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A reformulated implementation of single-sideband ptychography enables analysis and display of live detector data streams in 4D scanning transmission electron microscopy (STEM) using the LiberTEM open-source platform. This is combined with live first moment and further virtual STEM detector analysis. Processing of both real experimental and simulated data shows the characteristics of this method when data are processed progressively, as opposed to the usual offline processing of a complete data set. In particular, the single-sideband method is compared with other techniques such as the enhanced ptychographic engine in order to ascertain its capability for structural imaging at increased specimen thickness. Qualitatively interpretable live results are obtained also if the sample is moved, or magnification is changed during the analysis. This allows live optimization of instrument as well as specimen parameters during the analysis. The methodology is especially expected to improve contrast- and dose-efficient in situ imaging of weakly scattering specimens, where fast live feedback during the experiment is required.
Quantitative structural characterization of nanomaterials is important to tailor their functional properties. Corrosion of AgAu-alloy nanoparticles (NPs) results in porous structures, making them interesting for applications especially in the fields of catalysis and surface-enhanced Raman spectroscopy. For the present report, structures of dealloyed NPs were reconstructed three-dimensionally using scanning transmission electron microscopy tomography. These reconstructions were evaluated quantitatively, revealing structural information such as pore size, porosity, specific surface area, and tortuosity. Results show significant differences compared to the structure of dealloyed bulk samples and can be used as input for simulations of diffusion or mass transport processes, for example, in catalytic applications.
To unambiguously evaluate the indium and nitrogen concentrations in InxGa1−xNyAs1−y, two independent sources of information must be obtained experimentally. Based on high-resolution scanning transmission electron microscopy (STEM) images taken with a high-angle annular dark-field (HAADF) detector the strain state of the InGaNAs quantum well is determined as well as its characteristic HAADF-scattering intensity. The strain state is evaluated by applying elasticity theory and the HAADF intensity is used for a comparison with multislice simulations. The combination of both allows for determination of the chemical composition where the results are in accordance with X-ray diffraction measurements, three-dimensional atom probe tomography, and further transmission electron microscopy analysis. The HAADF-STEM evaluation was used to investigate the influence of As-stabilized annealing on the InGaNAs/GaAs sample. Photoluminescence measurements show an annealing-induced blue shift of the emission wavelength. The chemical analysis precludes an elemental diffusion as origin of the energy shift—instead the results are in agreement with a model based on an annealing-induced redistribution of the atomic next-neighbor configuration.
In an earlier publication Rosenauer et al. introduced a method for determination of composition in AlGaN/GaN heterostructures from high-angle annular dark field (HAADF) images. Static atomic displacements (SADs) were neglected during simulation of reference data because of the similar covalent radii of Al and Ga. However, SADs have been shown (Grillo et al.) to influence the intensity in HAADF images and therefore could be the reason for an observed slight discrepancy between measured and nominal concentrations. In the present study parameters of the Stillinger–Weber potential were varied in order to fit computed elastic constants, lattice parameters and bonding energies to experimental ones. A reference data set of HAADF images was simulated, in which the new parameterization was used to account for SADs. Two reference samples containing AlGaN layers with different Al concentrations were investigated and Al concentrations in the layers determined based on the new data set. We found that these concentrations were in good agreement with nominal concentrations as well as concentrations determined using alternative techniques such as strain state analysis and energy dispersive X-ray spectroscopy.
In GaAs-based pseudomorphic high-electron mobility transistor device structures, strain and composition of the InxGa1−xAs channel layer are very important as they influence the electronic properties of these devices. In this context, transmission electron microscopy techniques such as (002) dark-field imaging, high-resolution transmission electron microscopy (HRTEM) imaging, scanning transmission electron microscopy-high angle annular dark field (STEM-HAADF) imaging and selected area diffraction, are useful. A quantitative comparative study using these techniques is relevant for assessing the merits and limitations of the respective techniques. In this article, we have investigated strain and composition of the InxGa1−xAs layer with the mentioned techniques and compared the results. The HRTEM images were investigated with strain state analysis. The indium content in this layer was quantified by HAADF imaging and correlated with STEM simulations. The studies showed that the InxGa1−xAs channel layer was pseudomorphically grown leading to tetragonal strain along the  growth direction and that the average indium content (x) in the epilayer is ~0.12. We found consistency in the results obtained using various methods of analysis.
