Structural and chemical characterization of nanomaterials provides important information for understanding their functional properties. Nanomaterials with characteristic structure sizes in the nanometer range can be characterized by scanning transmission electron microscopy (STEM). In conventional STEM, two-dimensional (2D) projection images of the samples are acquired, information about the third dimension is lost.
View Article and Find Full Text PDFAtomic electric fields in a thin GaN sample are measured with the centre-of-mass approach in 4D-scanning transmission electron microscopy (4D-STEM) using a 12-segmented STEM detector in a Spectra 300 microscope. The electric fields, charge density and potential are compared to simulations and an experimental measurement using a pixelated 4D-STEM detector. The segmented detector benefits from a high recording speed, which enables measurements at low radiation doses.
View Article and Find Full Text PDFThe development of a novel reactive spray technology based on the well-known gas-phase metal oxide synthesis route provides innumerable opportunities for the production of non-oxide nanoparticles. Among these materials, metal sulfides are expected to have a high impact, especially in the development of electrochemical and photochemical high-surface-area materials. As a proof-of-principle, MnS, CoS, Cu S, ZnS, Ag S, In S , SnS, and Bi S are synthesized in an O -lean and sulfur-rich environment.
View Article and Find Full Text PDFThe ISTEM mode for TEM has been demonstrated to have several advantages in regard to resolution and precision. While previous works primarily focussed on the advantages due to the reduced spatial coherence, the actual image contrast, i.e.
View Article and Find Full Text PDFIn this paper we perform angular resolved annular-dark field (ADF) scanning-transmission electron microscopy (STEM) to study the scattered intensity in an InGaN layer buried in GaN as a function of the scattering angle. We achieved angular resolution with a motorized iris aperture in front of the ADF detector. Using this setup, we investigated how the intensities measured in various angular ranges agree with multislice simulations in the frozen-lattice approximation.
View Article and Find Full Text PDFThe measurement of electric fields in scanning transmission electron microscopy (STEM) is a highly investigated field of research. The constant improvement of spatial resolution in STEM and the development of new hardware for the fast acquisition of diffraction patterns even paved the way for the measurement of atomic electric fields. Although the basic principle that an electric field leads to a tilt of the focussed electron probe that can be detected as a shift of the diffraction pattern in the back focal plane of the objective lens seems quite simple, many challenges arose in the measurement of fields in a quantitative way.
View Article and Find Full Text PDFPorous networks of Pt nanoparticles interlinked by bifunctional organic ligands have shown high potential as catalysts in micro-machined hydrogen gas sensors. By varying the ligand among p-phenylenediamine, benzidine, 4,4''-diamino-p-terphenyl, 1,5-diaminonaphthalene, and trans-1,4-diaminocyclohexane, new variants of such networks were synthesized. Inter-particle distances within the networks, determined via transmission electron microscopy tomography, varied from 0.
View Article and Find Full Text PDF4D-scanning transmission electron microscopy (4D-STEM) can be used to measure electric fields such as atomic fields or polarization-induced electric fields in crystal heterostructures. The paper focuses on effects occurring in 4D-STEM at interfaces, where two model systems are used: an AlN/GaN nanowire superlattice as well as a GaN/vacuum interface. Two different methods are applied: First, we employ the centre-of mass (COM) technique which uses the average momentum transfer evaluated from the intensity distribution in the diffraction pattern.
View Article and Find Full Text PDFQuantitative 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.
View Article and Find Full Text PDFThe film thickness plays an important role in the performance of materials applicable to different technologies including chemical sensors, catalysis and/or energy materials. The relationship between the surface and volume of the functional layers is key to high performance evaluations. Here we demonstrate the thermophoretic deposition of different thicknesses of the functional layers designed using flame combustion of tin 2-ethylhexanoate dissolved in xylene, and measurement of thickness by scanning electron microscopy and focused ion beam.
View Article and Find Full Text PDFThe spinel LiMnO (LMO) is a promising cathode material for rechargeable Li-ion batteries due to its excellent properties, including cost effectiveness, eco-friendliness, high energy density, and rate capability. The commercial application of LiMnO is limited by its fast capacity fading during cycling, which lowers the electrochemical performance. In the present work, phase-pure and crystalline LiMnO spinel in the nanoscale were synthesized using single flame spray pyrolysis via screening 16 different precursor-solvent combinations.
