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- 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.%.
- 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).
- 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.
- ItemMagnetic Properties of GaAs/NiFe Coaxial Core-Shell Structures(Basel : MDPI, 2022) Monaico, Eduard V.; Morari, Vadim; Kutuzau, Maksim; Ursaki, Veaceslav V.; Nielsch, Kornelius; Tiginyanu, Ion M.Uniform nanogranular NiFe layers with Ni contents of 65%, 80%, and 100% have been electroplated in the potentiostatic deposition mode on both planar substrates and arrays of nanowires prepared by the anodization of GaAs substrates. The fabricated planar and coaxial core-shell ferromagnetic structures have been investigated by means of scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM). To determine the perspectives for applications, a comparative analysis of magnetic properties, in terms of the saturation and remanence moment, the squareness ratio, and the coercivity, was performed for structures with different Ni contents.
- ItemEuropium Clustering and Glassy Magnetic Behavior in Inorganic Clathrate-VIII Eu8Ga16Ge30(Basel : MDPI, 2022) Pérez, Nicolás; Sahoo, Manaswini; Schierning, Gabi; Nielsch, Kornelius; Nolas, George S.The temperature- and field-dependent, electrical and thermal properties of inorganic clathrate-VIII Eu8Ga16Ge30 were investigated. The type VIII clathrates were obtained from the melt of elements as reported previously. Specifically, the electrical resistivity data show hysteretic magnetoresistance at low temperatures, and the Seebeck coefficient and Hall data indicate magnetic interactions that affect the electronic structure in this material. Heat capacity and thermal conductivity data corroborate these findings and reveal the complex behavior due to Eu2+ magnetic ordering and clustering from approximately 13 to 4 K. Moreover, the low-frequency dynamic response indicates Eu8Ga16Ge30 to be a glassy magnetic system. In addition to advancing our fundamental understanding of the physical properties of this material, our results can be used to further the research for potential applications of interest in the fields of magnetocalorics or thermoelectrics.
- ItemExchange Bias Effect of Ni@(NiO,Ni(OH)2) Core/Shell Nanowires Synthesized by Electrochemical Deposition in Nanoporous Alumina Membranes(Basel : MDPI, 2023) García, Javier; Gutiérrez, Ruth; González, Ana S.; Jiménez-Ramirez, Ana I.; Álvarez, Yolanda; Vega, Víctor; Reith, Heiko; Leistner, Karin; Luna, Carlos; Nielsch, Kornelius; Prida, Víctor M.Tuning and controlling the magnetic properties of nanomaterials is crucial to implement new and reliable technologies based on magnetic hyperthermia, spintronics, or sensors, among others. Despite variations in the alloy composition as well as the realization of several post material fabrication treatments, magnetic heterostructures as ferromagnetic/antiferromagnetic coupled layers have been widely used to modify or generate unidirectional magnetic anisotropies. In this work, a pure electrochemical approach has been used to fabricate core (FM)/shell (AFM) Ni@(NiO,Ni(OH)2) nanowire arrays, avoiding thermal oxidation procedures incompatible with integrative semiconductor technologies. Besides the morphology and compositional characterization of these core/shell nanowires, their peculiar magnetic properties have been studied by temperature dependent (isothermal) hysteresis loops, thermomagnetic curves and FORC analysis, revealing the existence of two different effects derived from Ni nanowires’ surface oxidation over the magnetic performance of the array. First of all, a magnetic hardening of the nanowires along the parallel direction of the applied magnetic field with respect their long axis (easy magnetization axis) has been found. The increase in coercivity, as an effect of surface oxidation, has been observed to be around 17% (43%) at 300 K (50 K). On the other hand, an increasing exchange bias effect on decreasing temperature has been encountered when field cooling (3T) the oxidized Ni@(NiO,Ni(OH)2) nanowires below 100 K along their parallel lengths.
