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- ItemRevealing all states of dewetting of a thin gold layer on a silicon surface by nanosecond laser conditioning(Amsterdam : Elsevier, 2021) Ernst, Owen C.; Uebel, David; Kayser, Stefan; Lange, Felix; Teubner, Thomas; Boeck, TorstenDewetting is a ubiquitous phenomenon which can be applied to the laser synthesis of nanoparticles. A classical spinodal dewetting process takes place in four successive states, which differ from each other in their morphology. In this study all states are revealed by interaction of pulsed nanosecond UV laser light with thin gold layers with thicknesses between 1 nm and 10 nm on (100) silicon wafers. The specific morphologies of the dewetting states are discussed with particular emphasis on the state boundaries. The main parameter determining which state is formed is not the duration for which the gold remains liquid, but rather the input energy provided by the laser. This shows that each state transition has a separate measurable activation energy. The temperature during the nanosecond pulses and the duration during which the gold remains liquid was determined by simulation using the COMSOL Multiphysics® software package. Using these calculations, an accurate local temperature profile and its development over time was simulated. An analytical study of the morphologies and formed structures was performed using Minkowski measures. With aid of this tool, the laser induced structures were compared with thermally annealed samples, with perfectly ordered structures and with perfectly random structures. The results show that both, structures of the laser induced and the annealed samples, strongly resemble the perfectly ordered structures. This reveals a close relationship between these structures and suggests that the phenomenon under investigation is indeed a spinodal dewetting generated by an internal material wave function. The purposeful generation of these structures and the elucidation of the underlying mechanism of dewetting by short pulse lasers may assist the realisation of various technical elements such as nanowires in science and industry. © 2020
- ItemNumerical Modeling of Heat Transfer and Thermal Stress at the Czochralski Growth of Neodymium Scandate Single Crystals(Weinheim : Wiley-VCH, 2021) Böttcher, Klaus; Miller, Wolfram; Ganschow, SteffenThe Czochralski growth of NdScO3 single crystals along the [110]-direction is numerically analyzed with the focus on the influence of the optical thickness on the shape of the crystal–melt interface and on the generation of thermal stresses. Due to lack of data, the optical thickness (i.e., the absorption coefficient) is varied over the entire interval between optically thin and thick. While the thermal calculation in the entire furnace is treated as axisymmetric, the stress calculation of the crystal is done three-dimensionally in order to meet the spatial anisotropy of thermal expansion and elastic coefficients. The numerically obtained values of the deflection of the crystal/melt interface meet the experimental ones for absorption coefficients in the range between 40 and 200 m−1. The maximum values of the von Mises stress appear for the case of absorption coefficient between 20 and 40 m−1. Applying absorption coefficients in the range between 3 and 100 m−1 leads to local peaks of high temperature in the shoulder region and the tail region near the end of the cylindrical part.
- ItemReal Time Predictions of VGF-GaAs Growth Dynamics by LSTM Neural Networks(Basel : MDPI, 2021) Dropka, Natasha; Ecklebe, Stefan; Holena, MartinThe aim of this study was to assess the aptitude of the recurrent Long Short-Term Memory (LSTM) neural networks for fast and accurate predictions of process dynamics in vertical-gradient-freeze growth of gallium arsenide crystals (VGF-GaAs) using datasets generated by numerical transient simulations. Real time predictions of the temperatures and solid–liquid interface position in GaAs are crucial for control applications and for process visualization, i.e., for generation of digital twins. In the reported study, an LSTM network was trained on 1950 datasets with 2 external inputs and 6 outputs. Based on network performance criteria and training results, LSTMs showed the very accurate predictions of the VGF-GaAs growth process with median root-mean-square-error (RMSE) values of 2 × 10−3. This deep learning method achieved a superior predictive accuracy and timeliness compared with more traditional Nonlinear AutoRegressive eXogenous (NARX) recurrent networks.
