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- ItemCurrent Advances in TiO2-Based Nanostructure Electrodes for High Performance Lithium Ion Batteries(Basel : MDPI, 2018-2-6) Madian, Mahmoud; Eychmüller, Alexander; Giebeler, LarsThe lithium ion battery (LIB) has proven to be a very reliably used system to store electrical energy, for either mobile or stationary applications. Among others, TiO2-based anodes are the most attractive candidates for building safe and durable lithium ion batteries with high energy density. A variety of TiO2 nanostructures has been thoroughly investigated as anodes in LIBs, e.g., nanoparticles, nanorods, nanoneedles, nanowires, and nanotubes discussed either in their pure form or in composites. In this review, we present the recent developments and breakthroughs demonstrated to synthesize safe, high power, and low cost nanostructured titania-based anodes. The reader is provided with an in-depth review of well-oriented TiO2-based nanotubes fabricated by anodic oxidation. Other strategies for modification of TiO2-based anodes with other elements or materials are also highlighted in this report.
- ItemAuger- 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, SteffenLi-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.
- ItemStructural 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, RubenSubstantial 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.
- ItemLow-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, KarolinaIn 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.
- ItemRetained 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, OlgaDouble 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.
- ItemMicrostructure, 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.
- ItemPolaron-Mediated Luminescence in Lithium Niobate and Lithium Tantalate and Its Domain Contrast(Basel : MDPI, 2018-5-15) Reichenbach, Philipp; Kämpfe, Thomas; Haußmann, Alexander; Thiessen, Andreas; Woike, Theo; Steudtner, Robin; Kocsor, Laura; Szaller, Zsuzsanna; Kovács, László; Eng, Lukas M.In this review article, we discuss photoluminescence phenomena mediated by polarons in lithium niobate (LNO). At first we present the fundamentals on polaron states in LNO and their energy levels, i.e., on free and bound electron polarons, on hole polarons as well as on bipolarons. We discuss the absorption measurements on reduced as well as on doped LNO that made the characterization of the formed polaron states possible by their absorption bands. Next, we proceed by reporting on the two polaron-mediated photoluminescence bands that have been observed in LNO: (1) A near-infrared luminescence band in the range of 1.5 eV shows a mono-exponential decay and a strong dependence on iron doping. This luminescence is emitted by bound polarons returning from an excited state to the ground state. (2) A luminescence band at visible wavelengths with a maximum at 2.6 eV shows a stretched-exponential decay and is strongly enhanced by optical damage resistant doping around the doping threshold. This luminescence stems from the recombination of free electron and hole polarons. The next major topic of this review are domain contrasts of the visible photoluminescence that have been observed after electrical poling of the substrate, as singly inverted domains show a slightly reduced and faster decaying luminescence. Subsequent annealing results in an exponential decrease of that domain contrast. We show that this contrast decay is strongly related to the mobility of lithium ions, thus confirming the role of polar defect complexes, including lithium vacancies, for these domain contrasts. Finally we discuss the extension of our investigations to lithium tantalate (LTO) samples. While the results on the domain contrast and its decay are similar to LNO, there are remarkable differences in their luminescence spectra.
- ItemCore–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.
- ItemAero-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.
- ItemTSFZ Growth of Eu-Substituted Large-Size LSCO Crystals(Basel : MDPI, 2022) Voloshyna, Olesia; Romaka, Vitaliy V.; Karmakar, Koushik ;Seiro, Silvia; Maljuk, Andrey; Büchner, BerndThe travelling solvent floating zone (TSFZ) growth of Eu-substituted LSCO (La1.81−xEuxSr0.19CuO4, with nominal x = 0 ÷ 0.4) single crystals was systematically explored for the first time. The substitution of La with Eu considerably decreased the decomposition temperature. Optimal growth parameters were found to be: oxygen pressure 9.0–9.5 bars; Eu-free CuO-poor solvent (66 mol% CuO) with a molar ratio of La2O3:SrCO3:CuO = 4:4.5:16.5 and growth rate 0.6 mm/hour. The obtained single crystals were characterized with optical polarized microscopy, X-ray diffraction and energy-dispersive X-ray spectroscopy analysis. The solubility of Eu in LSCO appeared to be limited to x~0.36–0.38 under the used conditions. The substitution of La3+ with smaller Eu3+ ions led to a structural transition from tetragonal with space group I4/mmm for La1.81Sr0.19CuO4 (x = 0) to orthorhombic with space group Fmmm for La1.81−xSr0.19EuxCuO4 (x = 0.2, 0.3, 0.4), and to a substantial shrinking of the c-axis from 13.2446 Å (x = 0.0) to 13.1257 Å (x = 0.4). Such structural changes were accompanied by a dramatic decrease in the superconducting critical temperature, Tc, from 29.5 K for x = 0 to 13.8 K for 0.2. For x ≥ 0.3, no superconductivity was detected down to 4 K.