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- ItemMo-La2O3 multilayer metallization systems for high temperature surface acoustic wave sensor devices(Basel : MDPI AG, 2019) Menzel, S.B.; Seifert, M.; Priyadarshi, A.; Rane, G.K.; Park, E.; Oswald, S.; Gemming, T.Developing advanced thin film materials is the key challenge in high-temperature applications of surface acoustic wave sensor devices. One hundred nanometer thick (Mo-La2O3) multilayer systems were fabricated at room temperature on thermally oxidized (100) Si substrates (SiO2/Si) to study the effect of lanthanum oxide on the electrical resistivity of molybdenum thin films and their high-temperature stability. The multilayer systems were deposited by the magnetron sputter deposition of extremely thin (≤1 nm) La interlayers in between adjacent Mo layers. After deposition of each La layer the process was interrupted for 25 to 60 min to oxidize the La using the residual oxygen in the high vacuum of the deposition chamber. The samples were annealed at 800 °C in high vacuum for up to 120 h. In case of a 1 nm thick La interlayer in-between the Mo a continuous layer of La2O3 is formed. For thinner La layers an interlayer between adjacent Mo layers is observed consisting of a (La2O3-Mo) mixed structure of molybdenum and nm-sized lanthanum oxide particles. Measurements show that the (Mo-La2O3) multilayer systems on SiO2/Si substrates are stable at least up to 800 °C for 120 h in high vacuum conditions.
- ItemPhase formation and high-temperature stability of very thin co-sputtered Ti-Al and multilayered Ti/Al films on thermally oxidized si substrates(Basel : MDPI AG, 2020) Seifert, M.; Lattner, E.; Menzel, S.B.; Oswald, S.; Gemming, T.Ti-Al thin films with a thickness of 200 nm were prepared either by co-sputtering from elemental Ti and Al targets or as Ti/Al multilayers with 10 and 20 nm individual layer thickness on thermally oxidized Si substrates. Some of the films were covered with a 20-nm-thick SiO2 layer, which was used as an oxidation protection against the ambient atmosphere. The films were annealed at up to 800 °C in high vacuum for 10 h, and the phase formation as well as the film architecture was analyzed by X-ray diffraction, cross section, and transmission electron microscopy, as well as Auger electron and X-ray photoelectron spectroscopy. The results reveal that the co-sputtered films remained amorphous after annealing at 600 °C independent on the presence of the SiO2 cover layer. In contrast to this, the γ-TiAl phase was formed in the multilayer films at this temperature. After annealing at 800 °C, all films were degraded completely despite the presence of the cover layer. In addition, a strong chemical reaction between the Ti and SiO2 of the cover layer and the substrate took place, resulting in the formation of Ti silicide. In the multilayer samples, this reaction already started at 600 °C.
- ItemEffects of Promoter on Structural and Surface Properties of Zirconium Oxide-Based Catalyst Materials(Basel : MDPI AG, 2020) Borovinskaya, E.S.; Oswald, S.; Reschetilowski, W.Ternary mixed oxide systems CuO/ZnO/ZrO2 and CuO/NiO/ZrO2 were synthesized by one-pot synthesis for a better understanding of the synthesis-property relationships of zirconium oxide-based catalyst materials. The prepared mixed oxide samples were analysed by a broad range of characterisation methods (XRD, N2-physisorption, Temperature-Programmed Ammonia Desorption (TPAD), and XPS) to examine the structural and surface properties, as well as to identify the location of the potential catalytically active sites. By XPS analysis, it could be shown that a progressive enrichment of the surface composition with copper takes place by changing from ZnO to NiO as a promoter. Thus, by addition of the second component, not only electronic but also the geometric properties of active sites, i.e., copper species distribution within the catalyst surface, can be affected in a desired way.
- ItemAmorphous Li-Al-based compounds: A novel approach for designing high performance electrode materials for Li-ion batteries(Basel : MDPI AG, 2013) Thoss, F.; Giebeler, L.; Thomas, J.; Oswald, S.; Potzger, K.; Reuther, H.; Ehrenberg, H.; Eckert, J.A new amorphous compound with the initial atomic composition Al43Li43Y6Ni8 applied as electrode material for Li-ion batteries is investigated. Unlike other amorphous compounds so-far investigated as anode materials, it already contains Li as a base element in the uncycled state. The amorphous compound powder is prepared by high energy ball milling of a master alloy. It shows a strongly enhanced specific capacity in contrast to amorphous alloys without Li in the initial state. Therewith, by enabling a reversible (de)lithiation of metallic electrodes without the phase transition caused volume changes it offers the possibility of much increased specific capacities than conventional graphite anodes. According to the charge rate (C-rate), the specific capacity is reversible over 20 cycles at minimum in contrast to conventional crystalline intermetallic phases failing by volume changes. The delithiation process occurs quasi-continuously over a voltage range of nearly 4 V, while the lithiation is mainly observed between 0.1 V and 1.5 V. That way, the electrode is applicable for different potential needs. The electrode stays amorphous during cycling, thus avoiding volume changes. The cycling performance is further enhanced by a significant amount of Fe introduced as wear debris from the milling tools, which acts as a promoting element.
- ItemBinding energy referencing for XPS in Alkali metal-based battery materials research (II): Application to complex composite electrodes(Basel : MDPI AG, 2018) Oswald, S.; Thoss, F.; Zier, M.; Hoffmann, M.; Jaumann, T.; Herklotz, M.; Nikolowski, K.; Scheiba, F.; Kohl, M.; Giebeler, L.; Mikhailova, D.; Ehrenberg, H.X-ray photoelectron spectroscopy (XPS) is a key method for studying (electro-)chemical changes in metal-ion battery electrode materials. In a recent publication, we pointed out a conflict in binding energy (BE) scale referencing at alkali metal samples, which is manifested in systematic deviations of the BEs up to several eV due to a specific interaction between the highly reactive alkali metal in contact with non-conducting surrounding species. The consequences of this phenomenon for XPS data interpretation are discussed in the present manuscript. Investigations of phenomena at surface-electrolyte interphase regions for a wide range of materials for both lithium and sodium-based applications are explained, ranging from oxide-based cathode materials via alloys and carbon-based anodes including appropriate reference chemicals. Depending on material class and alkaline content, specific solutions are proposed for choosing the correct reference BE to accurately define the BE scale. In conclusion, the different approaches for the use of reference elements, such as aliphatic carbon, implanted noble gas or surface metals, partially lack practicability and can lead to misinterpretation for application in battery materials. Thus, this manuscript provides exemplary alternative solutions.