- ItemCorrelation of Electrical Properties and Acoustic Loss in Single Crystalline Lithium Niobate-Tantalate Solid Solutions at Elevated Temperatures(2021) Suhak, Yuriy; Roshchupkin, Dmitry; Redkin, Boris; Kabir, Ahsanul; Jerliu, Bujar; Ganschow, Steffen; Fritze, HolgerElectrical conductivity and acoustic loss Q−1 of single crystalline Li(Nb,Ta)O3 solid solutions (LNT) are studied as a function of temperature by means of impedance spectroscopy and resonant piezoelectric spectroscopy, respectively. For this purpose, bulk acoustic wave resonators with two different Nb/Ta ratios are investigated. The obtained results are compared to those previously reported for congruent LiNbO3. The temperature dependent electrical conductivity of LNT and LiNbO3 show similar behavior in air at high temperatures from 400 to 700 °C. Therefore, it is concluded that the dominant transport mechanism in LNT is the same as in LN, which is the Li transport via Li vacancies. Further, it is shown that losses in LNT strongly increase above about 500 °C, which is interpreted to originate from conductivity-related relaxation mechanism. Finally, it is shown that LNT bulk acoustic resonators exhibit significantly lower loss, comparing to that of LiNbO3.
- ItemCrystal growth and thermodynamic investigation of Bi2M2+O4 (M = Pd, Cu)(London : RSC, 2021) Wolff, Nora; Klimm, Detlef; Habicht, Klaus; Fritsch, KatharinaPhase equilibria that are relevant for the growth of Bi2MO4 have been studied experimentally, and the ternary phase diagrams of Bi2O3–PdO2–Pd and Bi2O3–Cu2O–CuO and its isopleth section Bi2O3–CuO were redetermined. It is shown that every melting and crystallization process is always accompanied by a redox process at the phase boundary and that for both title compounds, the valence of the transition metal is lowered during melting. Vice versa, during crystal growth, O2 must be transported through the melt to the phase boundary. Based on these new insights provided by our thermodynamic studies, Bi2CuO4 single crystals with a length of up to 7 cm and a diameter of 6 mm were grown by the OFZ technique to be used for investigations of magnetic, electronic and thermal transport properties. The grown crystals were characterized by powder X-ray diffraction, Laue, magnetization and specific heat measurements.
- ItemIs Reduced Strontium Titanate a Semiconductor or a Metal?(Basel : MDPI, 2021) Rodenbücher, Christian; Guguschev, Christo; Korte, Carsten; Bette, Sebastian; Szot, KristofIn recent decades, the behavior of SrTiO3 upon annealing in reducing conditions has been under intense academic scrutiny. Classically, its conductivity can be described using point defect chemistry and predicting n-type or p-type semiconducting behavior depending on oxygen activity. In contrast, many examples of metallic behavior induced by thermal reduction have recently appeared in the literature, challenging this established understanding. In this study, we aim to resolve this contradiction by demonstrating that an initially insulating, as-received SrTiO3 single crystal can indeed be reduced to a metallic state, and is even stable against room temperature reoxidation. However, once the sample has been oxidized at a high temperature, subsequent reduction can no longer be used to induce metallic behavior, but semiconducting behavior in agreement with the predictions of point defect chemistry is observed. Our results indicate that the dislocation-rich surface layer plays a decisive role and that its local chemical composition can be changed depending on annealing conditions. This reveals that the prediction of the macroscopic electronic properties of SrTiO3 is a highly complex task, and not only the current temperature and oxygen activity but also the redox history play an important role.
- ItemA new concept for temporal gating of synchrotron X-ray pulses(Chester : IUCr, 2021) Schmidt, D.; Bauer, R.; Chung, S.; Novikov, D.; Sander, M.; Pudell, J.E.; Herzog, M.; Pfuetzenreuter, D.; Schwarzkopf, J.; Chernikov, R.; Gaal, P.A new concept for temporal gating of synchrotron X-ray pulses based on laser-induced thermal transient gratings is presented. First experimental tests of the concept yield a diffraction efficiency of 0.18%; however, the calculations indicate a theoretical efficiency and contrast of >30% and 10−5, respectively. The full efficiency of the pulse picker has not been reached yet due to a long-range thermal deformation of the sample after absorption of the excitation laser. This method can be implemented in a broad spectral range (100 eV to 20 keV) and is only minimally invasive to an existing setup.
