Long-term static dissolution experiments, lasting up to ∼1500 days, were conducted on International Simple Glass (ISG) and SON68 glass under hyperalkaline pH, at 70 °C, and at a very high glass surface area to solution volume ratio. The study compared (1) glass dissolution kinetics, (2) secondary phase formation, and (3) the microstructure of the altered glass and secondary phase interface. Boron release indicated rapid initial dissolution followed by a slowdown mainly due to a significant pH drop.
View Article and Find Full Text PDFQuantitative interpretation of transmission electron microscopy (TEM) data of crystalline specimens often requires the accurate knowledge of the local crystal orientation. A method is presented which exploits momentum-resolved scanning TEM (STEM) data to determine the local mistilt from a major zone axis. It is based on a geometric analysis of Kikuchi bands within a single diffraction pattern, yielding the center of the Laue circle.
View Article and Find Full Text PDFMachine learning approaches for image analysis require extensive training datasets for an accurate analysis. This also applies to the automated analysis of electron microscopy data where training data are usually created by manual annotation. Besides nanoparticle shape and size distribution, their internal crystal structure is a major parameter to assess their nature and their physical properties.
View Article and Find Full Text PDFWe show that diffraction intensity into the first-order Laue zone (FOLZ) of a crystal can have a strong azimuthal dependence, where this FOLZ ring appears solely because of unidirectional atom position modulation. Such a modulation was already known to cause the appearance of elliptical columns in atom-resolution images, but we show that measurement of the angle via four-dimensional scanning transmission electron microscopy (4DSTEM) is far more reliable and allows the measurement of the modulation direction with a precision of about 1° and an accuracy of about 3°. This method could be very powerful in characterizing atomic structures in three dimensions by 4DSTEM, especially in cases where the structure is found only in nanoscale regions or crystals.
View Article and Find Full Text PDFThe LUX-ZEPLIN experiment is a dark matter detector centered on a dual-phase xenon time projection chamber operating at the Sanford Underground Research Facility in Lead, South Dakota, USA. This Letter reports results from LUX-ZEPLIN's first search for weakly interacting massive particles (WIMPs) with an exposure of 60 live days using a fiducial mass of 5.5 t.
View Article and Find Full Text PDFPhonon scattering at grain boundaries (GBs) is significant in controlling the nanoscale device thermal conductivity. However, GBs could also act as waveguides for selected modes. To measure localized GB phonon modes, milli-electron volt (meV) energy resolution is needed with subnanometer spatial resolution.
View Article and Find Full Text PDFUtilizing advanced transmission electron microscopy (TEM), the structure at the (110)-type twin boundary (TB) of Ce-doped GdFeO (C-GFO) has been investigated with picometer precision. Such a TB is promising to generate local ferroelectricity within a paraelectric system, while precise knowledge about its structure is still largely missing. In this work, a direct measurement of the cation off-centering with respect to the neighboring oxygen is enabled by integrated differential phase contrast (iDPC) imaging, and up to 30 pm Gd off-centering is highly localized at the TB.
View Article and Find Full Text PDFTreatment of food-producing animals with veterinary medicinal products (VMPs) can result in residues in foodstuffs (e.g. eggs, meat, milk, or honey) representing a potential consumer health risk.
View Article and Find Full Text PDFIridium oxide (IrO-NP) and palladium nanoparticles (Pd-NP) were supported on a 2,6-dicyanopyridine-based covalent-triazine framework (DCP-CTF) by energy-saving and sustainable microwave-assisted thermal decomposition reactions in propylene carbonate and in the ionic liquid [BMIm][NTf]. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) confirm well-distributed NPs with sizes from 2 to 13 nm stabilized on the CTF particles. Metal contents between 10 and 41 wt% were determined by flame atomic absorption spectroscopy (AAS).
View Article and Find Full Text PDF: Hip fractures are among the most typical geriatric fractures. Subtrochanteric fractures are considered difficult to treat, and, to date, there is no consensus on the optimal surgical treatment. : We analyzed data from the Registry for Geriatric Trauma, which includes patients ≥ 70 years old with hip fractures or periprosthetic fractures requiring surgery (21,734 patients in 2017-2019).
View Article and Find Full Text PDFIt is shown that higher order Laue zone (HOLZ) rings in high energy electron diffraction are specific to individual columns of atoms, and show different strengths, structure and radii for different atom columns along the same projection in a structure. An atomic resolution 4-dimensional STEM dataset is recorded from a <110> direction in a perovskite trilayer, where only the central LaFeO layer should show a period doubling that gives rise to an extra HOLZ ring. Careful comparison between experiment and multislice simulations is used to understand the origins of all features in the patterns.
View Article and Find Full Text PDFStatic dissolution experiments were carried out with the reference International Simple Glass under hyperalkaline pH at 70 °C and very high SA/V ratio. Three aspects of glass dissolution behavior were investigated, (1) the rate drop regime and the residual rate (stage II), (2) the formation of secondary phases including thermodynamic aspects, and (3) the microstructure of the interface of altered glass and secondary phases. A very low residual rate of 6 × 10 g/md was determined based on boron release, which was several orders of magnitude lower than the initial rate established between the start of the experiments and the first sampling on day 59.
