查看更多>>摘要：A novel precision grinding tool has been developed for manual-grinding of samples for analysis in a transmission electron microscope. The tool can be self-made by any scientific laboratory with a 3D printer. Using a simple method, the sample can be precisely aligned with the grinding plane, which enables preparation of samples with highly precise parallel faces. Combined with light weight and low vibration, the device is ideally suited for preparing extremely thin samples even below 10 μm thickness. The paper discusses design principles and materials, and the device is evaluated by preparing samples from magnesium alloy and silicon. Design files are included for 3D printing and CNC milling.
查看更多>>摘要：Over the years, computer scientists are working on building models that aid the scientific community in many ways by cutting laboratory expenses or by saving time. Such models find useful applications in microscopy images as well. Determining the morphology of nanoparticles from Transmission Electron Microscopy images is a manual and cumbersome task. In the past years, scientists have tried to build models to automate the process of nanoparticle segmentation in microscopy images. This study focuses on finding the best segmentation model, which achieves high metrics and is robust to microscopy parameters. For this purpose, eight different models have been compared. The training dataset consists of 150 BF-TEM Platinum nanoparticle images containing 3629 nanoparticles of all kinds. Further, we examine the generalizability of the models on E-TEM Gold nanoparticle images. We also describe essential considerations while choosing a network for segmenting nanoparticle images that generalize well across the Platinum BF-TEM and Gold E-TEM nanoparticles dataset. The layer gradients are visualized to further explain the black-box nature of neural networks.
查看更多>>摘要：Spectroscopy is widely used for the analysis of chemical, vibrational, and bonding information. Interpretations of the spectral features have been performed by comparing the objective spectra with reference spectra from experiments or simulations. However, the interpretation process by humans is not always straightforward, especially for spectra obtained from unknown or new materials. In the present study, we developed a method using machine learning techniques to obtain human-like interpretation automatically. We combined unsupervised and supervised learning methods; then applied it to the spectrum database which includes more than 400 spectra of water and organic molecules containing various ligands and chemical bonds. The proposed method has successfully found the correlations between the spectral features and descriptors of the atoms, bonds, and ligands. We demonstrated that the proposed method enabled the automatic determination of reasonable spectrum–structure relationships such as between π* resonance in C-K edges and multiple bonds. The proposed method enables the automatic determination of physically and chemically reasonable spectrum–structure relationships without arbitrariness in data-driven manner, which is considerably difficult only with simulation or conventional machine leaning techniques. Such relationships are useful for understanding what structural parameters cause changes in the spectrum, providing a way for the better interpretation of spatial distributed or time evolutionary data. Furthermore, although the present work focused on the ELNES/XANES spectrum from small organic molecules, the proposed method can be readily extended to other spectral data. It is expected to contribute to a better understanding of the spectrum–structure relationship in various spectroscopy applications.
查看更多>>摘要：A newly developed microscope prototype, namely npSCOPE, consisting of a Gas Field Ion Source (GFIS) column and a position sensitive Delay-line Detector (DLD) was used to perform Scanning Transmission Ion Microscopy (STIM) using keV He+ ions. One experiment used 25 keV ions and a second experiment used 30 keV ions. STIM imaging of a 50 nm thick free-standing gold membrane exhibited excellent contrast due to ion channelling and revealed rich microstructural features including isolated nanoscale twin bands which matched well with the contrast in the conventional ion-induced Secondary Electron (SE) imaging mode. Transmission Kikuchi Diffraction (TKD) and Backscattered Electron (BSE) imaging were performed on the same areas to correlate and confirm the microstructural features observed in STIM. Monte Carlo simulations of the ion and electron trajectories were performed with parameters similar to the experimental conditions to derive insights related to beam broadening and its effect in the degradation of transmission image resolution. For the experimental conditions used, STIM imaging showed a lateral resolution close to30 nm. Dark twin bands in bright grains as well as bright twin bands in dark grains were observed in STIM. Some of the twin bands were invisible in STIM. For the specific experimental conditions used, the ion transmission efficiency across a particular twin band was found to decrease by a factor of 2.8. Surprisingly, some grains showed contrast reversal when the Field of View (FOV) was changed indicating the sensitivity of the channelling contrast to even small changes in illumination conditions. These observations are discussed using ion channelling conditions and crystallographic orientations of the grains and twin bands. This study demonstrates for the first time the potential of STIM imaging using keV He+ ions to quantitatively investigate channelling in nanoscale structures including isolated crystalline defects.
