Micro-Computed Tomography (µCT) as a Tool for High-Resolution 3D Imaging and Analysis of Intraocular Lenses: Feasibility and Proof of the Methodology to Evaluate YAG Pits.

INTRODUCTION: Posterior capsule opacification (PCO) is the most frequent late sequelae after successful cataract surgery. Neodymium:yttrium aluminum garnet (Nd:YAG) laser capsulotomy is considered the gold standard and a well-accepted, safe, and effective measure in treating PCO. However, iatrogenic damage of the intraocular lens (IOL) due to inappropriate focusing is a quite common side effect. These permanent defects (YAG pits) can critically affect overall optical quality. METHODS: In this laboratory study, we used the micro-computed tomography (µCT) technique to obtain high-resolution 3D images of the lens and the YAG pits. RESULTS: To the best of our knowledge, this is the first description of a detailed analysis of IOLs with µCT technology. This non-destructive technique seems to be ideal for comparative studies, measuring dimensions of the damage, and visualizing shooting channels within the material. CONCLUSION: µCT is excellently suited to examine an IOL in detail, analyze optics and haptics in three dimensions, and to describe all kinds of changes within the IOL without damaging it.

Dislocations in ceramic electrolytes for solid-state Li batteries.

High power solid-state Li batteries (SSLB) are hindered by the formation of dendrite-like structures at high current rates. Hence, new design principles are needed to overcome this limitation. By introducing dislocations, we aim to tailor mechanical properties in order to withstand the mechanical stress leading to Li penetration and resulting in a short circuit by a crack-opening mechanism. Such defect engineering, furthermore, appears to enable whisker-like Li metal electrodes for high-rate Li plating. To reach these goals, the challenge of introducing dislocations into ceramic electrolytes needs to be addressed which requires to establish fundamental understanding of the mechanics of dislocations in the particular ceramics. Here we evaluate uniaxial deformation at elevated temperatures as one possible approach to introduce dislocations. By using hot-pressed pellets and single crystals grown by Czochralski method of Li6.4La3Zr1.4Ta0.6O12 garnets as a model system the plastic deformation by more than 10% is demonstrated. While conclusions on the predominating deformation mechanism remain challenging, analysis of activation energy, activation volume, diffusion creep, and the defect structure potentially point to a deformation mechanism involving dislocations. These parameters allow identification of a process window and are a key step on the road of making dislocations available as a design element for SSLB.

Mechanical behavior of in-situ alloyed Ti6Al4V(ELI)-3 at.% Cu lattice structures manufactured by laser powder bed fusion and designed for implant applications.

In the present study, cellular lattice structures for implant applications are reported for the first-time incorporating copper directly by in-situ alloying in the laser powder bed fusion process. The aim to incorporate 3 at.% Cu into Ti6Al4V(ELI) is selected for improved antibacterial properties while maintaining appropriate mechanical properties. Previously, topologically optimized Ti6Al4V(ELI) lattice structures were successfully designed, manufactured and studied for implant applications. The development of a new alloy produced by in-situ alloying of elemental powder mixture of Ti6Al4V(ELI) and pure Cu powders was used here for the production of identical lattice structures with improved antibacterial properties. One of the same as-designed CAD models was used for the manufacturing of these lattices compared to previous work on pure Ti6Al4V(ELI) lattices, making direct comparison of mechanical properties possible. Similar manufacturability highlights the applicability of this alloying technique to other lattice designs. Microstructural characterization was performed by optical and electron microscopies, as well as microCT. Mechanical characterization was performed by means of compression tests and hardness measurements. Results showed that in-situ alloying with copper leads to the formation of localized Cu-rich regions, refinement of martensitic phase and the formation of CuTi2 intermetallic precipitates, which increased the hardness and strength of the material. Deviations in wall thickness between the as-designed and as-manufactured lattices led to anisotropy of the mechanical properties of the lattices. Higher compressive strength values were obtained when thicker walls were oriented along the loading direction. Nevertheless, alloying with Cu had a higher impact on the compressive strength of lattice structure than the wall thickness deviations. The direct in-situ alloying of copper in Ti6Al4V(ELI) is a promising route for direct manufacturing of antibacterial implants.

Large magnetic gap at the Dirac point in Bi2Te3/MnBi2Te4 heterostructures.

