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Metal oxide nanoparticles exhibit outstanding catalytic properties, believed to be related to the presence of oxygen vacancies at the particle's surface. However, little quantitative information is known about concentrations of point defects inside and at surfaces of these nanoparticles, due to the challenges in achieving an atomically resolved experimental access. By employing off-axis electron holography, we demonstrate, using MgO nanoparticles as an example, a methodology that discriminates between mobile charge induced by electron beam irradiation and immobile charge associated with deep traps induced by point defects as well as distinguishes between bulk and surface point defects. Counting the immobile charge provides a quantification of the concentration of F 2+ centers induced by oxygen vacancies at the MgO nanocube surfaces.

Off-axis electron holography is a powerful technique that involves the formation of an interference pattern in a transmission electron microscope (TEM) by overlapping two parts of an electron wave, one of which has passed through a region of interest on a specimen and the other is a reference wave. The resulting off-axis electron hologram can be analyzed digitally to recover the phase difference between the two parts of the electron wave, which can then be interpreted to provide quantitative information about local variations in electrostatic potential and magnetic induction within and around the specimen. Off-axis electron holograms can be recorded while a specimen is subjected to external stimuli such as elevated or reduced temperature, voltage, or light. The protocol that is presented here describes the practical steps that are required to record, analyze, and interpret off-axis electron holograms, with a primary focus on the measurement of magnetic fields within and around nanoscale materials and devices. Presented here are the steps involved in the recording, analysis, and processing of off-axis electron holograms, as well as the reconstruction and interpretation of phase images and visualization of the results. Also discussed are the need for optimization of the specimen geometry, the electron optical configuration of the microscope, and the electron hologram acquisition parameters, as well as the need for the use of information from multiple holograms to extract the desired magnetic contributions from the recorded signal. The steps are illustrated through a study of specimens of B20-type FeGe, which contain magnetic skyrmions and were prepared with focused ion beams (FIBs). Prospects for the future development of the technique are discussed.

The mapping of electrostatic potentials and magnetic fields in liquids using electron holography has been considered to be unrealistic. Here, we show that hydrated cells of Magnetospirillum magneticum strain AMB-1 and assemblies of magnetic nanoparticles can be studied using off-axis electron holography in a fluid cell specimen holder within the transmission electron microscope. Considering that the holographic object and reference wave both pass through liquid, the recorded electron holograms show sufficient interference fringe contrast to permit reconstruction of the phase shift of the electron wave and mapping of the magnetic induction from bacterial magnetite nanocrystals. We assess the challenges of performing in situ magnetization reversal experiments using a fluid cell specimen holder, discuss approaches for improving spatial resolution and specimen stability, and outline future perspectives for studying scientific phenomena, ranging from interparticle interactions in liquids and electrical double layers at solid-liquid interfaces to biomineralization and the mapping of electrostatic potentials associated with protein aggregation and folding., (© 2017 The Author(s).)

A selection of recent results illustrating the application of off-axis electron holography to the study of magnetic microstructure in closely-spaced nanoparticles and nanowires is reviewed. Examples are taken from the characterization of FeNi nanoparticle chains, Co nanoparticle rings, two-dimensional arrays of naturally occurring magnetite crystals in minerals, and single crystalline Co nanowires. Approaches that can be used to separate the magnetic signal of interest from the mean inner potential contribution to the measured holographic phase shift are described, and the spatial and phase resolution that can be achieved are discussed., (2004 Wiley-Liss, Inc.)

Beam shaping—the ability to engineer the phase and the amplitude of massive and massless particles—has long interested scientists working on communication, imaging, and the foundations of quantum mechanics. In light optics, the shaping of electromagnetic waves (photons) can be achieved using techniques that include, but are not limited to, direct manipulation of the beam source (as in x-ray free electron lasers and synchrotrons), deformable mirrors, spatial light modulators, mode converters, and holograms. The recent introduction of holographic masks for electrons provides new possibilities for electron beam shaping. Their fabrication has been made possible by advances in micrometric and nanometric device production using lithography and focused on ion beam patterning. This article provides a tutorial on the generation, production, and analysis of synthetic holograms for transmission electron microscopy. It begins with an introduction to synthetic holograms, outlining why they are useful for beam shaping to study material properties. It then focuses on the fabrication of the required devices from theoretical and experimental perspectives, with examples taken from both simulations and experimental results. Applications of synthetic electron holograms as aberration correctors, electron vortex generators, and spatial mode sorters are then presented. [ABSTRACT FROM AUTHOR]

Inline holography in the transmission electron microscope is a versatile technique which provides real-space phase information that can be used for the correction of imaging aberrations, as well as for measuring electric and magnetic fields and strain distributions. It is able to recover high-spatial-frequency contributions of the phase effectively but suffers from the weak transfer of low-spatial-frequency information, as well as from incoherent scattering. Here, we combine gradient flipping and phase prediction in an iterative flux-preserving focal series reconstruction algorithm with incoherent background subtraction that gives extensive access to the missing low spatial frequencies. A procedure for optimizing the reconstruction parameters is presented, and results from Fe-filled C nanospheres, and MgO cubes are compared with phase images obtained using off-axis holography. [ABSTRACT FROM AUTHOR]