查看更多>>摘要：Ultimate resolution in scanning transmission electron microscopy (STEM) with state-of-the-art aberration correctors requires careful tuning of the experimental parameters. The optimum aperture semi-angle depends on the chosen high tension, the chromatic aberration and the energy width of the source as well as on potentially limiting intrinsic residual aberrations. In this paper we derive simple expressions and criteria for choosing the aperture semi-angle and for counterbalancing the intrinsic sixth-order three-lobe aberration of two-hexapole aberration correctors by means of the fourth-order three-lobe aberration. It is noteworthy that for such an optimally adjusted electron probe the so-called flat area of the Ronchigram is explicitly not maximized. The above considerations are validated by experiments with a CEOS ASCOR in a C-FEG-equipped JEOL NEOARM operated at 60 kV. Sub-Angstrom resolution is demonstrated for a Si[112] single crystal as well as for a single-layered MoS2 crystalline film. Lattice reflections of 73 pm for silicon and 93 pm for molybdenum disulfide are visible in the Fourier transform of the images, respectively. Moreover, single sulfur vacancies can be clearly identified in the MoS2.
查看更多>>摘要：We have developed a method to obtain a data cube using a semi-parallel detection scheme and an electrostatic hemispherical analyzer (HSA) with multi-channel detection. By improving the Auger intensity map measurement scheme, the number of detector energy sweeps is reduced, and faster measurement is achieved. The gain differences among the detection channel are corrected by post-processing, and a data cube of Auger electron spectra is constructed. A data cube was obtained for an example of a sample with a non-flat surface, lead-free solder. It was demonstrated to be possible to extract spectra from any position within the measurement area and create the elemental distribution maps.
查看更多>>摘要：Sub-sampling during image acquisition in scanning transmission electron microscopy (STEM) has been shown to provide a means to increase the overall speed of acquisition while at the same time providing an efficient means to control the dose, dose rate and dose overlap delivered to the sample. In this paper, we discuss specifically the parameters used to reconstruct sub-sampled images and highlight their effect on inpainting using the beta-process factor analysis (BPFA) methodology. The selection of the main control parameters can have a significant effect on the resolution, precision and sensitivity of the final inpainted images, and here we demonstrate a method by which these parameters can be optimised for any image in STEM. As part of this work, we also provide a link to open source code and a tutorial on its use, whereby these parameters can be tested for any datasets. When coupled with the hardware necessary to rapidly sub-sample images in STEM, this approach can have significant implications for imaging beam sensitive materials and dynamic processes.
查看更多>>摘要：Resolution is a key parameter for microscopy, but methods for standardizing its definition are often poorly defined. For a developing technique such as scanning helium microscopy, it is critical that a consensus-based protocol for determining instrument resolution is prepared as a written standard to allow both comparable quantitative measurements of surface topography and direct comparisons between different instruments. In this paper we assess a range of quantitative methods for determining instrument resolution and determine their relative merits when applied to the specific case of the scanning helium microscope (SHeM). Consequently, we present a preliminary protocol for measuring the resolution in scanning helium microscopy based upon utilizing appropriate test samples with sets of slits of well-defined dimensions to establish the quantitative resolution of any similar instrument.
查看更多>>摘要：Quantitative differential phase contrast imaging of materials in atomic-resolution scanning transmission electron microscopy using segmented detectors is limited by various factors, including coherent and incoherent aberrations, detector positioning and uniformity, and scan-distortion. By comparing experimental case studies of monolayer and few-layer graphene with image simulations, we explore which parameters require the most precise characterisation for reliable and quantitative interpretation of the reconstructed phases. Coherent and incoherent lens aberrations are found to have the most significant impact. For images over a large field of view, the impact of noise and non-periodic boundary conditions are appreciable, but in this case study have less of an impact than artefacts introduced by beam deflections coupling to beam scanning (imperfect tilt-shift purity).
查看更多>>摘要：The xenon plasma focused ion beam and scanning electron microscopy (PFIB-SEM) system is a promising tool for 3D tomography of nano-scale materials, including nanotextured black silicon (BSi), whose topography is difficult to measure with conventional microscopy techniques. Advantages of PFIB-SEM include high material removal rates, precise control of milling parameters and automated slice-and-view procedures. However, there is no universal sample preparation procedure nor is there an established ideal workflow for the PFIB-SEM slice-and-view process. This work demonstrates that specimen preparation, including the orientation of the volume of interest, is critical for the quality of the final reconstructed 3D model. It thoroughly explores three unique configurations incrementally optimized for higher total throughput. All three sampling configurations are applied to a resin-embedded BSi sample to determine the most favourable workflow and highlight each approach's advantages and disadvantages. The reconstructed 3D models of the BSi surface obtained are shown to be qualitatively closer to the topography measured directly by SEM. The height distribution data extracted from the rendered 3D models reveal a higher structure depth compared to that obtained from an atomic force microscopy measurement. Furthermore, the work demonstrates how samples with different rigidity react to long-term ion-beam interaction, as both amorphous (resin) and crystalline (Si) material is present in the tested specimen. This study improves the understanding of sample-beam interaction and broadens the utility of the 3D PFIB-SEM for more complicated sample structures.
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Elsevier