 (CNN),通过学习来预测在一个步骤中重新对准光圈所需的 x 和 y 移位。学习数据集是在显微镜上使用简化的数字孪生系统自动获取的。我们对不同的模型进行了测试和分析,以选择最佳设计。我们已经开发出一种人类水平的估算器,并打算将其安全地用于所有光圈。类似的过程可用于校准过程中的大多数步骤,只需做出最小的改动,从而使显微镜操作员能够减少执行这项任务所需的时间和培训。该方法还可用于在长时间实验过程中持续校正对准漂移,或在数据采集过程中确保照明条件的一致性。
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引用次数: 0
Exploring deep learning models for 4D-STEM-DPC data processing 探索用于 4D-STEM-DPC 数据处理的深度学习模型。
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-10-05 DOI: 10.1016/j.ultramic.2024.114058
Gregory Nordahl, Sivert Dagenborg, Jørgen Sørhaug, Magnus Nord
For the study of magnetic materials at the nanoscale, differential phase contrast (DPC) imaging is a potent tool. With the advancements in direct detector technology, and consequent popularity gain for four-dimensional scanning transmission electron microscopy (4D-STEM), there has been an ongoing development of new and enhanced ways for STEM-DPC big data processing. Conventional algorithms are experimentally tailored, and so in this article we explore how supervised learning with convolutional neural networks (CNN) can be utilized for automated and consistent processing of STEM-DPC data. Two different approaches are investigated, one with direct tracking of the beam with regression analysis, and one where a modified U-net is used for direct beam segmentation as a pre-processing step. The CNNs are trained on experimentally obtained 4D-STEM data, enabling them to effectively handle data collected under similar instrument acquisition parameters. The model outputs are compared to conventional algorithms, particularly in how they process data in the presence of strong diffraction contrast, and how they affect domain wall profiles and width measurement.
在纳米尺度的磁性材料研究中,差分相衬(DPC)成像是一种有效的工具。随着直接探测器技术的进步和四维扫描透射电子显微镜(4D-STEM)的普及,STEM-DPC 大数据处理的新方法和增强方法也在不断发展。传统算法都是根据实验量身定制的,因此在本文中,我们将探讨如何利用卷积神经网络(CNN)进行监督学习,以实现 STEM-DPC 数据的自动化和一致性处理。我们研究了两种不同的方法,一种是通过回归分析直接跟踪光束,另一种是在预处理步骤中使用改进的 U 网直接分割光束。CNN 在实验获得的 4D-STEM 数据上进行了训练,使其能够有效处理在类似仪器采集参数下收集的数据。模型输出结果与传统算法进行了比较,特别是在出现强烈衍射对比的情况下如何处理数据,以及如何影响畴壁轮廓和宽度测量。
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引用次数: 0
Application of a novel local and automatic PCA algorithm for diffraction pattern denoising in TEM-ASTAR analysis in microelectronics 在微电子学 TEM-ASTAR 分析中应用新型局部自动 PCA 算法进行衍射图样去噪。
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-10-01 DOI: 10.1016/j.ultramic.2024.114059
Tony Printemps, Karen Dabertrand, Jérémy Vives, Alexia Valery
This paper introduces a novel denoising method for TEM-ASTAR™ Diffraction Pattern (DP) datasets, termed LAT–PCA (Local Automatic Thresholding – Principal Component Analysis). This approach enhances the established PCA algorithm by partitioning the 4D dataset (a 2D map of 2D DPs) into localized windows. Within these windows, PCA identifies a basis where the physical signal predominantly resides in the higher-order principal components. By thresholding lower-order components, the method effectively reduces noise while retaining the essential features of the DPs. The locality of the approach, focusing on small windows, enhances computational efficiency and aligns with the localized nature of the crystallographic grain signals in ASTAR. The automatic aspect of the method employs a theoretical pure noise distribution, i.e. a Marchenko-Pastur Distribution, to set a threshold, beyond which the components are mostly noise.
The LAT–PCA method offers significant reductions in acquisition and post-processing times. With denoised data, selecting the correct parameters for accurate phase maps and grain orientations becomes more straightforward, facilitating robust quantitative grain analysis. Experiments performed on a silicon-germanium-carbon sample validate the method's efficacy. The sample was analyzed with varying acquisition times to produce a high signal-to-noise ratio reference dataset and a lower ratio test dataset. The LAT–PCA algorithm's denoising results on the test dataset were benchmarked against the reference, demonstrating considerable improvements and reliability.