Imaging of biomolecules by ionizing radiation, such as electrons, causes radiation damage which introduces structural and compositional changes of the specimen. The total number of high‐energy electrons per surface area that can be used for imaging in cryogenic electron microscopy (cryo‐EM) is severely restricted due to radiation damage, resulting in low signal‐to‐noise ratios (SNR). High resolution details are dampened by the transfer function of the microscope and detector, and are the first to be lost as radiation damage alters the individual molecules which are presumed to be identical during averaging. As a consequence, radiation damage puts a limit on the particle size and sample heterogeneity with which electron microscopy (EM) can deal. Since a transmission EM (TEM) image is formed from the scattering process of the electron by the specimen interaction potential, radiation damage is inevitable. However, we can aim to maximize the information transfer for a given dose and increase the SNR by finding alternatives to the conventional phase‐contrast cryo‐EM techniques. Here some alternative transmission electron microscopy techniques are reviewed, including phase plate, multi‐pass transmission electron microscopy, off‐axis holography, ptychography and a quantum sorter. Their prospects for providing more or complementary structural information within the limited lifetime of the sample are discussed. [ABSTRACT FROM AUTHOR]

The rapid development of electron tomography, in particular the introduction of novel tomographic imaging modes, has led to the visualization and analysis of three-dimensional structural and chemical information from materials at the nanometre level. In addition, the phase information revealed in electron holograms allows electrostatic and magnetic potentials to be mapped quantitatively with high spatial resolution and, when combined with tomography, in three dimensions. Here we present an overview of the techniques of electron tomography and electron holography and demonstrate their capabilities with the aid of case studies that span materials science and the interface between the physical sciences and the life sciences. [ABSTRACT FROM AUTHOR]

Low temperature (200–600 °C) annealing in the transmission electron microscope (TEM) is used to provide a significant noise reduction in phase images of focused-ion-beam-milled GaAs and Si p-n junctions recorded using off-axis electron holography, as well as increasing the measured phase shifts across the junctions. Our results suggest that annealing removes defects resulting from Ga+ implantation and reactivates dopant atoms in the thin TEM specimens. In GaAs, electrically inactive surface layer thicknesses are reduced from 80 to 17 nm on each specimen surface after annealing at 500 °C. In Si the improvement is from 25 to 5 nm. [ABSTRACT FROM AUTHOR]

• Conceptual difference between holography and STEM due to aperture. • Strong defocus dependency in first moment STEM imaging. • STEM more kinematic at optimum focus compared to electron holography. • Negligible effect of TDS on momentum transfer (for thin samples). Off-axis electron holography and first moment STEM are sensitive to electromagnetic potentials or fields, respectively. In this work, we investigate in what sense the results obtained from both techniques are equivalent and work out the major differences. The analysis is focused on electrostatic (Coulomb) potentials at atomic spatial resolution. It is shown that the probe-forming/objective aperture strongly affects the reconstructed electrostatic potentials and that, as a result of the different illumination setups, dynamical diffraction effects show a specific response with increasing specimen thickness. It is shown that thermal diffuse scattering is negligible for a wide range of specimen thicknesses, when evaluating the first moment of diffraction patterns. [ABSTRACT FROM AUTHOR]

Off-axis electron holography provides a direct means of retrieving the phase of the wavefield in a transmission electron microscope, enabling measurement of electric and magnetic fields at length scales from microns to nanometers. To maximise the accuracy of the technique, it is important to acquire holograms using experimental conditions that optimise the phase resolution for a given spatial resolution. These conditions are determined by a number of competing parameters, especially the spatial coherence and the instrument instabilities. Here, we describe a simple, yet accurate, model for predicting the dose rate and exposure time that give the best phase resolution in a single hologram. Experimental studies were undertaken to verify the model of spatial coherence and instrument instabilities that are required for the optimisation. The model is applicable to electron holography in both standard mode and Lorentz mode, and it is relatively simple to apply. [ABSTRACT FROM AUTHOR]

Abstract: The magnetic behaviour of magnetite at low temperatures is dominated by its transformation to a monoclinic crystal structure that is simultaneously ferrimagnetic, ferroelastic and ferroelectric below ∼125K (the Verwey transition). Here we use electron microscopy to reveal the relationship between ferrimagnetic and ferroelastic domain structures in monoclinic magnetite. We present dynamic observations of magnetite during heating and cooling across the Verwey transition, revealing a diversity of unexpected interaction phenomena between crystallographic twins and magnetic domain walls. This study provides a new understanding of the low-temperature magnetic properties of magnetite that will affect a broad range of rock magnetic studies, from the interpretation of magnetic remanence in terrestrial rocks and sediments to the search for biogenic magnetite in extraterrestrial materials. [ABSTRACT FROM AUTHOR]