Juri Barthel

Direct imaging of single Au atoms within GaAs nanowires.

Incorporation of catalyst atoms during the growth process of semiconductor nanowires reduces the electron mean free path and degrades their electronic properties. Aberration-corrected scanning transmission electron microscopy (STEM) is now capable of directly imaging single Au atoms within the dense matrix of a GaAs crystal, by slightly tilting the GaAs lattice planes with respect to the incident electron beam. Au doping values in the order of 10(17-18) cm(3) were measured, making ballistic transport through the nanowires practically inaccessible.

Metal carbonyls supported on iron oxide nanoparticles to trigger the CO-gasotransmitter release by magnetic heating

Magnetic iron oxide, maghemite (Fe2O3) nanoparticles with covalent surface-bound CO-releasing molecules (CORMs) can be triggered to release CO through heating in an alternating magnetic field. In the proof-of-concept study the rate of CO-release from [RuCl(CO3)(μ-DOPA)]@maghemite nanoparticles was doubled upon exposure to an external alternating magnetic field (31.7 kAm(-1), 247 kHz, 25 °C, 39.9 mTesla, DOPA = dioxyphenyl-alaninato).

Determination of the 3D shape of a nanoscale crystal with atomic resolution from a single image

Although the overall atomic structure of a nanoscale crystal is in principle accessible by modern transmission electron microscopy, the precise determination of its surface structure is an intricate problem. Here, we show that aberration-corrected transmission electron microscopy, combined with dedicated numerical evaluation procedures, allows the three-dimensional shape of a thin MgO crystal to be determined from only one single high-resolution image. The sensitivity of the reconstruction procedure is not only sufficient to reveal the surface morphology of the crystal with atomic resolution, but also to detect the presence of adsorbed impurity atoms. The single-image approach that we introduce offers important advantages for three-dimensional studies of radiation-sensitive crystals.

Aberration measurement in HRTEM: Implementation and diagnostic use of numerical procedures for the highly precise recognition of diffractogram patterns

The precise characterisation of the instrumental imaging properties in the form of aberration parameters constitutes an almost universal necessity in quantitative HRTEM, and is underlying most hardware and software techniques established in this field. We focus in this paper on the numerical analysis of individual diffractograms as a first preparatory step for further publications on HRTEM aberration measurement. The extraction of the defocus and the 2-fold astigmatism from a diffractogram is a classical pattern recognition problem, which we believe to have solved in a near-optimum way concerning precision, speed, and robustness. The newly gained measurement precision allows us to resolve fluctuations of the defocus and the 2-fold astigmatism and to assess thereby the optical stability of electron microscopes. Quantitative stability criteria are elaborated, which may serve as helpful guidelines for daily work as well as for microscope acceptance tests.

StripeSTEM, a technique for the isochronous acquisition of high angle annular dark-field images and monolayer resolved electron energy loss spectra

A technique capable of producing monolayer resolved electron energy loss (EEL) spectroscopy data along one direction in crystal structures is introduced. Unambiguous assignment of EEL spectra to atomic planes is possible via the execution of high angle annular dark-field (HAADF) imaging and EEL spectrum acquisition in parallel. The recording of instrumental instabilities in the HAADF image during the measurement enables a proper quantification by virtue of post-acquisition correction. Compared to the conventional line profile technique a dose reduction by several orders of magnitude can be achieved. The technique is applied to bulk SrTiO(3) and ZnO:In(2)O(3) in order to explore its capabilities and limits. Monolayer resolution was achieved for the Ti-L(23) and In-M(45) core-losses. Multislice calculations were carried out for the purpose of assessing the residual delocalisation of the inelastic signal. Fundamental limits to the resolution are imposed by dynamical dispersion of the electron wave in the crystal combined with the extension of the inelastic potential. In the present case, owing to the requirement of a high beam current, the geometrical probe size cannot be neglected when compared to the width of an inelastic scattering potential.