Nanoporous gold is a material with many possible applications e.g. in catalysts, sensors and electrode materials. We studied the functionalization of the nanoporous gold with TiO2 particles. Aiming at the low temperature oxidation of CO, the nanoporous gold can be coated with TiO2 in order to enhance catalytic activity. Structure and distribution of the TiO2 on the gold surface are important structural features, which were investigated by transmission electron microscopy. The preparation of the porous gold was tested with focused ion beam - preparation, conventional Ar+ ion beam preparation of nanoporous gold embedded in epoxy and ultramicrotome preparation of nanoporous gold embedded in epoxy. Considering the beam damage on the structure and the contamination of the surface, ultramicrotome preparation turned out to be the best solution. It was shown, that the gold ligaments are abundantly covered by approximately 5 nm TiO2 particles. The determination of the largest lattice fringe distance in high resolution mode revealed that the crystalline nanoparticles consist of the anatase phase. The spatial Ti distribution was measured with energy filtered transmission electron microscopy. Scanning transmission electron microscopy tomography was applied to reconstruct the three-dimensional structure of the gold coated with TiO2 particles.
This article deals with the measurement of strain in semiconductor heterostructures from convergent beam electron diffraction patterns. In particular, three different algorithms in the field of (circular) pattern recognition are presented that are able to detect diffracted disc positions accurately, from which the strain in growth direction is calculated. Although the three approaches are very different as one is based on edge detection, one on rotational averages, and one on cross correlation with masks, it is found that identical strain profiles result for an InxGa1−xNyAs1−y/GaAs heterostructure consisting of five compressively and tensile strained layers. We achieve a precision of strain measurements of 7–9·10−4 and a spatial resolution of 0.5–0.7 nm over the whole width of the layer stack which was 350 nm. Being already very applicable to strain measurements in contemporary nanostructures, we additionally suggest future hardware and software designs optimized for fast and direct acquisition of strain distributions, motivated by the present studies.
A hybrid assembly was built using ZnO nanowire (NW) arrays and colloidal CdSe quantum dots (QDs) stabilized by 3-mercaptopropionic acid (MPA). The QDs were chemically linked to the nanowires through the bonds formed between the outgoing carboxyl groups of the QD stabilizers and the zinc ions on the nanowire surface. An efficient clustering attachment of the QDs was achieved via partial removal of the stabilizers of the QDs. The photoconductivity of the NW/QD assembly was investigated by selective excitation of the CdSe QDs. Oxygen desorption from the nanowire surface enhances the photoconductivity and a model involving electron transfer between the QDs and the nanowires is proposed to explain the experimental results.
Transmission electron microscopy (TEM) has been applied to analyze the thickness and the In-concentration of InGaN layers in GaN/InGaN/GaN- and AlGaN/InGaN/AlGaN-quantum well (QW) structures. Two series of samples were grown by metal organic chemical vapor deposition varying either only the growth duration for the InGaN QW or by changing the Al- concentration in the buffer layers at unaltered InGaN growth conditions. A rising average In- concentration from 6.5 to 15.4 % and a decreasing growth rate are observed with increasing growth duration. The increase of the Al-concentration in the buffer layers from 0 to 36 % strongly affects the In-incorporation during the InGaN growth, which decreases from 17.5 to 2.5 %. All samples are characterized by an inhomogeneous In-distribution containing In-rich agglomerates with a size of only a few nanometers and less pronounced composition fluctuations on a scale of 100 nm.
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