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- ItemSynthesis and crystal structure of a one-dimensional chain-like strontium(II) coordination polymer built of N-methyldiethanolamine and isobutyrate ligands(Chester : International Union of Crystallography, 2021) Seiss, Maximilian; Schmitz, Sebastian; Börner, Martin; Monakhov, Kirill Yu.The one-dimensional coordination polymer (I) [Sr(ib)2 (H2mda)]n (Hib = isobutyric acid, C4H8O2, and H2mda = N-methyldiethanolamine, C5H13NO2), namely, catena-poly[[(N-methyldiethanolamine-k3O, N, O')strontium(II)]-di-μ2- isobutyrato-K3O, O':O;K3O:O, O'], was prepared by the one-pot aerobic reaction of [Zr6O4 (OH)4 (ib)12 (H2O)].3Hib with Sr(NO3)2 and H2mda in the presence of MnCl2 and Et3N in acetonitrile. The use of MnCl2 is key to the isolation of I as high-quality colorless crystals in good yield. The molecular solid-state structure of I was determined by single-crystal X-ray diffraction. Compound I crystallizes in the monoclinic space group P21/c and shows a one-dimensional polymeric chain structure. Each monomeric unit of this coordination polymer consists of a central SrII ion in the NO8 coordination environment of two deprotonated ib- ligands and one fully protonated H2mda ligand. The C and O atoms of the H2mda ligand were refined as disordered over two sets of sites with site occupancies of 0.619 (3) and 0.381 (3). Compound I shows thermal stability up to 130°C in air. © 2021 International Union of Crystallography. All rights reserved.
- ItemDeveloping a Laser Induced Liquid Beam Ion Desorption Spectral Database as Reference for Spaceborne Mass Spectrometers(Malden, Mass. : American Geophysical Union, 2022) Klenner, Fabian; Umair, Muhammad; Walter, Sebastian H. G.; Khawaja, Nozair; Hillier, Jon; Nölle, Lenz; Zou, Zenghui; Napoleoni, Maryse; Sanderink, Arnaud; Zuschneid, Wilhelm; Abel, Bernd; Postberg, FrankSpaceborne impact ionization mass spectrometers, such as the Cosmic Dust Analyzer on board the past Cassini spacecraft or the SUrface Dust Analyzer being built for NASA's upcoming Europa Clipper mission, are of crucial importance for the exploration of icy moons in the Solar System, such as Saturn's moon Enceladus or Jupiter's moon Europa. For the interpretation of data produced by these instruments, analogue experiments on Earth are essential. To date, thousands of laboratory mass spectra have been recorded with an analogue experiment for impact ionization mass spectrometers. Simulation of mass spectra of ice grains in space is achieved by a Laser Induced Liquid Beam Ion Desorption (LILBID) approach. The desorbed cations or anions are analyzed in a time-of-flight mass spectrometer. The amount of unstructured raw data is increasingly challenging to sort, process, interpret and compare with data from space. Thus far this has been achieved manually for individual mass spectra because no database containing the recorded reference spectra was available. Here we describe the development of a comprehensive, extendable database containing cation and anion mass spectra from the laboratory LILBID facility. The database is based on a Relational Database Management System with a web server interface and enables filtering of the laboratory data using a wide range of parameters. The mass spectra can be compared not only with data from past and future space missions but also mass spectral data generated by other, terrestrial, techniques. The validated and approved subset of the database is available for general public (https://lilbid-db.planet.fu-berlin.de).
- ItemCryo-printed microfluidics enable rapid prototyping for optical-cell analysis(Heidelberg : Springer, 2022) Garmasukis, Rokas; Hackl, Claudia; Dusny, Christian; Elsner, Christian; Charvat, Ales; Schmid, Andreas; Abel, BerndThis paper highlights an innovative, low-cost rapid-prototyping method for generating microfluidic chips with extraordinary short fabrication times of only a few minutes. Microchannels and inlet/outlet ports are created by controlled deposition of aqueous microdroplets on a cooled surface resulting in printed ice microstructures, which are in turn coated with a UV-curable acrylic cover layer. Thawing leaves an inverse imprint as a microchannel structure. For an exemplary case, we applied this technology for creating a microfluidic chip for cell-customized optical-cell analysis. The chip design includes containers for cell cultivation and analysis. Container shape, length, position, and angle relative to the main channel were iteratively optimized to cultivate and analyze different cell types. With the chip, we performed physiological analyses of morphologically distinct prokaryotic Corynebacterium glutamicum DM1919, eukaryotic Hansenula polymorpha RB11 MOX-GFP, and phototrophic Synechocystis sp. PCC 6803 cells via quantitative time-lapse fluorescence microscopy. The technology is not limited to rapid prototyping of complex biocompatible microfluidics. Further exploration may include printing with different materials other than water, printing on other substrates in-situ biofunctionalization, the inclusion of electrodes and many other applications.
