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Synthesis and crystal structure of a one-dimensional chain-like strontium(II) coordination polymer built of N-methyldiethanolamine and isobutyrate ligands
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.
Plasma-assisted synthesis and high-resolution characterization of anisotropic elemental and bimetallic core-shell magnetic nanoparticles
2014, Hennes, M., Lotnyk, A., Mayr, S.G.
Magnetically anisotropic as well as magnetic core-shell nanoparticles (CS-NPs) with controllable properties are highly desirable in a broad range of applications. With this background, a setup for the synthesis of heterostructured magnetic core-shell nanoparticles, which relies on (optionally pulsed) DC plasma gas condensation has been developed. We demonstrate the synthesis of elemental nickel nanoparticles with highly tunable sizes and shapes and Ni@Cu CS-NPs with an average shell thickness of 10 nm as determined with scanning electron microscopy, high-resolution transmission electron microscopy and energy-dispersive X-ray spectroscopy measurements. An analytical model that relies on classical kinetic gas theory is used to describe the deposition of Cu shell atoms on top of existing Ni cores. Its predictive power and possible implications for the growth of heterostructured NP in gas condensation processes are discussed.
Cryo-printed microfluidics enable rapid prototyping for optical-cell analysis
2022, Garmasukis, Rokas, Hackl, Claudia, Dusny, Christian, Elsner, Christian, Charvat, Ales, Schmid, Andreas, Abel, Bernd
This 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.
Improvement of the optical properties after surface error correction of aluminium mirror surfaces
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.
Strong out-of-plane magnetic anisotropy in ion irradiated anatase TiO2 thin films
2016, Stiller, M., Barzola-Quiquia, J., Esquinazi, P., Spemann, D., Meijer, J., Lorenz, M., Grundmann, M.
The temperature and field dependence of the magnetization of epitaxial, undoped anatase TiO2 thin films on SrTiO3 substrates was investigated. Low-energy ion irradiation was used to modify the surface of the films within a few nanometers, yet with high enough energy to produce oxygen and titanium vacancies. The as-prepared thin film shows ferromagnetism which increases after irradiation with low-energy ions. An optimal and clear magnetic anisotropy was observed after the first irradiation, opposite to the expected form anisotropy. Taking into account the experimental parameters, titanium vacancies as di-Frenkel pairs appear to be responsible for the enhanced ferromagnetism and the strong anisotropy observed in our films. The magnetic impurities concentrations was measured by particle-induced X-ray emission with ppm resolution. They are ruled out as a source of the observed ferromagnetism before and after irradiation.
Topography evolution of germanium thin films synthesized by pulsed laser deposition
2017, Schumacher, P., Mayr, S.G., Rauschenbach, B.
Germanium thin films were deposited by Pulsed Laser Deposition (PLD) onto single crystal Ge (100) and Si (100) substrates with a native oxide film on the surface. The topography of the surface was investigated by Atomic Force Microscopy (AFM) to evaluate the scaling behavior of the surface roughness of amorphous and polycrystalline Ge films grown on substrates with different roughnesses. Roughness evolution was interpreted within the framework of stochastic rate equations for thin film growth. Here the Kardar-Parisi-Zhang equation was used to describe the smoothening process. Additionally, a roughening regime was observed in which 3-dimensional growth occurred. Diffusion of the deposited Ge adatoms controlled the growth of the amorphous Ge thin films. The growth of polycrystalline thin Ge films was dominated by diffusion processes only in the initial stage of the growth.
Heterobimetallic conducting polymers based on salophen complexes via electrosynthesis
2023, Bia, Francesca, Gualandi, Isacco, Griebel, Jan, Rasmussen, Leon, Hallak, Bassam, Tonelli, Domenica, Kersting, Berthold
In 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.
Nanometer-resolved mechanical properties around GaN crystal surface steps
2014, Buchwald, J., Sarmanova, M., Rauschenbach, B., Mayr, S.G.
The mechanical properties of surfaces and nanostructures deviate from their bulk counterparts due to surface stress and reduced dimensionality. Experimental indentation-based techniques present the challenge of measuring these effects, while avoiding artifacts caused by the measurement technique itself. We performed a molecular dynamics study to investigate the mechanical properties of a GaN step of only a few lattice constants step height and scrutinized its applicability to indentation experiments using a finite element approach (FEM). We show that the breakdown of half-space symmetry leads to an "artificial" reduction of the elastic properties of comparable lateral dimensions which overlays the effect of surface stress. Contact resonance atomic force microscopy (CR-AFM) was used to compare the simulation results with experiments.
Developing a Laser Induced Liquid Beam Ion Desorption Spectral Database as Reference for Spaceborne Mass Spectrometers
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, Frank
Spaceborne 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).
Characteristics of diamond turned NiP smoothed with ion beam planarization technique
2017, Li, Yaguo, Takino, Hideo, Frost, Frank
Background: Diamond turning is widely used in machining metals and semiconductors but the turning marks are incurred on machined components due to the mechanics of the technology. The marks are generally harmful to the systems comprising of the machined components. Therefore, the capability of ion beam planarization (IBP) to reduce turning marks of diamond turned metal surfaces was investigated using NiP as an example. Methods: The turning marks and thereby roughness was reduced by IBP with respect to different spatial wavelengths and amplitudes of turning marks. Different thickness of coating resist was also examined in order to find out the potential effects of resist thickness on the reduction of turning marks and roughness. Additionally, the effect of multiple planarization steps was also analyzed. Results: The spatial wavelength and depth of turning marks have only minor impact on the degree of surface roughness reduction. Thicker coating tends to achieve smoother surface after coating turned NiP while ion beam etching can keep surface roughness almost unchanged in our experiments. The surface roughness of diamond turned NiP drops exponentially with processing steps under experimented conditions. Using up to five IBP steps, the surface roughness can be reduced up to one order of magnitude (from Rq ~ 6.5 nm to Rq ~ 0.7 nm). Conclusions: IBP technique performs very well in reducing turning marks on diamond turned NiP surfaces. The surface roughness can be further improved by optimizing the properties of planarizing resist layer and coating processes to enhance the IBP technique as a final surface finishing technology.