In summary, LAT–PCA is an effective, automatic solution for denoising TEM DP datasets. Its adaptability to different noise levels and local processing capability makes it a valuable tool for enhancing dataset quality and reducing the time required for data acquisition and analysis. This method can minimize acquisition time, conserve microscope usage, and reduce sample drift and deterioration, leading to more accurate characterizations with fewer deformation artifacts.
本文介绍了一种用于 TEM-ASTAR™ 衍射图样 (DP) 数据集的新型去噪方法,称为 LAT-PCA(局部自动阈值-主成分分析)。这种方法将 4D 数据集(2D DP 的 2D 地图)划分为局部窗口,从而增强了既定的 PCA 算法。在这些窗口内,PCA 会确定物理信号主要存在于高阶主成分中的基础。通过阈值化低阶成分,该方法在保留 DPs 基本特征的同时有效地减少了噪音。该方法的局部性侧重于小窗口,提高了计算效率,并与 ASTAR 中晶体学晶粒信号的局部性相一致。该方法的自动方面采用了理论上的纯噪声分布(即马琴科-帕斯图尔分布)来设定一个阈值,超过该阈值的成分大多是噪声。LAT-PCA 方法大大减少了采集和后处理时间。有了去噪数据,为精确的相图和晶粒取向选择正确的参数就变得更加简单,从而促进了稳健的定量晶粒分析。在硅锗碳样品上进行的实验验证了该方法的有效性。样品在不同的采集时间下进行分析,以产生高信噪比参考数据集和低信噪比测试数据集。LAT-PCA 算法在测试数据集上的去噪结果与参考数据集进行了比对,结果表明,LAT-PCA 算法有显著的改进,而且非常可靠。总之,LAT-PCA 是对 TEM DP 数据集进行去噪的有效自动解决方案。它对不同噪声水平的适应性和局部处理能力使其成为提高数据集质量、减少数据采集和分析所需时间的重要工具。这种方法可以最大限度地缩短采集时间,节省显微镜的使用时间,减少样品漂移和劣化,从而以更少的形变伪影实现更准确的表征。
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引用次数: 0
A simple and intuitive model for long-range 3D potential distributions of in-operando TEM-samples: Comparison with electron holographic tomography 操作中 TEM 样品长程三维电势分布的简单直观模型:与电子全息断层扫描的比较。
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-09-28 DOI: 10.1016/j.ultramic.2024.114057
Hüseyin Çelik , Robert Fuchs , Simon Gaebel , Christian M. Günther , Michael Lehmann , Tolga Wagner
Electron holography is a powerful tool to investigate the properties of micro- and nanostructured electronic devices. A meaningful interpretation of the holographic data, however, requires an understanding of the 3D potential distribution inside and outside the sample. Standard approaches to resolve these potential distributions involve projective tilt series and their tomographic reconstruction, in addition to extensive simulations. Here, a simple and intuitive model for the approximation of such long-range potential distributions surrounding a nanostructured coplanar capacitor is presented. The model uses only independent convolutions of an initial potential distribution with a Gaussian kernel, allowing the reconstruction of the entire potential distribution from only one measured projection. By this, a significant reduction of the required computational power as well as a drastically simplified measurement process is achieved, paving the way towards quantitative electron holographic investigation of electrically biased nanostructures.
电子全息技术是研究微型和纳米结构电子器件特性的有力工具。然而,要对全息数据进行有意义的解读,需要了解样品内外的三维电势分布。解析这些电势分布的标准方法包括投影倾斜序列及其层析重建,以及大量的模拟。本文介绍了一个简单直观的模型,用于逼近纳米结构共面电容器周围的长程电势分布。该模型仅使用初始电势分布与高斯核的独立卷积,从而只需一个测量投影就能重建整个电势分布。这样,所需的计算能力大大降低,测量过程也大大简化,为电偏压纳米结构的定量电子全息研究铺平了道路。
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引用次数: 0
EBSD and TKD analyses using inverted contrast Kikuchi diffraction patterns and alternative measurement geometries 使用倒置对比菊地衍射图样和替代测量几何图形进行 EBSD 和 TKD 分析
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-09-21 DOI: 10.1016/j.ultramic.2024.114055
Grzegorz Cios , Aimo Winkelmann , Gert Nolze , Tomasz Tokarski , Benedykt R. Jany , Piotr Bała
Electron backscatter diffraction (EBSD) patterns can exhibit Kikuchi bands with inverted contrast due to anomalous absorption. This can be observed, for example, on samples with nanoscale topography, in case of a low tilt backscattering geometry, or for transmission Kikuchi diffraction (TKD) on thicker samples. Three examples are discussed where contrast-inverted physics-based simulated master patterns have been applied to find the correct crystal orientation. As first EBSD example, self-assembled gold nanostructures made of Au fcc and Au hcp phases on single-crystal germanium were investigated. Gold covered about 12% of the mapped area, with only two thirds being successfully interpreted using standard Hough-based indexing. The remaining third was solved by brute force indexing using a contrast-inverted master pattern. The second EBSD example deals with maps collected at a non-tilted surface instead of the commonly used 70° tilted one. As TKD example, a jet-polished foil made of duplex stainless steel 2205 was examined. The thin part close to the hole edge producing normal-contrast patterns were standard indexed. The areas of the foil that become thicker with increasing distance from the edge of the hole produce contrast-inverted patterns. They covered three times the evaluable area and were successfully processed using the contrast-inverted master pattern. In the last example, inverted patterns collected at a non-tiled sample were mathematically inverted to normal contrast, and Hough/Radon-based indexing was successfully applied.
