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The central commitment of the 2015 World Climate Conference is to limit geothermal heating by massively reducing greenhouse gas emissions by decreasing the use of fossil fuels and promoting environmentally friendly energy. However, since renewable energies have so far not been available as required and are difficult to store, there is a short-term solution in the conversion, storage and reuse of climate-damaging combustion gases. An efficient solution for using CO2 is to convert it into a gas that can be stored and used to generate energy. With the so-called “power-to-gas technology”, a significant reduction in greenhouse gas emissions can be achieved by methanation of CO2 if methane slip is avoided. Methanation is a chemical reaction in which carbon dioxide reacts with hydrogen to methane. This transformation, which normally takes place at 350 ° C to 600 ° C, is also known as the Sabatier reaction. In addition to methane and water, the remaining reactants such as carbon dioxide, hydrogen, oxygen and nitrogen as well as small amounts of impurities from the combustion process, occur as reaction products. Reaction containers and lines are usually made of stainless steel. Due to high ambient temperature and aggressive ambient media, corrosion can also occur with the generally temperature and corrosion-resistant 316L material, influence material properties and lead to material failure. To assess the influence of the CO2 methanation process on 316L, a laboratory-scale methanation reactor was fractioned and examined after use. Corrosion deposits were found in various components of the reactor (gas supply line, gas outlet, reactor segment). Depending on their position within the component, these corrosion layers are structured very differently. Microstructure and element composition of the layers were analyzed using scanning electron microscopy combined with energy-dispersive X-ray spectroscopy. While the gas supply shows only moderate corrosion attack, crevice, contact- and pitting corrosion were detected in the corroded area of the gas outlet. Three zones (multilayer structure, particle accumulation and brittle passive film) were identified within the corrosion layers. The multi-layer zone is composed of columnar and granular structures, the particle accumulations consist of cylindrical and spherical particles. The element composition within the corrosion layers suggests contact corrosion caused by the material of the sealing rings.
Die Weltklimakonferenz fordert eine massive Senkung der Treibhausgasemissionen mittels Abkehr von der Nutzung fossiler Brennstoffe hin zur Verwendung umweltverträglich hergestellter Energie. Da erneuerbare Energien aber bisher nicht durchweg bedarfsgerecht zur Verfügung stehen und schlecht speicherbar sind, besteht eine kurzfristige Lösungsmöglichkeit in Umwandlung, Speicherung und Wiederverwendung klimaschädlicher Verbrennungsgase. Eine effiziente Lösung zur Nutzung von CO2 ist dessen Umwandlung in ein speicherbares, zur Energieerzeugung nutzbares Gas. Mit der Methanisierung von CO2 kann eine erhebliche Reduzierung der Treibhausgasemissionen erreicht werden, wenn Methanschlupf vermieden wird. Bei dieser sogenannten Sabatier-Reaktion, die normalerweise bei 350°C bis 600°C stattfindet, reagiert Kohlendioxid mit Wasserstoff zu Methan. Als Reaktionsprodukte treten außer Methan und Wasser die Rest-Reaktanten sowie kleine Mengen an Verunreinigungen aus dem Verbrennungsprozess auf.
Reaktionsbehälter und Leitungen bestehen üblicherweise aus Edelstahl. Durch hohe Umgebungs-temperatur und aggressive Umgebungsmedien kann auch bei dem normalerweise temperatur- und korrosionsbeständigen Werkstoff 316L Korrosion auftreten, Materialeigenschaften beeinflussen und zu Materialversagen führen. Zur Bewertung des Einflusses des CO2 Methanisierungs-Prozesses auf 316L wurde ein Methanisierungs-Reaktor im Labormaßstab nach der Nutzung demontiert und untersucht. In verschiedenen Bauteilen des Reaktors (Gaszuleitung, Gasaustritt, Reaktorsegment) wurden Korrosionsbeläge gefunden. Abhängig von ihrer Lage im Bauteil sind diese Korrosionsschichten sehr unterschiedlich aufgebaut. Mikrostruktur und Elementzusammensetzung der Schichten wurden mittels Rasterelektronenmikroskopie kombiniert mit energiedispersiver Röntgenspektroskopie analysiert. Während die Gaszuleitung nur moderaten Korrosionsangriff zeigt konnten im Bereich des Gasaustritts Spalt-, Kontakt- und Lochkorrosion nachgewiesen werden. Innerhalb der Korrosions¬schichten wurden drei Zonen (Mehrschichtenstruktur, Partikelansammlung und brüchiger Passivfilm) identifiziert. Die Mehrschichtzone setzt sich aus kolumnaren und granularen Strukturen zusammen, die Partikelansammlungen bestehen aus zylinderförmigen und kugelförmigen Partikeln. Die Elementzusammensetzung innerhalb der Korrosionsschichten lässt auf Kontaktkorrosion verursacht durch das Material der Dichtringe schließen.