- ItemInvestigating the electrochemical stability of Li7La3Zr2O12 solid electrolytes using field stress experiments(London [u.a.] : RSC, 2021) Smetaczek, Stefan; Pycha, Eva; Ring, Joseph; Siebenhofer, Matthäus; Ganschow, Steffen; Berendts, Stefan; Nenning, Andreas; Kubicek, Markus; Rettenwander, Daniel; Limbeck, Andreas; Fleig, JürgenCubic Li7La3Zr2O12 (LLZO) garnets are among the most promising solid electrolytes for solid-state batteries with the potential to exceed conventional battery concepts in terms of energy density and safety. The electrochemical stability of LLZO is crucial for its application, however, controversial reports in the literature show that it is still an unsettled matter. Here, we investigate the electrochemical stability of LLZO single crystals by applying electric field stress via macro- and microscopic ionically blocking Au electrodes in ambient air. Induced material changes are subsequently probed using various locally resolved analysis techniques, including microelectrode electrochemical impedance spectroscopy (EIS), laser induced breakdown spectroscopy (LIBS), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), and microfocus X-ray diffraction (XRD). Our experiments indicate that LLZO decomposes at 4.1–4.3 V vs. Li+/Li, leading to the formation of Li-poor phases like La2Zr2O7 beneath the positively polarized electrode. The reaction is still on-going even after several days of polarization, indicating that no blocking interfacial layer is formed. The decomposition can be observed at elevated as well as room temperature and suggests that LLZO is truly not compatible with high voltage cathode materials.
- ItemPerformance of fully instrumented detector planes of the forward calorimeter of a Linear Collider detector(London : Inst. of Physics, 2015) Abramowicz, H.; Abusleme, A.; Afanaciev, K.; Aguilar, J.; Alvarez, E.; Avila, D.; Benhammou, Y.; Bortko, L.; Borysov, O.; Bergholz, M.; Bozovic-Jelisavcic, I.; Castro, E.; Chelkov, G.; Coca, C.; Daniluk, W.; Dumitru, L.; Elsener, K.; Fadeyev, V.; Firlej, M.; Firu, E.; Fiutowski, T.; Ghenescu, V.; Gostkin, M.; Henschel, H.; Idzik, M.; Ishikawa, A.; Kananov, S.; Kollowa, S.; Kotov, S.; Kotula, J.; Kozhevnikov, D.; Kruchonok, V.; Krupa, B.; Kulis, Sz.; Lange, W.; Lesiak, T.; Levy, A.; Levy, I.; Lohmann, W.; Lukic, S.; Milke, C.; Moron, J.; Moszczynski, A.; Neagu, A.T.; Novgorodova, O.; Oliwa, K.; Orlandea, M.; Pandurovic, M.; Pawlik, B.; Preda, T.; Przyborowski, D.; Rosenblat, O.; Sailer, A.; Sato, Y.; Schumm, B.; Schuwalow, S.; Smiljanic, I.; Smolyanskiy, P.; Swientek, K.; Teodorescu, E.; Terlecki, P.; Wierba, W.; Wojton, T.; Yamaguchi, S.; Yamamoto, H.; Zawiejski, L.; Zgura, I.S.; Zhemchugov, A.Detector-plane prototypes of the very forward calorimetry of a future detector at an e+e− collider have been built and their performance was measured in an electron beam. The detector plane comprises silicon or GaAs pad sensors, dedicated front-end and ADC ASICs, and an FPGA for data concentration. Measurements of the signal-to-noise ratio and the response as a function of the position of the sensor are presented. A deconvolution method is successfully applied, and a comparison of the measured shower shape as a function of the absorber depth with a Monte-Carlo simulation is given.
- ItemSample chamber for synchrotron based in-situ X-ray diffraction experiments under electric fields and temperatures between 100 K and 1250 K(Chester : IUCr, 2021) Nentwich, Melanie; Weigel, Tina; Richter, Carsten; Stöcker, Hartmut; Mehner, Erik; Jachalke, Sven; Novikov, Dmitri V.; Zschornak, Matthias; Meyer, Dirk C.Many scientific questions require X-ray experiments conducted at varying temperatures, sometimes combined with the application of electric fields. Here, a customized sample chamber developed for beamlines P23 and P24 of PETRA III at DESY to suit these demands is presented. The chamber body consists mainly of standard vacuum parts housing the heater/cooler assembly supplying a temperature range of 100 K to 1250 K and an xyz manipulator holding an electric contact needle for electric measurements at both high voltage and low current. The chamber is closed by an exchangeable hemispherical dome offering all degrees of freedom for single-crystal experiments within one hemisphere of solid angle. The currently available dome materials (PC, PS, PEEK polymers) differ in their absorption and scattering characteristics, with PEEK providing the best overall performance. The article further describes heating and cooling capabilities, electric characteristics, and plans for future upgrades of the chamber. Examples of applications are discussed.