On the optical stability of high-resolution transmission electron microscopes.

In the recent two decades the technique of high-resolution transmission electron microscopy experienced an unprecedented progress through the introduction of hardware aberration correctors and by the improvement of the achievable resolution to the sub-Ångström level. The important aspect that aberration correction at a given resolution requires also a well defined amount of optical stability has received little attention so far. Therefore we investigate the qualification of a variety of high-resolution electron microscopes to maintain an aberration corrected optical state in terms of an optical lifetime. We develop a comprehensive statistical framework for the estimation of the optical lifetime and find remarkably low values between tens of seconds and a couple of minutes. Probability curves are introduced, which inform the operator about the chance to work still in the fully aberration corrected state.

Weakly-coordinated stable platinum nanocrystals

Stable platinum nanocrystals with small diameters (1.0–2.3 nm), that are stable for a long time, with narrow size distributions were easily and reproducibly prepared without any additional stabilizers in glycol, glycerol, the ionic liquids (ILs) 1-n-butyl-3-methyl-imidazolium tetrafluoroborate [BMIm][BF4] and N-butyl-N-trimethyl-ammonium bis(trifluoromethylsulfonyl)imide [N4111][NTf2] or diphenylmethane (CH2Ph2) by thermal, photolytic or microwave assisted decomposition of the organometallic precursor methylcyclopentadienyl-trimethylplatinum(IV), (MeCp)PtMe3. Decomposition of the easily dispensible, air and moisture stable organometallic Pt(IV) precursor (MeCp)PtMe3 leads to well defined, small, crystalline and longterm stable Pt-nanoparticle (Pt-NP) dispersions without any additional surface-capping ligands. The Pt-NP/IL dispersion was shown to be a highly active catalyst (TOF 96 000 h−1 at 0.0125 mol% Pt and quantitative conversion) for the biphasic hydrosilylation of phenylacetylene with triethylsilane, to the distal and proximal products triethyl(2- and1-phenylvinyl)silane.

On the origin of differential phase contrast at a locally charged and globally charge-compensated domain boundary in a polar-ordered material

Differential phase contrast (DPC) imaging in the scanning transmission electron microscope is applied to the study of a charged antiphase domain boundary in doped bismuth ferrite. A clear differential signal is seen, which matches the expected direction of the electric field at the boundary. However, further study by scanned diffraction reveals that there is no measurable deflection of the primary diffraction disc and hence no significant free E-field in the material. Instead, the DPC signal arises from a modulation of the intensity profile within the primary diffraction disc in the vicinity of the boundary. Simulations are used to show that this modulation arises purely from the local change in crystallographic structure at the boundary and not from an electric field. This study highlights the care that is required when interpreting signals recorded from ferroelectric materials using both DPC imaging and other phase contrast techniques.

Atomic-scale measurement of structure and chemistry of a single-unit-cell layer of LaAlO3 embedded in SrTiO3

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.

Performance of a direct detection camera for off-axis electron holography

The performance of a direct detection camera (DDC) is evaluated in the context of off-axis electron holographic experiments in a transmission electron microscope. Its performance is also compared directly with that of a conventional charge-coupled device (CCD) camera. The DDC evaluated here can be operated either by the detection of individual electron events (counting mode) or by the effective integration of many such events during a given exposure time (linear mode). It is demonstrated that the improved modulation transfer functions and detective quantum efficiencies of both modes of the DDC give rise to significant benefits over the conventional CCD cameras, specifically, a significant improvement in the visibility of the holographic fringes and a reduction of the statistical error in the phase of the reconstructed electron wave function. The DDCs linear mode, which can handle higher dose rates, allows optimisation of the dose rate to achieve the best phase resolution for a wide variety of experimental conditions. For suitable conditions, the counting mode can potentially utilise a significantly lower dose to achieve a phase resolution that is comparable to that achieved using the linear mode. The use of multiple holograms and correlation techniques to increase the total dose in counting mode is also demonstrated.