Ultramicroscopy最新文献

Backscattered electron (BSE) imaging based on scanning electron microscopy (SEM) has been widely used in scientific and industrial disciplines. However, achieving consistent standards and precise quantification in BSE images has proven to be a long-standing challenge. Previous methods incorporating dedicated calibration processes and Monte Carlo simulations have still posed practical limitations for widespread adoption. Here we introduce a bolometer platform that directly measures the absorbed thermal energy of the sample and demonstrates that it can help to analyze the atomic number (Z) of the investigated samples. The technique, named Atomic Number Electron Microscopy (ZEM), employs the conservation of energy as the foundation of standardization and can serve as a nearly ideal BSE detector. Our approach combines the strengths of both BSE and ZEM detectors, simplifying quantitative analysis for samples of various shapes and sizes. The complementary relation between the ZEM and BSE signals also makes the detection of light elements or compounds more accessible than existing microanalysis techniques.

We built a custom-made holder with a Hall-effect sensor to measure the single point magnetic flux density inside a transmission electron microscope (TEM, JEM-F200, JEOL). The measurement point is at the same place as the sample inside the TEM. We utilized information collected with the Hall-effect sensor holder to study magnetic domain wall (DW) dynamics by in-situ Lorentz microscopy. We generated an external magnetic field to the sample using the objective lens (OL) of the TEM. Based on our measurements with the Hall-effect sensor holder, the OL has nearly linear response, and when it is switched off, the strength of the magnetic field in the sample region is very close to 0 mT.

A ferritic-pearlitic sample studied has globular and lamellar cementite (Fe₃C) carbides in the ferrite matrix. Based on the in-situ Lorentz microscopy experiments, DWs in the ferritic matrix perpendicular to the lamellar carbides start to move first at ∼10 mT. At 160 mT, DWs inside the globular carbide start to disappear, and the saturation occurs at ∼210 mT. At 288 mT, the DWs parallel to the lamellar carbides still exist. Thus, these lamellar carbides are very strong pinning sites for DWs. We also run dynamical micromagnetic simulations to reproduce the DW disappearance in the globular carbide. As in the in-situ experiments, the DWs stay stable until the external field reaches the magnitude of 160 mT, and the DWs disappear before the field is 214 mT. In general, the micromagnetic simulations supported very well the interpretation of the experimental findings.

Electron beam damage in electron microscopes is becoming more and more problematic in material research with the increasing demand of characterization of new beam sensitive material such as Li based compounds used in lithium-ion batteries. To avoid radiolysis damage, it has become common practice to use Cryo-EM, however, knock-on damage can still occur in conventional TEM/STEM with a high-accelerating voltage (200–300 keV). In this work, electron energy loss spectroscopy with an accelerating voltage of 30,20 and 10 keV was explored with h-BN, TiB₂ and TiN compounds. All Ti L_2,3, N K and B K edges were successfully observed with an accelerating voltage as low as 10 keV. An accurate elemental quantification for all three samples was obtained using a multi-linear least square (MLLS) procedure which gives at most a 5 % of standard deviation which is well within the error of the computation of the inelastic partial-cross section used for the quantification. These results show the great potential of using low-voltage EELS which is another step towards a knock-on damage free analysis.

In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field $B=2$ T, and with the magnetic objective lens switched off (Lorenz mode), i.e. $B=0$ T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF.

Ewald sphere curvature correction, which extends beyond the projection approximation, stretches the shallow depth of field in cryo-EM reconstructions of thick particles. Here we show that even for previously assumed thin particles, reconstruction artifacts which we refer to as ghosts can appear. By retrieving the lost phases of the electron exitwaves and accounting for the first Born approximation scattering within the particle, we show that these ghosts can be effectively eliminated. Our simulations demonstrate how such ghostbusting can improve reconstructions as compared to existing state-of-the-art software. Like ptychographic cryo-EM, our Ghostbuster algorithm uses phase retrieval to improve reconstructions, but unlike the former, we do not need to modify the existing data acquisition pipelines.