电子反向散射衍射 (EBSD) 图样会因反常吸收而出现反向对比的菊池带。例如,在具有低倾斜反向散射几何形状的纳米级形貌样品上,或者在较厚样品上的透射菊池衍射(TKD)中,都可以观察到这种情况。本文讨论了三个应用对比反转物理模拟母图来找到正确晶体取向的例子。作为第一个 EBSD 例子,研究了单晶锗上由 Au fcc 和 Au hcp 相组成的自组装金纳米结构。金覆盖了大约 12% 的映射区域,只有三分之二的区域可以使用标准的基于 Hough 的索引法成功解释。剩下的三分之一则通过使用对比度反转的主图案进行强制索引来解决。第二个 EBSD 例子涉及在非倾斜表面而不是常用的 70° 倾斜表面采集的地图。以 TKD 为例,研究了由双相不锈钢 2205 制成的喷射抛光箔。对靠近孔边缘的薄部分进行了标准分度,以产生正常对比图案。随着与孔边缘距离的增加,箔片变厚的部分会产生对比度反转的图案。它们覆盖了三倍的可评估区域,并成功地使用对比度反转的母图案进行了处理。在最后一个例子中,在非平铺样品上采集的反差图案通过数学方法反转为正常反差,并成功应用了基于 Hough/Radon 的索引。
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引用次数: 0
Ultra-low-noise transimpedance amplifier with a single HEMT in pre-amplifier for measuring shot noise in cryogenic STM 超低噪声互阻抗放大器,前置放大器采用单 HEMT,用于测量低温 STM 中的射出噪声
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-09-19 DOI: 10.1016/j.ultramic.2024.114051
Ying-Xin Liang
In this work, a design of transimpedance amplifier (TIA) for cryogenic scanning tunneling microscope (CryoSTM) is proposed. TIA with the tip-sample component in CryoSTM is called as CryoSTM-TIA. With transimpedance gain of 1 GΩ, the bandwidth of the CryoSTM-TIA is larger than 200 kHz. The distinctive feature of the proposed CryoSTM-TIA is that its pre-amplifier is made of a single cryogenic high electron mobility transistor (HEMT), so the apparatus equivalent input noise current power spectral density at 100 kHz is lower than 6 (fA)2/Hz. In addition, “bias-cooling method” can be used to in-situ control the density of the frozen DX centers in the HEMT doping area, changing its structure to reduce the device noises. With this apparatus, fast scanning tunneling spectra measurements with high-energy-resolution are capable to be performed. And, it is capable to measure scanning tunneling shot noise spectra (STSNS) at the atomic scale for various quantum systems, even if the shot noise is very low. It provides a powerful tool to investigate novel quantum states by measuring STSNS, such as detecting the existence of Majorana bound states in the topological quantum systems.