Magnetically doped topological insulators enable the quantum anomalous Hall effect (QAHE), which provides quantized edge states for lossless charge-transport applications1-8. The edge states are hosted by a magnetic energy gap at the Dirac point2, but hitherto all attempts to observe this gap directly have been unsuccessful. Observing the gap is considered to be essential to overcoming the limitations of the QAHE, which so far occurs only at temperatures that are one to two orders of magnitude below the ferromagnetic Curie temperature, TC (ref. 8). Here we use low-temperature photoelectron spectroscopy to unambiguously reveal the magnetic gap of Mn-doped Bi2Te3, which displays ferromagnetic out-of-plane spin texture and opens up only below TC. Surprisingly, our analysis reveals large gap sizes at 1 kelvin of up to 90 millielectronvolts, which is five times larger than theoretically predicted9. Using multiscale analysis we show that this enhancement is due to a remarkable structure modification induced by Mn doping: instead of a disordered impurity system, a self-organized alternating sequence of MnBi2Te4 septuple and Bi2Te3 quintuple layers is formed. This enhances the wavefunction overlap and size of the magnetic gap10. Mn-doped Bi2Se3 (ref. 11) and Mn-doped Sb2Te3 form similar heterostructures, but for Bi2Se3 only a nonmagnetic gap is formed and the magnetization is in the surface plane. This is explained by the smaller spin-orbit interaction by comparison with Mn-doped Bi2Te3. Our findings provide insights that will be crucial in pushing lossless transport in topological insulators towards room-temperature applications.

Self-organized Sr leads to solid state twinning in nano-scaled eutectic Si phase.

A new mechanism for twin nucleation in the eutectic Al-Si alloy with trace Sr impurities is proposed. Observations made by sub-angstrom resolution scanning transmission electron microscopy and X-ray probing proved the presence of <110> Sr columns located preferentially at twin boundaries. Density functional theory simulations indicate that Sr atoms bind in the Si lattice only along the <110> direction, with preferential positions at first and second nearest neighbors for interstitial and substitutional Sr, respectively. Density functional theory total energy calculations confirm that twin nucleation at Sr columns is energetically favorable. Hence, twins may nucleate in Si precipitates after solidification, which provides a different perspective to the currently accepted mechanism which suggests twin formation during precipitate growth.

On the quantitativeness of EDS STEM.

Chemical mapping using energy dispersive X-ray spectroscopy (EDS) in scanning transmission electron microscopy (STEM) has recently shown to be a powerful technique in analyzing the elemental identity and location of atomic columns in materials at atomic resolution. However, most applications of EDS STEM have been used only to qualitatively map whether elements are present at specific sites. Obtaining calibrated EDS STEM maps so that they are on an absolute scale is a difficult task and even if one achieves this, extracting quantitative information about the specimen - such as the number or density of atoms under the probe - adds yet another layer of complexity to the analysis due to the multiple elastic and inelastic scattering of the electron probe. Quantitative information may be obtained by comparing calibrated EDS STEM with theoretical simulations, but in this case a model of the structure must be assumed a priori. Here we first theoretically explore how exactly elastic and thermal scattering of the probe confounds the quantitative information one is able to extract about the specimen from an EDS STEM map. We then show using simulation how tilting the specimen (or incident probe) can reduce the effects of scattering and how it can provide quantitative information about the specimen. We then discuss drawbacks of this method - such as the loss of atomic resolution along the tilt direction - but follow this with a possible remedy: precession averaged EDS STEM mapping.

A quantitative analysis of a multi-phase polycrystalline cubic boron nitride tool material using DualEELS.

This paper presents a quantitative analysis of a polycrystalline cubic boron nitride tool material by electron energy-loss spectroscopy spectrum imaging acquired in dual range mode. Having both the low-loss and core-loss regions acquired nearly simultaneously provides the advantage of accurate corrections for thickness effects and thus the possibility to perform quantification calculations. This has resulted in extracted bonding maps with areal (atoms/nm(2)) or volumetric (atoms/nm(3)) densities. Spectroscopic signatures in the low-loss and core-loss energy ranges, of the elements (Al, B, C, N, Ti and O) present in the existing phases, were studied and used when extracting the element specific bonding maps by the multiple linear least squares fitting procedure. Variations of elemental concentrations across the investigated area were determined, despite of phase overlap in the beam direction or energy overlaps in the EELS spectrum. Moreover, the surface oxidation of Ti(C,N) and AlN as well as the amorphisation of α-Al(2)O(3) is discussed.

Monochromated, spatially resolved electron energy-loss spectroscopic measurements of gold nanoparticles in the plasmon range.