Nanostructured materials continue to find applications in various electronic and sensing devices, chromatography, separations, drug delivery, renewable energy, and catalysis. While major advancements on the synthesis and characterization of these materials have already been made, getting information about their structures at sub-nanometer resolution remains challenging. It is also unfortunate to find that many emerging or already available powerful analytical methods take time to be fully adopted for characterization of various nanomaterials. The scanning low energy electron microscopy (SLEEM) is a good example to this. In this report, we show how clearer structural and surface information at nanoscale can be obtained by SLEEM, coupled with deep learning. The method is demonstrated using Au nanoparticles-loaded mesoporous silica as a model system. Moreover, unlike conventional scanning electron microscopy (SEM), SLEEM does not require the samples to be coated with conductive films for analysis; thus, not only it is convenient to use but it also does not give artifacts. The results further reveal that SLEEM and deep learning can serve as great tools to analyze materials at nanoscale well. The biggest advantage of the presented method is its availability, as most modern SEMs are able to operate at low energies and deep learning methods are already being widely used in many fields.

In this study, we report a strain visualization method using large-angle convergent-beam electron diffraction (LACBED).¹ We compare the proposed method with the strain maps acquired via STEM-NBD, a combination of scanning transmission electron microscopy (STEM) and nanobeam electron diffraction (NBD). Although STEM-NBD can precisely measure the lattice parameters, it requires a large amount of data and personal computer (PC) resources to obtain a two-dimensional strain map. Deficiency lines in the transmitted disk of LACBED reflect the crystalline structure information and move, curve, or disappear in the deformed area. Properly setting the optical conditions makes it possible to acquire real-space images over a broad area in conjunction with deficiency lines on the transmitted disk. The proposed method acquires images by changing the relative position between the specimen and the deficiency line and can grasp the strain information with a small number of images. In addition, the proposed method does not require high-resolution images. It can reduce the required PC memory or storage consumption in comparison with that of STEM-NBD, which requires a high-resolution diffraction pattern (DP) from each point of the region of interest. Compared with the two-dimensional maps of LACBED and NBD, NBD could detect large distortions in the area where the deficiency line curved, moved, or disappeared. The curving or moving direction of the deficiency line is qualitatively consistent with the NBD results. If quantitative strain values are not essential, strain visualization using LACBED can be considered an effective technique. We believe that the strain information of a sample can be obtained effectively using both methods.

Atomic-scale electron microscopy traditionally probes thin specimens, with thickness below 100 nm, and its feasibility for bulk samples has not been documented. In this study, we explore the practicality of scanning transmission electron microscope (STEM) imaging with secondary electrons (SE), using a silicon-wedge specimen having a maximum thickness of 18 μm. We find that the atomic structure is present in the entire thickness range of the SE images although the background intensity increases moderately with thickness. The consistent intensity of secondary electron (SE) images at atomic positions and the modest increase in background intensity observed in silicon suggest a limited contribution from SEs generated by backscattered electrons, a conclusion supported by our multislice calculations. We conclude that achieving atomic resolution in SE imaging for bulk specimens is indeed attainable using aberration-corrected STEM and an aberration-corrected scanning electron microscope (SEM) may have the capacity for atomic-level resolution, holding great promise for future strides in materials research.

We present the design, fabrication and discuss the performance of a new combined high-resolution Scanning Tunneling and Thermopower Microscope (STM/SThEM). We also describe the development of the electronic control, the user interface, the vacuum system, and arrangements to reduce acoustical noise and vibrations. We demonstrate the microscope’s performance with atomic-resolution topographic images of highly oriented pyrolytic graphite (HOPG) and local thermopower measurements in the semimetal ${\mathrm{Bi}}_2{\mathrm{Te}}_3$. Our system offers a tool to investigate the relationship between electronic structure and thermoelectric properties at the nanoscale.

Compressive sensing (CS) can reconstruct the rest information almost without distortion by advanced computational algorithm, which significantly simplifies the process of atomic force microscope (AFM) scanning with high imaging quality. In common CS-AFM, the partial measurements randomly come from the whole region to be measured, which easily leads to detail loss and poor image quality in regions of interest (ROIs). Consequently, important microscopic phenomena are missed probably. In this paper, we developed an adaptive under-sampling strategy for CS-AFM to optimize the process of sampling. Under a certain under-sampling ratio, the weight coefficient of ROIs and regions of base (ROBs) were set to control the distribution of under-sampling points and corresponding measurement matrix. A series of simulations were completed to demonstrate the relationship between the weight coefficient of ROIs and image quality. After that, we verified the effectiveness of the method on our homemade AFM. Through a lot of simulations and experiments, we demonstrated how the proposed method optimized the sampling process of CS-AFM, which speeded up the process of AFM imaging with high quality.