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- ItemHow to grow single-crystalline and epitaxial NiTi films in (100)- and (111)-orientation(Bristol : IOP Publishing, 2023) Lünser, Klara; Undisz, Andreas; Nielsch, Kornelius; Fähler, SebastianUnderstanding the martensitic microstructure in nickel-titanium (NiTi) thin films helps to optimize their properties for applications in microsystems. Epitaxial and single-crystalline films can serve as model systems to understand the microstructure, as well as to exploit the anisotropic mechanical properties of NiTi. Here, we analyze the growth of NiTi on single-crystalline MgO(100) and Al2O3(0001) substrates and optimize film and buffer deposition conditions to achieve epitaxial films in (100)- and (111)-orientation. On MgO(100), we compare the transformation behavior and crystal quality of (100)-oriented NiTi films on different buffer layers. We demonstrate that a vanadium buffer layer helps to decrease the low-angle grain boundary density in the NiTi film, which inhibits undesired growth twins and leads to higher transformation temperatures. On Al2O3(0001), we analyze the orientation of a chromium buffer layer and find that it grows (111)-oriented only in a narrow temperature range around 500 ∘C. By depositing the Cr buffer below the NiTi film, we can prepare (111)-oriented, epitaxial films with transformation temperatures above room temperature. Transmission electron microscopy confirms a martensitic microstructure with Guinier Preston-zone precipitates at room temperature. We identify the deposition conditions to approach the ideal single crystalline state, which is beneficial for the analysis of the martensitic microstructure and anisotropic mechanical properties in different film orientations.
- ItemInfluence of Alumina Addition on the Optical Properties and the Thermal Stability of Titania Thin Films and Inverse Opals Produced by Atomic Layer Deposition(Basel : MDPI, 2021) Waleczek, Martin; Dendooven, Jolien; Dyachenko, Pavel; Petrov, Alexander Y.; Eich, Manfred; Blick, Robert H.; Detavernier, Christophe; Nielsch, Kornelius; Furian, Kaline P.; Zierold, RobertTiO2 thin films deposited by atomic layer deposition (ALD) at low temperatures (<100 °C) are, in general, amorphous and exhibit a smaller refractive index in comparison to their crystalline counterparts. Nonetheless, low-temperature ALD is needed when the substrates or templates are based on polymeric materials, as the deposition has to be performed below their glass transition or melting temperatures. This is the case for photonic crystals generated via ALD infiltration of self-assembled polystyrene templates. When heated up, crystal phase transformations take place in the thin films or photonic structures, and the accompanying volume reduction as well as the burn-out of residual impurities can lead to mechanical instability. The introduction of cation doping (e.g., Al or Nb) in bulk TiO2 parts is known to alter phase transitions and to stabilize crystalline phases. In this work, we have developed low-temperature ALD super-cycles to introduce Al2O3 into TiO2 thin films and photonic crystals. The aluminum oxide content was adjusted by varying the TiO2:Al2O3 internal loop ratio within the ALD super-cycle. Both thin films and inverse opal photonic crystal structures were subjected to thermal treatments ranging from 200 to 1200 °C and were characterized by in- and ex-situ X-ray diffraction, spectroscopic ellipsometry, and spectroscopic reflectance measurements. The results show that the introduction of alumina affects the crystallization and phase transition temperatures of titania as well as the optical properties of the inverse opal photonic crystals (iPhC). The thermal stability of the titania iPhCs was increased by the alumina introduction, maintaining their photonic bandgap even after heat treatment at 900 °C and outperforming the pure titania, with the best results being achieved with the super-cycles corresponding to an estimated alumina content of 26 wt.%.
- ItemCan gadolinium compete with La-Fe-Co-Si in a thermomagnetic generator?(Abingdon : Taylor & Francis, 2021) Dzekan, Daniel; Diestel, Anett; Berger, Dietmar; Nielsch, Kornelius; Fähler, SebastianA thermomagnetic generator is a promising technology to harvest low-grade waste heat and convert it into electricity. To make this technology competitive with other technologies for energy harvesting near room temperature, the optimum thermomagnetic material is required. Here we compare the performance of a state of the art thermomagnetic generator using gadolinium and La-Fe-Co-Si as thermomagnetic material, which exhibit strong differences in thermal conductivity and type of magnetic transition. gadolinium is the established benchmark material for magnetocaloric cooling, which follows the reverse energy conversion process as compared to thermomagnetic energy harvesting. Surprisingly, La-Fe-Co-Si outperforms gadolinium in terms of voltage and power output. Our analysis reveals the differences in thermal conductivity are less important than the particular shape of the magnetization curve. In gadolinium an unsymmetrical magnetization curve is responsible for an uncompensated magnetic flux, which results in magnetic stray fields. These stray fields represent an energy barrier in the thermodynamic cycle and reduce the output of the generator. Our detailed experiments and simulations of both, thermomagnetic materials and generator, clearly reveal the importance to minimize magnetic stray fields. This is only possible when using materials with a symmetrical magnetization curve, such as La-Fe-Co-Si.
