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Register a new userAtomic Imaging Using Secondary Electrons in a Scanning Transmission Electron Microscope : Experimental Observations and Possible Mechanisms
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We report our detailed investigation of high-resolution imaging using secondary electrons (SE) with a subnanometer probe in an aberration-corrected transmission electron microscope, Hitachi HD2700C. This instrument also allows us to acquire the corresponding annular-dark-field (ADF) images simultaneously and separately. We demonstrate that atomic SE imaging is achievable for a wide range of elements, from uranium to carbon. Using the ADF images as a reference, we study the SE image intensity and contrast as a function of applied bias, atomic number, crystal tilt and thickness to shed light on the origin of the unexpected ultrahigh resolution in SE imaging. We have also demonstrated that the SE signal is sensitive to the terminating species at a crystal surface. Possible mechanisms for atomicscale SE imaging are proposed. The ability to image both the surface and bulk of a sample at atomic scale is unprecedented, and could revolutionize the field of electron microscopy and imaging.
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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).
In this study, we have used a Zr-Nb alloy containing well-defined nano-precipitates as a model material in which to study imaging contrast
Ultra-fast transmission electron microscopy (UTEM) combines sub-picosecond time-resolution with the versatility of TEM spectroscopies. It allows one to study the dynamics of materials properties combining complementary techniques. However, until now, time-resolved cathodoluminescence, which is expected to give access to the optical properties dynamics, was still unavailable in a UTEM. In this paper, we report time-resolved cathodoluminescence measurements in an ultrafast transmission electron microscope. We measured lifetime maps, with a 12 nm spatial resolution and sub-nanoseconds resolution, of nano-diamonds with a high density of NV center. This study paves the way to new applications of UTEM and to correlative studies of optically active nanostructures.
When magnetic properties are analysed in a TEM using the technique of electron magnetic circular dichroism (EMCD), one of the critical parameters is the sample orientation, and this, independently on the chosen acquisition geometry. Since small orientation changes can have a strong impact on the EMCD measurement, it is experimentally non trivial to measure the EMCD signal as a function of sample orientation. The classical EMCD experimental setup requires to tilt the crystal in a 2 beam orientation and to acquire two electron energy loss spectra at two conjugate scattering angles. The effect of a mistilt from the perfect 2-beam orientation on the measured EMCD signals has not been explored yet due to different experimental constraints. In order to maintain the exact sample location and orientation for the acquisition of the EMCD signal, we have developed a methodology to simultaneously map the quantitative EMCD signals and the local orientation of the crystal. We analyse, both experimentally and with simulations, how the measured magnetic signals evolve with a change in the crystal tilt from the exact 2-beam orientation. Based on this analysis, we establish an accurate relationship between the crystal orientations and the EMCD signals. Our results demonstrate that a small crystal tilt away from the 2-beam orientation can significantly alter the strength and the distribution of the EMCD signals. From an optimisation of the crystal orientation, we obtain quantitative EMCD measurements.
Machine learning has emerged as a powerful tool for the analysis of mesoscopic and atomically resolved images and spectroscopy in electron and scanning probe microscopy, with the applications ranging from feature extraction to information compression and elucidation of relevant order parameters to inversion of imaging data to reconstruct structural models. However, the fundamental limitation of machine learning methods is their correlative nature, leading to extreme susceptibility to confounding factors. Here, we implement the workflow for causal analysis of structural scanning transmission electron microscopy (STEM) data and explore the interplay between physical and chemical effects in ferroelectric perovskite across the ferroelectric-antiferroelectric phase transitions. The combinatorial library of the Sm-doped BiFeO3 is grown to cover the composition range from pure ferroelectric BFO to orthorhombic 20% Sm-doped BFO. Atomically resolved STEM images are acquired for selected compositions and are used to create a set of local compositional, structural, and polarization field descriptors. The information-geometric causal inference (IGCI) and additive noise model (ANM) analysis are used to establish the pairwise causal directions between the descriptors, ordering the data set in the causal direction. The causal chain for IGCI and ANM across the composition is compared and suggests the presence of common causal mechanisms across the composition series. Ultimately, we believe that the causal analysis of the multimodal data will allow exploring the causal links between multiple competing mechanisms that control the emergence of unique functionalities of morphotropic materials and ferroelectric relaxors.
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