- ItemHeterobimetallic conducting polymers based on salophen complexes via electrosynthesis(London [u.a.] : RSC, 2023) Bia, Francesca; Gualandi, Isacco; Griebel, Jan; Rasmussen, Leon; Hallak, Bassam; Tonelli, Domenica; Kersting, BertholdIn this work, we report the first electrochemical synthesis of two copolymeric bimetallic conducting polymers by a simple anodic electropolymerization method. The adopted precursors are electroactive transition metal (M = Ni, Cu and Fe) salophen complexes, which can be easily obtained by direct chemical synthesis. The resulting films, labeled poly-NiCu and poly-CuFe, were characterized by cyclic voltammetry in both organic and aqueous media, attenuated total reflectance Fourier transform infrared spectroscopy, UV-vis spectroscopy, scanning electron microscopy, and coupled energy dispersive X-ray spectroscopy. The films are conductive and exhibit great electrochemical stability in both organic and aqueous media (resistant over 100 cycles without significant loss in current response or changes in electrochemical behavior), which makes them good candidates for an array of potential applications. Electrochemical detection of ascorbic acid was performed using both materials.
- ItemImprovement of the optical properties after surface error correction of aluminium mirror surfaces(London : Biomed Central, 2021) Ulitschka, M.; Bauer, J.; Frost, F.; Arnold, T.Ion beam finishing techniques of aluminium mirrors have a high potential to meet the increasing demands on applications of high-performance mirror devices for visible and ultraviolet spectral range. Reactively driven ion beam machining using oxygen and nitrogen gases enables the direct figure error correction up to 1 μm machining depth while preserving the initial roughness. However, the periodic turning mark structures, which result from preliminary device shaping by single-point diamond turning, often limit the applicability of mirror surfaces in the short-periodic spectral range. Ion beam planarization with the aid of a sacrificial layer is a promising process route for surface smoothing, resulting in successfully reduction of the turning mark structures. A combination with direct surface smoothing to perform a subsequent improvement of the microroughness is presented with a special focus on roughness evolution, chemical composition, and optical surface properties. As a result, an ion beam based process route is suggested, which allows almost to recover the reflective properties and an increased long-term stability of smoothed aluminium surfaces.
- ItemTarget ion and neutral spread in high power impulse magnetron sputtering(New York, NY : Inst., 2022) Hajihoseini, H.; Brenning, N.; Rudolph, M.; Raadu, M.A.; Lundin, D.; Fischer, J.; Minea, T. M.; Gudmundsson, J.T.In magnetron sputtering, only a fraction of the sputtered target material leaving the ionization region is directed toward the substrate. This fraction may be different for ions and neutrals of the target material as the neutrals and ions can exhibit a different spread as they travel from the target surface toward the substrate. This difference can be significant in high power impulse magnetron sputtering (HiPIMS) where a substantial fraction of the sputtered material is known to be ionized. Geometrical factors or transport parameters that account for the loss of produced film-forming species to the chamber walls are needed for experimental characterization and modeling of the magnetron sputtering discharge. Here, we experimentally determine transport parameters for ions and neutral atoms in a HiPIMS discharge with a titanium target for various magnet configurations. Transport parameters are determined to a typical substrate, with the same diameter (100 mm) as the cathode target, and located at a distance 70 mm from the target surface. As the magnet configuration and/or the discharge current are changed, the transport parameter for neutral atoms ζ tn remains roughly the same, while transport parameters for ions ζ ti vary greatly. Furthermore, the relative ion-to-neutral transport factors, ζ ti / ζ tn, that describe the relative deposited fractions of target material ions and neutrals onto the substrate, are determined to be in the range from 0.4 to 1.1.
- ItemWeak electron irradiation suppresses the anomalous magnetization of N-doped diamond crystals(Weinheim : Wiley-VCH, 2021) Setzer, Annette; Esquinazi, Pablo D.; Daikos, Olesya; Scherzer, Tom; Pöppl, Andreas; Staacke, Robert; Lühmann, Tobias; Pezzagna, Sebastien; Knolle, Wolfgang; Buga, Sergei; Abel, Bernd; Meijer, JanSeveral diamond bulk crystals with a concentration of electrically neutral single substitutional nitrogen atoms of ≲80 ppm, the so-called C or P1 centers, are irradiated with electrons at 10 MeV energy and low fluence. The results show a complete suppression of the irreversible behavior in field and temperature of the magnetization below 30 K, after a decrease in ≲40 ppm in the concentration of C centers produced by the electron irradiation. This result indicates that magnetic C centers are at the origin of the large hysteretic behavior found recently in nitrogen-doped diamond crystals. This is remarkable because of the relatively low density of C centers, stressing the extraordinary role of the C centers in triggering those phenomena in diamond at relatively high temperatures. After annealing the samples at high temperatures in vacuum, the hysteretic behavior is partially recovered.
