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    Origami-Inspired Shape Memory Folding Microactuator
    (Basel : MDPI, 2020) Seigner, Lena; Bezsmertna, Olha; Fähler, Sebastian; Tshikwand, Georgino; Wendler, Frank; Kohl, Manfred
    This paper presents the design, fabrication and performance of origami-based folding microactuators based on a cold-rolled NiTi foil of 20 µm thickness showing the one-way shape memory effect. Origami refers to a variety of techniques of transforming planar sheets into three-dimensional (3D) structures by folding, which has been introduced in science and engineering for, e.g., assembly and robotics. Here, NiTi microactuators are interconnected to rigid sections (tiles) forming an initial planar system that self-folds into a set of predetermined 3D shapes upon heating. While this concept has been demonstrated at the macro scale, we intend to transfer this concept into microtechnology by combining state-of-the art methods of micromachining. NiTi foils are micromachined by laser cutting or photolithography to achieve double-beam structures allowing for direct Joule heating with an electrical current. A thermo-mechanical treatment is used for shape setting of as-received specimens to reach a maximum folding angle of 180°. The bending moments, bending radii and load-dependent folding angles upon Joule heating are evaluated. The shape setting process is particularly effective for small bending radii, which, however generates residual plastic strain. After shape setting, unloaded beam structures show recoverable bending deflection between 0° and 140° for a maximum heating power of 900 mW. By introducing additional loads to account for the effect of the tiles, the smooth folding characteristic evolves into a sharp transition, whereby full deflection up to 180° is reached. The achieved results are an important step towards the development of cooperative multistable microactuator systems for 3D self-assembly.
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    Directly Anodized Sulfur-Doped TiO2 Nanotubes as Improved Anodes for Li-ion Batteries
    (Basel : MDPI, 2020) Sabaghi, Davood; Madian, Mahmoud; Omar, Ahmad; Oswald, Steffen; Uhlemann, Margitta; Maghrebi, Morteza; Baniadam, Majid; Mikhailova, Daria
    TiO2 represents one of the promising anode materials for lithium ion batteries due to its high thermal and chemical stability, relatively high theoretical specific capacity and low cost. However, the electrochemical performance, particularly for mesoporous TiO2, is limited and must be further developed. Elemental doping is a viable route to enhance rate capability and discharge capacity of TiO2 anodes in Li-ion batteries. Usually, elemental doping requires elevated temperatures, which represents a challenge, particularly for sulfur as a dopant. In this work, S-doped TiO2 nanotubes were successfully synthesized in situ during the electrochemical anodization of a titanium substrate at room temperature. The electrochemical anodization bath represented an ethylene glycol-based solution containing NH4F along with Na2S2O5 as the sulfur source. The S-doped TiO2 anodes demonstrated a higher areal discharge capacity of 95 µAh·cm−2 at a current rate of 100 µA·cm−2 after 100 cycles, as compared to the pure TiO2 nanotubes (60 µAh·cm−2). S-TiO2 also exhibited a significantly improved rate capability up to 2500 µA·cm−2 as compared to undoped TiO2. The improved electrochemical performance, as compared to pure TiO2 nanotubes, is attributed to a lower impedance in S-doped TiO2 nanotubes (STNTs). Thus, the direct S-doping during the anodization process is a promising and cost-effective route towards improved TiO2 anodes for Li-ion batteries.
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    Auger- and X-ray Photoelectron Spectroscopy at Metallic Li Material: Chemical Shifts Related to Sample Preparation, Gas Atmosphere, and Ion and Electron Beam Effects
    (Basel : MDPI, 2022) Oswald, Steffen
    Li-based batteries are a key element in reaching a sustainable energy economy in the near future. The understanding of the very complex electrochemical processes is necessary for the optimization of their performance. X-ray photoelectron spectroscopy (XPS) is an accepted method used to improve understanding around the chemical processes at the electrode surfaces. Nevertheless, its application is limited because the surfaces under investigation are mostly rough and inhomogeneous. Local elemental analysis, such as Auger electron spectroscopy (AES), could assist XPS to gain more insight into the chemical processes at the surfaces. In this paper, some challenges in using electron spectroscopy are discussed, such as binding energy (BE) referencing for the quantitative study of chemical shifts, gas atmospheric influences, or beam damage (including both AE and XP spectroscopy). Carefully prepared and surface-modified metallic lithium material is used as model surface, considering that Li is the key element for most battery applications.
