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Recent advances in scanning transmission electron microscopy (STEM) have rekindled interest in multi-channel detectors and prompted the exploration of unconventional scan patterns. These emerging needs are not yet addressed by standard commercial hardware. The system described here incorporates a flexible scan generator that enables exploration of low-acceleration scan patterns, while data are recorded by a scalable eight-channel array of nonmultiplexed analog-to-digital converters. System integration with SerialEM provides a flexible route for automated acquisition protocols including tomography. Using a solid-state quadrant detector with additional annular rings, we explore the generation and detection of various STEM contrast modes. Through-focus bright-field scans relate to phase contrast, similarly to wide-field TEM. More strikingly, comparing images acquired from different off-axis detector elements reveals lateral shifts dependent on defocus. Compensation of this parallax effect leads to decomposition of integrated differential phase contrast (iDPC) to separable contributions relating to projected electric potential and to defocus. Thus, a single scan provides both a computationally refocused phase contrast image and a second image in which the signed intensity, bright or dark, represents the degree of defocus.
The electron microscope has made paramount contributions to understanding the structure of biological molecules, cells, and tissues. In general, the most faithful preservation of biological specimens and other soft-organic materials is achieved through cryogenic fixation. The embedding medium is the native aqueous environment itself, immobilized in vitrified form by rapid or pressurized cooling. Until recently, imaging of such vitrified thin specimens by electron cryo-microscopy has been nearly synonymous with wide-field transmission electron microscopy (TEM). Several new approaches have entered the cryo-microscopy field, including soft x-ray imaging, serial surface imaging using focused ion beam scanning electron microscopy, phase plates, and scanning TEM (STEM). In this article, we focus on the STEM method and its adaptation to biological cryo-microscopy. Cryogenic imaging of unstained specimens by STEM introduces specific challenges. Difficulties were long considered insurmountable, and the potential advantages were underappreciated. Future developments in experimental setup and detector technologies will allow for extension of the method to thicker specimens with improved resolution and analytic capabilities.
Ultrathin ferroelectric heterostructures (SrTiO3/BaTiO3/BaRuO3/SrRuO3) were studied by scanning transmission electron microscopy (STEM) in terms of structural distortions and atomic displacements. The TiO2-termination at the top interface of the BaTiO3 layer was changed into a BaO-termination by adding an additional BaRuO3 layer. High-angle annular dark-field (HAADF) imaging by aberration-corrected STEM revealed that an artificially introduced BaO-termination can be achieved by this interface engineering. By using fast sequential imaging and frame-by-frame drift correction, the effect of the specimen drift was significantly reduced and the signal-to-noise ratio of the HAADF images was improved. Thus, a quantitative analysis of the HAADF images was feasible, and an in-plane and out-of-plane lattice spacing of the BaTiO3 layer of 3.90 and 4.22 Å were determined. A 25 pm shift of the Ti columns from the center of the unit cell of BaTiO3 along the c-axis was observed. By spatially resolved electron energy-loss spectroscopy studies, a reduction of the crystal field splitting (CFS, ΔL3=1.93 eV) and an asymmetric broadening of the eg peak were observed in the BaTiO3 film. These results verify the presence of a ferroelectric polarization in the ultrathin BaTiO3 film.
A single layer of LaAlO3 with a nominal thickness of one unit cell, which is sandwiched between a SrTiO3 substrate and a SrTiO3 capping layer, is quantitatively investigated by high-resolution transmission electron microscopy. By the use of an aberration-corrected electron microscope and by employing sophisticated numerical image simulation procedures, significant progress is made in two aspects. First, the structural as well as the chemical features of the interface are determined simultaneously on an atomic scale from the same specimen area. Second, the evaluation of the structural and chemical data is carried out in a fully quantitative way on the basis of the absolute image contrast, which has not been achieved so far in materials science investigations using high-resolution electron microscopy. Considering the strong influence of even subtle structural details on the electronic properties of interfaces in oxide materials, a fully quantitative interface analysis, which makes positional data available with picometer precision together with the related chemical information, can contribute to a better understanding of the functionality of such interfaces.
This is a copy of the slides presented at the meeting but not formally written up for the volume.
We present a high-resolution transmission electron microscopy study, on the unit-cell scale, of the degree of tetragonality and the displacements of cations away from the centrosymmetry positions in an ultra-thin epitaxial PbZr0.2Ti0.8O3 film on a SrRuO3 electrode layer deposited on a SrTiO3 substrate. TEM results show that the lattice is highly tetragonal at the centre of the film with a c/a ratio of about 1.08, while it shows a reduced degree of tetragonality in the regions close to the interfaces. Most strikingly, we find that the maximum off-centre displacements for the central area of the film do not scale with the tetragonality in comparison with the bulk materials. The calculated switched polarization from the measured cationic displacement is 80 ìC/cm2 , and thus only half of the nominal bulk value. It is in very good agreement with electrical measurements of the switched polarization obtained via the PUND method. Furthermore, a systematic reduction of the atomic displacements is measured at the interfaces. This suggests that interface-induced suppression of the ferroelectric polarization plays a critical role in the size effect of nanoscale ferroelectrics. These issues will be discussed further in this presentation. This work was partially supported by the National Science Foundation (NSF) under Grants DMR-0132918, NSF-MRSEC DMR-0080008, and an NSF US-Europe program DMR-0244288. V.N also acknowledges the support of the Alexander von Humboldt Foundation for his stay in Germany and the financial support of an Australian Research Council Discovery Grant 0666231.
We report on magnetic properties of the GaN layers implanted with 3d transition metal ions. GaN layers grown by MOVPE on sapphire substrates, p- or n-doped, were implanted by Mn, Cr or V ions with a dose of 5×1016 cm−2 and implantation energy of 200 keV. Subsequently, a rapid thermal annealing in nitrogen atmosphere for 5 minutes at different temperatures (700°C – 1050°C) was performed. The magnetization as a function of magnetic field as well as the dependence on temperature revealed paramagnetic behavior for all samples. In addition, an antiferromagnetic coupling between implanted ions was found.
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