View Article and Find Full Text PDFGold nanoparticles (Au NPs) are studied as delivery systems to enhance the effect of the glutaminase1 inhibitor CB839, a promising drug candidate already in clinical trials for tumor treatments. Au NPs were synthesized using a bottom-up approach and covered with polymers able to bind CB839 as a Au-polymer-CB839 conjugate. The drug loading efficiency (DLE) was determined using high-performance liquid chromatography and characterization of the CB839-loaded NPs was done with various microscopic and spectroscopic methods.
View Article and Find Full Text PDFElectron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI) are used to extract crystallographic information from bulk samples, such as their crystal structure and orientation as well as the presence of any dislocation and grain boundary defects. These techniques rely on the backscattered electron signal, which has a large distribution in electron energy. Here, the influence of plasmon excitations on EBSD patterns and ECCI dislocation images is uncovered by multislice simulations including inelastic scattering.
View Article and Find Full Text PDFUnlabelled: Patients suffering from complications during inpatient treatment after hip fracture surgery are associated with a worse mid-term outcome. While surgically treatable complications only delay the healing process, internal complications seem to worsen the outcome in the long run. All complications come with significant increased costs during the hospital stay.
View Article and Find Full Text PDFAim: Due to demographic change, the number of geriatric patients is still rising. Although hip fractures are the subject of current research, little is known about the remaining geriatric trauma entities. The aim of this study was to collect data of the age-related traumatological intensive care unit (ICU) population, its underlying diagnosis, and the influence on mortality and length of stay in the ICU.
View Article and Find Full Text PDFCovalent triazine frameworks (CTFs) are little investigated, albeit they are promising candidates for electrocatalysis, especially for the oxygen evolution reaction (OER). In this work, nickel nanoparticles (from Ni(COD)) were supported on CTF-1 materials, which were synthesized from 1,4-dicyanobenzene at 400 °C and 600 °C by the ionothermal method. CTF-1-600 and Ni/CTF-1-600 show high catalytic activity towards OER and a clear activity for the electrochemical oxygen reduction reaction (ORR).
View Article and Find Full Text PDFOff-axis electron holography and first moment STEM are sensitive to electromagnetic potentials or fields, respectively. In this work, we investigate in what sense the results obtained from both techniques are equivalent and work out the major differences. The analysis is focused on electrostatic (Coulomb) potentials at atomic spatial resolution.
View Article and Find Full Text PDFThe ability to create atomically perfect, epitaxial heterostructures of correlated complex perovskite oxides using state-of-art thin film deposition techniques has generated new physical phenomena at engineered interfaces. Here we report on the impact of growth kinetics on the magnetic structure and exchange coupling at the interface in heterostructures combining layers of antiferromagnetic LaSrFeO (LSFO) and ferromagnetic LaSrMnO (LSMO) on (0 0 1)-oriented SrTiO (STO) substrates. Two growth orders are investigated, (a) LSMO/LSFO/STO(0 0 1) and (b) LSFO/LSMO/STO(0 0 1), where the LSFO layer is grown by molecular beam epitaxy and the LSMO layer by high oxygen pressure sputtering.
View Article and Find Full Text PDFNiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS).
View Article and Find Full Text PDFAim: The importance of proximal femoral fractures is increasing due to demographic change. Despite appropriate care, these are associated with poor results. We are still lagging behind, and require information on the long-term functional outcome of these patients and the predictive factors involved.
View Article and Find Full Text PDFBackground And Objective: Malnutrition in geriatric trauma patients is associated with an increased risk of complications and mortality and is therefore a key risk factor. The assessment of the affected patients plays an important role in improving the outcome of this growing patient group.
Material And Methods: In 2016 a questionnaire was sent to 571 departments specialized in traumatology and orthopedics throughout Germany.
Decomposition of rare-earth tris(,'-diisopropyl-2-methylamidinato)metal(III) complexes [RE{MeC(N(iPr))}] (RE(amd); RE = Pr(III), Gd(III), Er(III)) and tris(2,2,6,6-tetramethyl-3,5-heptanedionato)europium(III) (Eu(dpm)) induced by microwave heating in the ionic liquids (ILs) 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF]), 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([BMIm][NTf]) and in propylene carbonate (PC) yield oxide-free rare-earth metal nanoparticles (RE-NPs) in [BMIm][NTf] and PC for RE = Pr, Gd and Er or rare-earth metal-fluoride nanoparticles (REF-NPs) in the fluoride-donating IL [BMIm][BF] for RE = Pr, Eu, Gd and Er. The crystalline phases and the absence of significant oxide impurities in RE-NPs and REF-NPs were verified by powder X-ray diffraction (PXRD), selected area electron diffraction (SAED) and high-resolution X-ray photoelectron spectroscopy (XPS). The size distributions of the nanoparticles were determined by transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) to an average diameter of (11 ± 6) to (38 ± 17) nm for the REF-NPs from [BMIm][BF].
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