- ItemDefect-Induced Magnetism in Nonmagnetic Oxides: Basic Principles, Experimental Evidence, and Possible Devices with ZnO and TiO2(Weinheim : Wiley-VCH, 2020) Esquinazi, Pablo David; Hergert, Wolfram; Stiller, Markus; Botsch, Lukas; Ohldag, Hendrik; Spemann, Daniel; Hoffmann, Martin; Adeagbo, Waheed A.; Chassé, Angelika; Nayak, Sanjeev K.; Ben Hamed, HichemThe magnetic moment and the magnetic order induced by localized defects, like vacancies, interstitials, and/or nonmagnetic (NM) ions, in a NM oxide atomic lattice are discussed. When the defect concentration is of the order of or larger than ≈3 at%, magnetic order at room temperature can appear. Herein, the theoretical basic principles needed to understand and compute this new magnetic phenomenon in solids are developed in detail. In particular, the main results of density functional theory (DFT) calculations are used to estimate the magnetization and X-ray magnetic circular dichroism (XMCD) values. The main experimental evidences on this phenomenon are reviewed, especially magnetization, the element-specific XMCD, and transport properties in two selected oxides, ZnO and TiO2. Emphasis is given on the simplicity and efficiency ion irradiation methods have to trigger magnetic order in these oxides as well as a very sensitive method to characterize magnetic impurities. Two possible applications of this phenomenon are discussed, namely spin filtering at magnetic/NM interfaces in ZnO and perpendicular magnetic anisotropy triggered in TiO2 anatase microstructures. The existing literature on defect-induced magnetism in oxides is shortly reviewed, which provides further evidence on the robustness of this phenomenon in solids.
- ItemMolecular Beam Epitaxy Growth and Characterization of Germanium-Doped Cubic AlxGa1−xN(Weinheim : Wiley-VCH, 2020) Deppe, Michael; Henksmeier, Tobias; Gerlach, Jürgen W.; Reuter, Dirk; As, Donat J.In cubic (c-)GaN Ge has emerged as a promising alternative to Si for n-type doping, offering the advantage of slightly improved electrical properties. Herein, a study on Ge doping of the ternary alloy c-AlxGa1−xN is presented. Ge-doped c-AlxGa1−xN layers are grown by plasma-assisted molecular beam epitaxy. In two sample series, both the Al mole fraction x and the doping level are varied. The incorporation of Ge is verified by time-of-flight secondary ion mass spectrometry. Ge incorporation and donor concentrations rise exponentially with increasing Ge cell temperature. A maximum donor concentration of 1.4 × 1020 cm−3 is achieved. While the incorporation of Ge is almost independent of x, incorporation of O, which acts as an unintentional donor, increases for higher x. Dislocation densities start increasing when doping levels of around 3 × 1019 cm−3 are exceeded. Also photoluminescence intensities begin to drop at these high doping levels. Optical emission of layers with x > 0.25 is found to originate from a defect level 0.9 eV below the indirect bandgap, which is not related to Ge. In the investigated range 0 ≤ x ≤ 0.6, Ge is a suitable donor in c-AlxGa1−xN up to the low 1019 cm−3 range.
- ItemMagnetic measurement methods to probe nanoparticle–matrix interactions(Berlin : de Gruyter, 2021) Liebl, Maik; Eberbeck, Dietmar; Coene, Annelies; Leliaert, Jonathan; Jauch, Philine; Kruteva, Margarita; Fruhner, Lisa; Barnsley, Lester; Mayr, Stefan G.; Wiekhorst, FrankMagnetic nanoparticles (MNPs) are key elements in several biomedical applications, e.g., in cancer therapy. Here, the MNPs are remotely manipulated by magnetic fields from outside the body to deliver drugs or generate heat in tumor tissue. The efficiency and success of these approaches strongly depend on the spatial distribution and quantity of MNPs inside a body and interactions of the particles with the biological matrix. These include dynamic processes of the MNPs in the organism such as binding kinetics, cellular uptake, passage through cell barriers, heat induction and flow. While magnetic measurement methods have been applied so far to resolve the location and quantity of MNPs for therapy monitoring, these methods can be advanced to additionally access these particle–matrix interactions. By this, the MNPs can further be utilized as probes for the physical properties of their molecular environment. In this review, we first investigate the impact of nanoparticle–matrix interactions on magnetic measurements in selected experiments. With these results, we then advanced the imaging modalities magnetorelaxometry imaging and magnetic microsphere tracking to spatially resolve particle–matrix interactions.