A deep surface modified TiZr layer was fabricated by high-intensity low-energy titanium ion implantation into zirconium alloy Zr-1Nb alloy with the various dose in the range of (5.4–9.56) × 1020 ion/cm2. The gradient distribution of titanium as well as vacancy type defects were analysed. The effects of ion implantation on microstructure, phase composition and elemental distribution of TiZr layer were analysed by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and glow-discharge optical emission spectroscopy, respectively. The results show the appearance of Zr-Ti intermetallic phases of different stoichiometry after Ti implantation. The intermetallic phases are transformed from both Zr0.7Ti0.3 and Zr0.5Ti0.5 to single Zr0.6Ti0.4 phase with the increase in the implantation dose.
The depth of Ti penetration into the bulk of Zr increases from 6 to 13 μm with the implantation dose. The higher current density (170 mA/cm2) leads to the increase in the grain size and surface roughness. It was revealed that TiZr layer (~10 μm thickness) is represented by α′ + α(TiZr) lamellar microstructure with gradient distribution of Ti through the layer depth. Transmission electron microscopy was used for investigation of the physical basis of Ti diffusion and its influence on the evolution of the defect structure after surface modification. Furthermore, it was found that on the surface between substrate and implanted layer was found an amorphous layer, which occur as a result of further stress accumulations from the higher implantation doses.
Oxidation behavior of Zr–1Nb in air at 400°C after Titanium Plasma Immersion Ion Implantation
(2018)
Zirconium alloys have been widely used in nuclear reactors due to low thermal neutron capture cross-section, excellent corrosion resistance and acceptable mechanical properties [1, 2]. Nowadays several methods apply for improving hydrogen and corrosion resistance such as addition of stabilizing additives (yttrium) [3, 4], deposition of thin solid films [5, 6], micro-arc oxidation [7] and modification of the surface by electron beam [8, 9]. Despite the multiplicity of the methods hydrogen embrittlement is still a pressing issue. Previous results [10, 11] have shown the positive influence of plasma immersion titanium implantation on the hydrogenation behavior of Zr–1Nb and Zr–2.5 Nb. After Ti implantation hydrogen preferably accumulates in the modified surface layer comprising the implanted Ti. Furthermore, the hydrogen concentration is considerably less inside the zirconium modified sample than in the as-received samples.
The integration of elements into the zirconium lattice can influence the valence of the surface and change corrosion and oxidation rates of the alloys. So it is very important not to decrease the zirconium oxidation resistance due to Ti implantation. Therefore, the purpose of this research is to study of the influence of Ti implantation on surface morphology, oxidation rate and phase structure of the Zr–1Nb alloy after oxidation on air at 400 0C for 5, 24, 72 and 240 h. The surface structure of the samples and their elemental composition were investigated with the scanning electron microscope Mira II XMH (Tescan) with energy dispersive x-ray spectroscopy system (EDS). X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC) as well as X-ray diffraction (XRD) was used to characterise the influence of titanium implantation on the oxidation behaviour. The results show that the oxidation kinetics after Ti modification of the zirconium alloy changed. Although the weight gain of the implanted sample remains approximately the same, it can be considered that Ti implantation stabilizes the oxide layer and has beneficial influence on the oxidation protection of Zr-1Nb.
Investigation of TiAlN HiPIMS coating deposited on the newly developed Ni-based superalloy AD730
(2016)
The development of new alloys for gas turbine engines has been focused on withstanding against increasing service temperatures. AD730™ is a recently developed nickel-based superalloy for turbine disk applications with superior
properties at 700°C, which is higher than the common service temperature for IN718. Use of coatings to enhance the properties of materials, such as wear resistance is widely known in various applications. This research presents an experimental study of TiAlN coatings, deposited onto AD730 superalloy using High Power Impulse Magnetron Sputtering (HiPIMS). Phase structure and chemical composition of the TiAlN films were characterized by X-ray diffractometry. Transmission electron microscopy as well as scanning electron microscopy were used to analyze the
microstructure of the coating. Mechanical properties, including hardness, Young's modulus, and adhesion strength were measured using nanoindentation und scratch test.
Effect of pulse time on structure and mechanical properties of HPPMS deposited AlTiN coatings
(2016)
The use of PVD AlTiN as a protective coating on cutting tools is well known. With the introduction of pulsed deposition techniques like High Power Pulsed Sputtering
(HPPMS), a possibility is provided to the coating developers to design their coatings by the variation in pulse parameters. To analyze the effect of pulse time HPPMS
AlTiN coatings were deposited on Si (100) as well as 100Cr6 steel plates at a temperature of 500°C in a reactive gas environment. Oscilloscope measurements depicted a change in current-voltage characteristics with variation in pulse time. This influence the coating structure, deposition rates and phase formations as well. Nanoindentation results show a variation in the mechanical properties of the coatings with the change in pulse time. This study focuses on the potential of HPPMS technology for enhancement of mechanical and structural properties of AlTiN coating.