View Article and Find Full Text PDFIn this paper we study the effect of lens aberrations (spherical aberration and astigmatism), beam tilt, contamination and shot noise on the accuracy and precision of position determination in imaging scanning transmission electron microscopy (ISTEM) on the example of BaTiO. ISTEM images are simulated as a function of sample thickness and defocus starting from a nearly perfect microscope setting. A defocus range was identified, in which atom column positions were reliably visible and could be decently measured.
View Article and Find Full Text PDFModern quantitative TEM methods such as the ζ-factor technique require precise knowledge of the electron beam current. To this end, a macroscopic Faraday cup was designed and constructed. It can replace the viewing screen in the projection chamber of a TEM and guarantees highly accurate measurement of the electron beam with precision only limited by the used amperemeter.
View Article and Find Full Text PDFThe angle-resolved electron scattering is investigated in scanning-transmission electron microscopy (STEM) using a motorised iris aperture placed above a conventional annular detector. The electron intensity scattered into various angle ranges is compared with simulations that were carried out in the frozen-lattice approximation. As figure of merit for the agreement of experiment and simulation we evaluate the specimen thickness which is compared with the thickness obtained from position-averaged convergent beam electron diffraction (PACBED).
View Article and Find Full Text PDFStrain analysis by nano-beam electron diffraction allows for measurements of strain with nanometre resolution in a large field of view. This is done by evaluating distances between diffraction discs in diffraction patterns acquired while a focussed electron beam is scanned across the sample in a transmission electron microscope. The bottleneck of this method is a precise determination of diffraction disc positions, which suffers from the inner structure of the discs caused by dynamical diffraction.
View Article and Find Full Text PDFScanning transmission electron microscopy (STEM) allows to gain quantitative information on the atomic-scale structure and composition of materials, satisfying one of todays major needs in the development of novel nanoscale devices. The aim of this study is to quantify the impact of inelastic, i.e.
View Article and Find Full Text PDFTin dioxide (SnO) nanoparticles synthesized flame spray pyrolysis (FSP) have promising applications for gas sensors. The formation of SnO nanoparticles in the gas-phase has been investigated using single droplet combustion and FSP. Precursor solutions of Tin (II) 2-ethylhexanoate dissolved in Xylene with varying Sn concentrations were selected as the precursor-solvent system.
View Article and Find Full Text PDFImages acquired in transmission electron microscopes can be distorted for various reasons such as e.g. aberrations of the lenses of the imaging system or inaccuracies of the image recording system.
View Article and Find Full Text PDFStrain analyses from experimental series of nano-beam electron diffraction (NBED) patterns in scanning transmission electron microscopy are performed for different specimen tilts. Simulations of NBED series are presented for which strain analysis gives results that are in accordance with experiment. This consequently allows to study the relation between measured strain and actual underlying strain.
View Article and Find Full Text PDFFor simulation of transmission electron microscopic images and diffraction patterns, the accurate inclusion of thermal diffuse scattering by phonons is important. In the frozen phonon multislice algorithm, this is possible, if thermal displacements according to the realistic, quantum mechanical distribution can be generated. For pure crystals, quantum mechanical calculations based on DFT yield those displacements.
View Article and Find Full Text PDFUltrathin bimetallic nanowires are of importance and interest for applications in electronic devices such as sensors and heterogeneous catalysts. In this work, we have designed a new, highly reproducible and generalized wet chemical method to synthesize uniform and monodispersed Au-based alloy (AuCu, AuPd, and AuPt) nanowires with tunable composition using microwave-assisted reduction at the liquid-liquid interface. These ultrathin alloy nanowires are below 4 nm in diameter and about 2 μm long.
View Article and Find Full Text PDFThe chemical composition of four SiGe layers grown on silicon was determined from quantitative scanning transmission electron microscopy (STEM). The chemical analysis was performed by a comparison of the high-angle annular dark field (HAADF) intensity with multislice simulations. It could be shown that amorphous surface layers originating from the preparation process by focused-ion beam (FIB) at 30 kV have a strong influence on the quantification: the local specimen thickness is overestimated by approximately a factor of two, and the germanium concentration is substantially underestimated.
View Article and Find Full Text PDFMagnetic skyrmions are topologically protected whirls that decay through singular magnetic configurations known as Bloch points. We used Lorentz transmission electron microscopy to infer the energetics associated with the topological decay of magnetic skyrmions far from equilibrium in the chiral magnet Fe Co Si. We observed that the lifetime τ of the skyrmions depends exponentially on temperature, [Formula: see text].
View Article and Find Full Text PDFDenisovite is a rare mineral occurring as aggregates of fibres typically 200-500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD), electron crystallography, modelling and Rietveld refinement will be reported.
View Article and Find Full Text PDF