Gold nanoparticles show optical properties different from bulk material due to resonance phenomena which depend on local structure and geometry. Electron energy-loss spectrometry (EELS) in scanning transmission electron microscopy (STEM) allows the spatially resolved measurement of these properties at a resolution of few nanometers. In this work, the first monochromated measurements of gold nanoparticles (spheres, rods and triangles) are presented. Due to the improved energy resolution of about 0.2 eV, surface plasmon excitations at energies below 1 eV could be accurately measured from raw experimental data.

The influence of beam defocus on volume growth rates for electron beam induced platinum deposition.

Electron beam induced deposition (EBID) is a versatile method for the controlled fabrication of conducting, semi-conducting and non-conducting structures down to the nanometer scale. In contrast to ion beam induced deposition, EBID processes are free of sputter effects, ion implantation and massive heat generation; however, they have much lower deposition rates. To push the deposition efficiency further towards its intrinsic limits, the individual influences of the process parameters have to be explored. In this work a platinum pre-cursor is used for the deposition of conducting nanorods on highly oriented pyrolytic graphite. The study shows the influence of a beam defocus during deposition on the volume growth rates. The temporal evolution of volume growth rates reveals a distinct maximum which is dependent on the defocus introduced, leading to an increase of deposited volumes by a factor 2.5 after the same deposition times. The observed maximum is explained by an increasing and saturating electron yield contributing to the final deposition process and constantly decreasing diffusion abilities of the pre-cursor molecules toward the tip of the nanorods, which is further supported by dwell time experiments.

High resolution EELS using monochromator and high performance spectrometer: comparison of V2O5 ELNES with NEXAFS and band structure calculations.

Using single crystal V2O5 as a sample, we tested the performance of the new aberration corrected GATAN spectrometer on a monochromatised 200 kV FEG FEI (S)TEM. The obtained V L and O K ELNES were compared with that obtained in a common GATAN GIF and that in the new spectrometer, without monochromatised beam. The performance of the new instrumentation is impressive: recorded with an energy-resolution of 0.22 eV, the V L(3) edge reveals all the features due to the bulk electronic structure, that are also revealed in near-edge X-ray absorption fine structure (NEXAFS) with a much higher energy-resolution (0.08 eV). All features of the ELNES and NEXAFS are in line with a theoretical spectrum derived from band-structure calculations.

Electron energy-loss near-edge structures of 3d transition metal oxides recorded at high-energy resolution.

Near-edge fine structures of the metal L(2,3) and O K-edges in transition metal-oxides have been studied with a transmission electron microscope equipped with a monochromator and a high-resolution imaging filter. This system enables the recording of EELS spectra with an energy resolution of 0.1eV thus providing new near-edge fine structure details which could not be observed previously by EELS in conventional TEM instruments. EELS-spectra from well-defined oxides like titanium oxide (TiO(2)), vanadium oxide (V(2)O(5)), chromium oxide (Cr(2)O(3)), iron oxide (Fe(2)O(3)), cobalt oxide (CoO) and nickel oxide (NiO) have been measured with the new system. These spectra are compared with EELS data obtained from a conventional microscope and the main spectral features are interpreted. Additionally, the use of monochromised TEMs is discussed in view of the natural line widths of K and L(2,3) edges.

Quantitative Energy-filtering Transmission Electron Microscopy in Materials Science.

Energy-filtered transmission electron microscopy (EFTEM) can be used to acquire elemental distribution images at high lateral resolution within short acquisition times. In this article, we present an overview of typical problems from materials science which can be preferentially solved by means of EFTEM. In the first example, we show how secondary phases in a steel specimen can be easily detected by recording jump ratio images of the matrix element under rocking beam illumination. Secondly, we describe how elemental maps can be converted into concentration maps. A Ba-Nd-titanate ceramics serves as a typical materials science example exhibiting three different compounds with varying composition. In order to reduce diffraction and/or thickness variation effects which may be a problem for quantification of crystalline specimens, we calculated atomic ratio maps by dividing two elemental maps and subsequent normalizing by the partial ionization cross-sections (or k-factors). Additionally, the atomic ratio maps are correlated using the scatter diagram technique thus leading to quantitative chemical phase maps. Finally, we show how the near-edge structures (electron energy-loss near edge fine structures, or ELNES) can be used for mapping chemical bonding states thus differentiating between various modifications of an element. In order to distinguish between diamond and non-diamond carbon in diamond coated materials, we have investigated a diamond layer on a substrate with the help of ELNES mapping utilizing the pi*-peak of the C-K ionization edge.