- ItemStress and Microstructure Evolution in Mo Thin Films without or with Cover Layers during Thermal-Cycling(Basel : MDPI, 2020) Park, Eunmi; Seifert, Marietta; Rane, Gayatri K.; Menzel, Siegfried B.; Gemming, Thomas; Nielsch, KorneliusThe intrinsic stress behavior and microstructure evolution of Molybdenum thin films were investigated to evaluate their applicability as a metallization in high temperature microelectronic devices. For this purpose, 100 nm thick Mo films were sputter-deposited without or with an AlN or SiO2 cover layer on thermally oxidized Si substrates. The samples were subjected to thermal cycling up to 900 °C in ultrahigh vacuum; meanwhile, the in-situ stress behavior was monitored by a laser based Multi-beam Optical Sensor (MOS) system. After preannealing at 900 °C for 24 h, the uncovered films showed a high residual stress at room temperature and a plastic behavior at high temperatures, while the covered Mo films showed an almost entirely elastic deformation during the thermal cycling between room temperature and 900 °C with hardly any plastic deformation, and a constant stress value during isothermal annealing without a notable creep. Furthermore, after thermal cycling, the Mo films without as well as with a cover layer showed low electrical resistivity (≤10 μΩ·cm).
- ItemIncreasing the Diversity and Understanding of Semiconductor Nanoplatelets by Colloidal Atomic Layer Deposition(Weinheim : Wiley-VCH, 2020) Reichhelm, Annett; Hübner, René; Damm, Christine; Nielsch, Kornelius; Eychmüller, AlexanderNanoplatelets (NPLs) are a remarkable class of quantum confined materials with size-dependent optical properties, which are determined by the defined thickness of the crystalline platelets. To increase the variety of species, the colloidal atomic layer deposition method is used for the preparation of increasingly thicker CdSe NPLs. By growing further crystalline layers onto the surfaces of 4 and 5 monolayers (MLs) thick NPLs, species from 6 to 13 MLs are achieved. While increasing the thickness, the heavy-hole absorption peak shifts from 513 to 652 nm, leading to a variety of NPLs for applications and further investigations. The thickness and number of MLs of the platelet species are determined by high-resolution transmission electron microscopy (HRTEM) measurements, allowing the interpretation of several contradictions present in the NPL literature. In recent years, different assumptions are published, leading to a lack of clarity in the fundamentals of this field. Regarding the ongoing scientific interest in NPLs, there is a certain need for clarification, which is provided in this study. © 2020 The Authors. Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
- ItemHeterostructured Bismuth Telluride Selenide Nanosheets for Enhanced Thermoelectric Performance(Weinheim : Wiley-VCH GmbH, 2020) Bauer, Christoph; Veremchuk, Igor; Kunze, Christof; Benad, Albrecht; Dzhagan, Volodymyr M.; Haubold, Danny; Pohl, Darius; Schierning, Gabi; Nielsch, Kornelius; Lesnyak, Vladimir; Eychmüller, AlexanderThe n-type semiconductor system Bi2Te3Bi2Se3 is known as a low-temperature thermoelectric material with a potentially high efficiency. Herein, a facile approach is reported to synthesize core/shell heterostructured Bi2Te2Se/Bi2Te3 nanosheets (NSs) with lateral dimensions of 1-3 mu m and thickness of about 50nm. Bi2Te3 and Bi2Se3, as well as heterostructured Bi2Te2Se/Bi2Te3 NSs are obtained via colloidal synthesis. Heterostructured NSs show an inhomogeneous distribution of the chalcogen atoms forming selenium and tellurium-rich layers across the NS thickness, resulting in a core/shell structure. Detailed morphological studies reveal that these structures contain nanosized pores. These features contribute to the overall thermoelectric properties of the material, inducing strong phonon scattering at grain boundaries in compacted solids. NSs are processed into nanostructured bulks through spark plasma sintering of dry powders to form a thermoelectric material with high power factor. Electrical characterization of our materials reveals a strong anisotropic behavior in consolidated pellets. It is further demonstrated that by simple thermal annealing, core/shell structure can be controllably transformed into alloyed one. Using this approach pellets with Bi2Te2.55Se0.45 composition are obtained, which exhibit low thermal conductivity and high power factor for in-plane direction with zT of 1.34 at 400K.