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    Towards Bacteria Counting in DI Water of Several Microliters or Growing Suspension Using Impedance Biochips
    (Basel : MDPI, 2020) Kiani, Mahdi; Tannert, Astrid; Du, Nan; Hübner, Uwe; Skorupa, Ilona; Bürger, Danilo; Zhao, Xianyue; Blaschke, Daniel; Rebohle, Lars; Cherkouk, Charaf; Neugebauer, Ute; Schmidt, Oliver G.; Schmidt, Heidemarie
    We counted bacterial cells of E. coli strain K12 in several-microliter DI water or in several-microliter PBS in the low optical density (OD) range (OD = 0.05–1.08) in contact with the surface of Si-based impedance biochips with ring electrodes by impedance measurements. The multiparameter fit of the impedance data allowed calibration of the impedance data with the concentration cb of the E. coli cells in the range of cb = 0.06 to 1.26 × 109 cells/mL. The results showed that for E. coli in DI water and in PBS, the modelled impedance parameters depend linearly on the concentration of cells in the range of cb = 0.06 to 1.26 × 109 cells/mL, whereas the OD, which was independently measured with a spectrophotometer, was only linearly dependent on the concentration of the E. coli cells in the range of cb = 0.06 to 0.50 × 109 cells/mL.
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    Structural and Electric Properties of Epitaxial Na0.5Bi0.5TiO3-Based Thin Films
    (Basel : MDPI, 2021) Magalhaes, Bruno; Engelhardt, Stefan; Molin, Christian; Gebhardt, Sylvia E.; Nielsch, Kornelius; Hühne, Ruben
    Substantial efforts are dedicated worldwide to use lead-free materials for environmentally friendly processes in electrocaloric cooling. Whereas investigations on bulk materials showed that Na0.5Bi0.5TiO3 (NBT)-based compounds might be suitable for such applications, our aim is to clarify the feasibility of epitaxial NBT-based thin films for more detailed investigations on the correlation between the composition, microstructure, and functional properties. Therefore, NBT-based thin films were grown by pulsed laser deposition on different single crystalline substrates using a thin epitaxial La0.5Sr0.5CoO3 layer as the bottom electrode for subsequent electric measurements. Structural characterization revealed an undisturbed epitaxial growth of NBT on lattice-matching substrates with a columnar microstructure, but high roughness and increasing grain size with larger film thickness. Dielectric measurements indicate a shift of the phase transition to lower temperatures compared to bulk samples as well as a reduced permittivity and increased losses at higher temperatures. Whereas polarization loops taken at −100 °C revealed a distinct ferroelectric behavior, room temperature data showed a significant resistive contribution in these measurements. Leakage current studies confirmed a non-negligible conductivity between the electrodes, thus preventing an indirect characterization of the electrocaloric properties of these films.
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    Low-Temperature Magnetothermodynamics Performance of Tb1-xErxNi2 Laves-Phases Compounds for Designing Composite Refrigerants
    (Basel : MDPI, 2022) Ćwik, Jacek; Koshkid’ko, Yurii; Nenkov, Konstantin; Tereshina-Chitrova, Evgenia; Weise, Bruno; Kowalska, Karolina
    In this paper, the results of heat capacity measurements performed on the polycrystalline Tb1-xErxNi2 intermetallic compounds with x = 0.25, 0.5 and 0.75 are presented. The Debye temperatures and lattice contributions as well as the magnetic part of the heat capacity were determined and analyzed. The heat capacity measurements reveal that the substitution of Tb atoms for Er atoms leads to a linear reduction of the Curie temperatures in the investigated compounds. The ordering temperatures decrease from 28.3 K for Tb0.25Er0.75Ni2 to 12.9 K for Tb0.75Er0.25Ni2. Heat capacity measurements enabled us to calculate with good approximation the isothermal magnetic entropy ΔSmag and adiabatic temperature changes ΔTad for Tb1-xErxNi2, for the magnetic field value equal to 1 T and 2 T. The optimal molar ratios of individual Tb0.75Er0.25Ni2, Tb0.5Er0.5Ni2 and Tb0.25Er0.75Ni2 components in the final composite were theoretically determined. According to the obtained results, the investigated composites make promising candidates that can find their application as an active body in a magnetic refrigerator performing an Ericsson cycle at low temperatures. Moreover, for the Tb0.5Er0.5Ni2 compound, direct measurements of adiabatic temperature change in the vicinity of the Curie temperature in the magnetic field up to 14 T were performed. The obtained high-field results are compared to the data for the parent TbNi2 and ErNi2 compounds, and their magnetocaloric properties near the Curie temperature are analyzed in the framework of the Landau theory for the second-order phase transitions.