- ItemCore–Shell GaAs-Fe Nanowire Arrays: Fabrication Using Electrochemical Etching and Deposition and Study of Their Magnetic Properties(Basel : MDPI, 2022) Monaico, Eduard V.; Morari, Vadim; Ursaki, Veaceslav V.; Nielsch, Kornelius; Tiginyanu, Ion M.The preparation of GaAs nanowire templates with the cost-effective electrochemical etching of (001) and (111)B GaAs substrates in a 1 M HNO3 electrolyte is reported. The electrochemical etching resulted in the obtaining of GaAs nanowires with both perpendicular and parallel orientations with respect to the wafer surface. Core–shell GaAs-Fe nanowire arrays have been prepared by galvanostatic Fe deposition into these templates. The fabricated arrays have been investigated by means of scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM). The magnetic properties of the polycrystalline Fe nanotubes constituting the shells of the cylindrical structures, such as the saturation and remanence moment, squareness ratio, and coercivity, were analyzed in relation to previously reported data on ferromagnetic nanowires and nanotubes.
- ItemInfluencing Martensitic Transition in Epitaxial Ni-Mn-Ga-Co Films with Large Angle Grain Boundaries(Basel : MDPI, 2020) Lünser, Klara; Diestel, Anett; Nielsch, Kornelius; Fähler, SebastianMagnetocaloric materials based on field-induced first order transformations such as Ni-Mn-Ga-Co are promising for more environmentally friendly cooling. Due to the underlying martensitic transformation, a large hysteresis can occur, which in turn reduces the efficiency of a cooling cycle. Here, we analyse the influence of the film microstructure on the thermal hysteresis and focus especially on large angle grain boundaries. We control the microstructure and grain boundary density by depositing films with local epitaxy on different substrates: Single crystalline MgO(0 0 1), MgO(1 1 0) and Al2O3(0 0 0 1). By combining local electron backscatter diffraction (EBSD) and global texture measurements with thermomagnetic measurements, we correlate a smaller hysteresis with the presence of grain boundaries. In films with grain boundaries, the hysteresis is decreased by about 30% compared to single crystalline films. Nevertheless, a large grain boundary density leads to a broadened transition. To explain this behaviour, we discuss the influence of grain boundaries on the martensitic transformation. While grain boundaries act as nucleation sites, they also lead to different strains in the material, which gives rise to various transition temperatures inside one film. We can show that a thoughtful design of the grain boundary microstructure is an important step to optimize the hysteresis.
- ItemEffect of Silver Doping on the Superconducting and Structural Properties of YBCO Films Grown by PLD on Different Templates(Basel : MDPI, 2022) Shipulin, Ilya A.; Thomas, Aleena Anna; Holleis, Sigrid; Eisterer, Michael; Nielsch, Kornelius; Hühne, RubenWe report the local structural and superconducting properties of undoped and Ag-doped YBa2Cu3O6+x (YBCO) films with a thickness of up to 1 µm prepared by pulsed laser deposition on SrTiO3 (STO) single crystals and on ion-beam-assisted deposition (IBAD) and rolling-assisted biaxially textured substrate (RABiTS)-based metal templates. X-ray diffraction demonstrates the high crystalline quality of the films on both single crystalline substrates and metal-based templates, respectively. Although there was only a slight decrease in Tc of up to 1.5 K for the Ag-doped YBCO films on all substrates, we found significant changes in their transport characteristics. The effect of the silver doping mainly depended on the concentration of silver, the type of substrate, and the temperature and magnetic field. In general, the greatest improvement in Jc over a wide range of magnetic fields and temperatures was observed for the 5%Ag-doped YBCO films on STO substrates, showing a significant increase compared to undoped films. Furthermore, a slight Jc improvement was observed for the 2%Ag-doped YBCO films on the RABiTS templates at temperatures below 65 K, whereas Jc decreased for the Ag-doped films on IBAD-MgO-based templates compared to undoped YBCO films. Using detailed electron microscopy studies, small changes in the local microstructure of the Ag-doped YBCO films were revealed; however, no clear correlation was found with the transport properties of the films.
- 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.