- ItemVoltage-controlled on switching and manipulation of magnetization via the redox transformation of β-FeOOH nanoplatelets(Bristol : IOP Publ., 2020) Nichterwitz, Martin; Neitsch, Sabine; Röher, Stefan; Wolf, Daniel; Nielsch, Kornelius; Leistner, KarinRedox-based metal/metal oxide transformations achieved via electrolytic gating recently emerged as a novel, magneto-ionic route for voltage control of magnetism. So far, mainly metal or oxide thin films and nanoporous metal alloy structures are used as starting materials. The present study demonstrates a magneto-ionic transformation starting from a stable electrodeposited FeOOH nanoplatelet structure. The application of a low voltage in a Li-based electrolyte results in the reduction of the virtually non-magnetic FeOOH into ferromagnetic Fe, yielding an ON switching of magnetization. The magnetization can be tuned in a large range by the time of voltage application and remains stable after voltage-switch off. A reversible magneto-ionic change of magnetization of up to 15% is achieved in the resulting iron films with a thickness of about 30 nm. This large magneto-ionic effect is attributed to the enhanced roughness of the iron films obtained from the nanoplatelet structure. The robust, voltage-controlled, and non-volatile ON switching of magnetism starting from a stable oxide structure is promising for the development of energy-efficient magnetic switches, magnetic actuation and may offer new avenues in magnetoelectronic devices. © 2019 IOP Publishing Ltd.
- ItemInfluence of Lattice Mismatch on Structural and Functional Properties of Epitaxial Ba0.7Sr0.3TiO3 Thin Films(Basel : MDPI, 2023) Wawra, Jonas; Nielsch, Kornelius; Hühne, RubenSubstrate-induced strains can significantly influence the structural properties of epitaxial thin films. In ferroelectrics, this might lead to significant changes in the functional properties due to the strong electromechanical coupling in those materials. To study this in more detail, epitaxial Ba0.7Sr0.3TiO3 films, which have a perovskite structure and a structural phase transition close to room temperature, were grown with different thicknesses on REScO3 (RE–rare earth element) substrates having a smaller lattice mismatch compared to SrTiO3. A fully strained SrRuO3 bottom electrode and Pt top contacts were used to achieve a capacitor-like architecture. Different X-ray diffraction techniques were applied to study the microstructure of the films. Epitaxial films with a higher crystalline quality were obtained on scandates in comparison to SrTiO3, whereas the strain state of the functional layer was strongly dependent on the chosen substrate and the thickness. Differences in permittivity and a non-linear polarization behavior were observed at higher temperatures, suggesting that ferroelectricity is supressed under tensile strain conditions in contrast to compressive strain for our measurement configuration, while a similar reentrant relaxor-like behavior was found in all studied layers below 0°C.
- ItemTowards tellurium-free thermoelectric modules for power generation from low-grade heat(London : Nature Publishing Group, 2021) Ying, Pingjun; He, Ran; Mao, Jun; Zhang, Qihao; Reith, Heiko; Sui, Jiehe; Ren, Zhifeng; Nielsch, Kornelius; Schierning, GabiThermoelectric technology converts heat into electricity directly and is a promising source of clean electricity. Commercial thermoelectric modules have relied on Bi2Te3-based compounds because of their unparalleled thermoelectric properties at temperatures associated with low-grade heat (<550 K). However, the scarcity of elemental Te greatly limits the applicability of such modules. Here we report the performance of thermoelectric modules assembled from Bi2Te3-substitute compounds, including p-type MgAgSb and n-type Mg3(Sb,Bi)2, by using a simple, versatile, and thus scalable processing routine. For a temperature difference of ~250 K, whereas a single-stage module displayed a conversion efficiency of ~6.5%, a module using segmented n-type legs displayed a record efficiency of ~7.0% that is comparable to the state-of-the-art Bi2Te3-based thermoelectric modules. Our work demonstrates the feasibility and scalability of high-performance thermoelectric modules based on sustainable elements for recovering low-grade heat.
- ItemInterface-Dominated Topological Transport in Nanograined Bulk Bi2 Te3(Weinheim : Wiley-VCH, 2021) Izadi, Sepideh; Han, Jeong Woo; Salloum, Sarah; Wolff, Ulrike; Schnatmann, Lauritz; Asaithambi, Aswin; Matschy, Sebastian; Schlörb, Heike; Reith, Heiko; Perez, Nicolas; Nielsch, Kornelius; Schulz, Stephan; Mittendorff, Martin; Schierning, Gabi3D topological insulators (TI) host surface carriers with extremely high mobility. However, their transport properties are typically dominated by bulk carriers that outnumber the surface carriers by orders of magnitude. A strategy is herein presented to overcome the problem of bulk carrier domination by using 3D TI nanoparticles, which are compacted by hot pressing to macroscopic nanograined bulk samples. Bi2Te3 nanoparticles well known for their excellent thermoelectric and 3D TI properties serve as the model system. As key enabler for this approach, a specific synthesis is applied that creates nanoparticles with a low level of impurities and surface contamination. The compacted nanograined bulk contains a high number of interfaces and grain boundaries. Here it is shown that these samples exhibit metallic-like electrical transport properties and a distinct weak antilocalization. A downward trend in the electrical resistivity at temperatures below 5 K is attributed to an increase in the coherence length by applying the Hikami–Larkin–Nagaoka model. THz time-domain spectroscopy reveals a dominance of the surface transport at low frequencies with a mobility of above 103 cm2 V−1 s−1 even at room temperature. These findings clearly demonstrate that nanograined bulk Bi2Te3 features surface carrier properties that are of importance for technical applications.