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    Retained Free Energy with Enhanced Nucleation during Electrostatic Levitation of Undercooled Fe-Co Alloys
    (Basel : MDPI, 2021) Matson, Douglas M.; Liu, Xuanjiang; Rodriguez, Justin E.; Jeon, Sangho; Shuleshova, Olga
    Double recalescence in many ferrous alloy systems involves rapid solidification of metastable ferrite from the undercooled melt with subsequent transformation to stable austenite. Containerless processing is used to monitor the process using pyrometry and high-speed cinematography such that delay behavior can be predicted based on the application of the retained damage model (RDM). When comparing Fe-Cr-Ni alloys to Fe-Co alloys, the cluster attachment rate is enhanced while free energy retention is reduced. These trends are tied to specific alloy properties. A retained free energy criterion is proposed based on the ratio of thermophysical properties used to define the transformation driving force such that the thermodynamic limit for energy retention may be predicted. Surprisingly, at long delay times, healing occurs such that much of the retained free energy is not available to enhance the transition from metastable to stable phases. At delay times less than one second, no healing is observed and the RDM correctly predicts transformation delay behavior over a wide range of alloy compositions.
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    Microstructure, Texture, and Strength Development during High-Pressure Torsion of CrMnFeCoNi High-Entropy Alloy
    (Basel : MDPI, 2020) Skrotzki, Werner; Pukenas, Aurimas; Odor, Eva; Joni, Bertalan; Ungar, Tamas; Völker, Bernhard; Hohenwarter, Anton; Pippan, Reinhard; George, Easo P.
    The equiatomic face-centered cubic high-entropy alloy CrMnFeCoNi was severely deformed at room and liquid nitrogen temperature by high-pressure torsion up to shear strains of about 170. Itsmicrostructurewas analyzed by X-ray line profile analysis and transmission electronmicroscopy and its texture by X-ray microdiffraction. Microhardness measurements, after severe plastic deformation, were done at room temperature. It is shown that at a shear strain of about 20, a steady state grain size of 24 nm, and a dislocation density of the order of 1016 m-2 is reached. The dislocations are mainly screw-type with low dipole character. Mechanical twinning at room temperature is replaced by a martensitic phase transformation at 77 K. The texture developed at room temperature is typical for sheared face-centered cubic nanocrystalline metals, but it is extremely weak and becomes almost random after high-pressure torsion at 77 K. The strength of the nanocrystalline material produced by high-pressure torsion at 77 K is lower than that produced at room temperature. The results are discussed in terms of different mechanisms of deformation, including dislocation generation and propagation, twinning, grain boundary sliding, and phase transformation. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.
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    Core–Shell Structures Prepared by Atomic Layer Deposition on GaAs Nanowires
    (Basel : MDPI, 2022) Ursaki, Veaceslav V.; Lehmann, Sebastian; Zalamai, Victor V.; Morari, Vadim; Nielsch, Kornelius; Tiginyanu, Ion M.; Monaico, Eduard V.
    GaAs nanowire arrays have been prepared by anodization of GaAs substrates. The nanowires produced on (111)B GaAs substrates were found to be oriented predominantly perpendicular to the substrate surface. The prepared nanowire arrays have been coated with thin ZnO or TiO2 layers by means of thermal atomic layer deposition (ALD), thus coaxial core–shell hybrid structures are being fabricated. The hybrid structures have been characterized by scanning electron microscopy (SEM) for the morphology investigations, by Energy Dispersive X-ray (EDX) and X-ray diffraction (XRD) analysis for the composition and crystal structure assessment, and by photoluminescence (PL) spectroscopy for obtaining an insight on emission polarization related to different recombination channels in the prepared core–shell structures.
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    Aero-TiO2 Prepared on the Basis of Networks of ZnO Tetrapods
    (Basel : MDPI, 2022) Ciobanu, Vladimir; Ursaki, Veaceslav V.; Lehmann, Sebastian; Braniste, Tudor; Raevschi, Simion; Zalamai, Victor V.; Monaico, Eduard V.; Colpo, Pascal; Nielsch, Kornelius; Tiginyanu, Ion M.
    In this paper, new aeromaterials are proposed on the basis of titania thin films deposited using atomic layer deposition (ALD) on a sacrificial network of ZnO microtetrapods. The technology consists of two technological steps applied after ALD, namely, thermal treatment at different temperatures and etching of the sacrificial template. Two procedures are applied for etching, one of which is wet etching in a citric acid aqua solution, while the other one is etching in a hydride vapor phase epitaxy (HVPE) system with HCl and hydrogen chemicals. The morphology, composition, and crystal structure of the produced aeromaterials are investigated depending on the temperature of annealing and the sequence of the technological steps. The performed photoluminescence analysis suggests that the developed aeromaterials are potential candidates for photocatalytic applications.