本研究提出了一种用于低温扫描隧道显微镜(CryoSTM)的跨阻抗放大器(TIA)设计方案。在 CryoSTM 中带有尖端-样品组件的 TIA 称为 CryoSTM-TIA。在跨导增益为 1 GΩ 时,CryoSTM-TIA 的带宽大于 200 kHz。所提出的 CryoSTM-TIA 的显著特点是其前置放大器由单个低温高电子迁移率晶体管(HEMT)制成,因此 100 kHz 时的仪器等效输入噪声电流功率谱密度低于 6 (fA)2/Hz。此外,"偏置冷却法 "可用于原位控制 HEMT 掺杂区中冷冻 DX 中心的密度,改变其结构以降低器件噪声。利用这种仪器,可以进行高能量分辨率的快速扫描隧道光谱测量。此外,它还能在原子尺度上测量各种量子系统的扫描隧道射电噪声谱(STSNS),即使射电噪声非常低。它为通过测量 STSNS 来研究新型量子态提供了强有力的工具,例如探测拓扑量子系统中是否存在马约拉纳束缚态。
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引用次数: 0
On the temporal transfer function in STEM imaging from finite detector response time 从有限探测器响应时间看 STEM 成像中的时间传递函数
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-09-19 DOI: 10.1016/j.ultramic.2024.114056
Jonathan J.P. Peters , Tiarnan Mullarkey , Julie Marie Bekkevold , Matthew Geever , Ryo Ishikawa , Naoya Shibata , Lewys Jones
Faster scanning in scanning transmission electron microscopy has long been desired for the ability to better control dose, minimise effects of environmental distortions, and to capture the dynamics of in-situ experiments. Advances in scan controllers and scan deflection systems have enabled scanning with pixel dwell times on the order of tens of nanoseconds. At these speeds, the finite response time of the electron detector must be considered as the signal from one electron detection event can contribute to multiple pixels, blurring the features within the image. Here we introduce a temporal transfer function (TTF) to describe and model the effects of detector response time on imaging, as well as a framework for incorporating these effects into simulation.
人们一直希望在扫描透射电子显微镜中实现更快的扫描,以便更好地控制剂量,将环境失真的影响降至最低,并捕捉原位实验的动态变化。扫描控制器和扫描偏转系统的进步使扫描像素停留时间达到几十纳秒。在这种速度下,必须考虑电子探测器的有限响应时间,因为一个电子探测事件产生的信号可能会影响多个像素,从而模糊图像中的特征。在此,我们介绍一种时间传递函数(TTF),用于描述和模拟探测器响应时间对成像的影响,以及将这些影响纳入模拟的框架。
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引用次数: 0
Characterization of strongly coupled quartz tuning fork sensors for precision force measurement in atomic force microscopy 用于原子力显微镜精确测力的强耦合石英音叉传感器的特性分析
IF 2.1 3区 工程技术 Q2 MICROSCOPY Pub Date : 2024-09-18 DOI: 10.1016/j.ultramic.2024.114052
Cedric Shaskey , Amun Jarzembski , Andrew Jue , Keunhan Park

Miniaturized quartz tuning forks (QTFs) have been adopted as force sensors for non-contact atomic force microscopy (AFM). However, the coupled oscillation behaviors of the QTF prongs are not well understood, preventing quantitative measurement of the nanoscale tip-sample interaction forces. This article presents a lumped model that accurately delineates the coupled mechanical oscillations of QTF prongs, establishing rigorous relationships between experimental observables and tip-sample interaction forces. The first-order resonance spectra of a commercial QTF were fully characterized by correlating its piezoelectric response with the actual mechanical oscillation measured with a Fabry-Pérot interferometer. In order to uniquely determine the modeling parameters (i.e., the effective masses, spring constants, and damping constants), the experimental results were compared with the lumped model predictions while masses were added to one prong. The results reveal that the QTF’s center of mass is highly damped, preventing the observation of a symmetric resonance mode. In addition, the mass loading experiment demonstrates that the mechanical oscillations of the QTF prongs are strongly coupled, accounting for 59% (84%) of the effective stiffness at the in-plane (out-of-plane), antisymmetric resonance mode. We believe that the obtained QTF characterization results will pave the way for quantitative measurements of non-contact interaction forces in QTF-based AFM platforms, significantly improving the precision and reliability of nanoscale force measurements.

微型石英音叉(QTF)已被用作非接触式原子力显微镜(AFM)的力传感器。然而,人们对 QTF 叉的耦合振荡行为还不甚了解,因此无法定量测量纳米尺度的针尖-样品相互作用力。本文提出了一个能准确描述 QTF 棱角耦合机械振荡的块状模型,在实验观测值与尖端-样品相互作用力之间建立了严格的关系。通过将商用 QTF 的压电响应与使用法布里-佩罗干涉仪测量的实际机械振荡相关联,全面描述了商用 QTF 的一阶共振频谱。为了唯一确定建模参数(即有效质量、弹簧常数和阻尼常数),在一个棱柱上添加质量时,将实验结果与块状模型预测结果进行了比较。结果表明,QTF 的质心阻尼很大,因此无法观察到对称共振模式。此外,质量加载实验表明,QTF 两棱柱的机械振荡具有很强的耦合性,在平面内(平面外)的非对称共振模式下,占有效刚度的 59% (84%)。我们相信,所获得的 QTF 表征结果将为定量测量基于 QTF 的原子力显微镜平台的非接触相互作用力铺平道路,从而显著提高纳米级力测量的精度和可靠性。
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引用次数: 0
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Ultramicroscopy
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