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Ferritic-austenitic chromia-forming alloys are frequently used as boiler tubes and heat exchanger materials for fossil-,biomass, and co-fired power plants. In all applied environments several strongly corrosive gaseous species such as CO2, SO2, SO3, H2O, O2 exist, causing materials degradation by high-temperature corrosion. The elucidation of degradation mechanisms introduced by multiple gases is challenging due to the presence of different oxidizing agents contributing to the competing reactions for oxidation, sulfurization or carburization. The degradation processes can be divided into initial stages, a transitional stage and the further proceeding steady-state oxidation reaction. Especially the long-term steady-state oxidation and further materials’ life-time are strongly dependent on the initial stages. The adsorption and absorption of the reactive species at the alloy surface and the growing oxide in the initial reaction is further influenced by dissociation and re-reactions of the gas phase molecules. To understand these mechanisms from a fundamental point of view in more detail, dedicated experiments and advanced characterization techniques on various length scale need to be applied. Real-time approaches using highly energetic synchrotron X-ray diffraction showed a high potential to enlighten competitively mechanisms by following the corrosion reactions in-situ in the environment they occur. Despite various other thin film characterization techniques, time of flight secondary ion mass spectroscopy (ToF-SIMS) is a powerful tool to visualize light atoms or labeled isotopes enabling the Differentiation between different oxidizing species. It was especially shown to be applicable in challenging atmospheres containing KCl deposits or in CO/CO2/O2 environments. The present study analyses the competing oxidation/sulfidation process in a humid atmosphere on two ferritic alloys with 2 and 9 % in weight chromium by in situ energy dispersive X-ray diffraction (EDXRD) and comparative tube furnace exposure using S16O2 and H2 18O atmosphere.
P92 is one of the important steels for super heater tubes used in combustion plants. However, in fossil fuel fired environments the formation of oxides and sulfides are challenging the material. To understand early corrosion mechanisms, which are important for process prediction, high temperature in-situ ageing experiments of Fe-Cr-Mn alloys in SO2 and SO2+H2O atmosphere were performed, applying energy dispersive X-ray diffraction (EDXRD) analysis.
We investigated the effect of water vapor in the initial stages of SO2 corrosion of an Fe-9Cr-0.5Mn model alloy at 650 °C. Two separate experiments were run, one with 99.5%-Ar + 0.5%-SO2 and one with 69.5%-Ar + 0.5%-SO2 with 30%-H2O atmosphere. During the experiment the scale growth was observed in-situ, using energy dispersive X-ray diffraction (EDXRD). Our results confirm an increased speed of oxygen transport into the material, with the addition of water, while the transport of sulfur appears to be less affected.
In-situ analysis of solid state phase transformation in TRIP-aided steels by synchrotron diffraction
(2011)
Energy dispersive synchrotron diffraction (EDXRD) analysis and 3 dimensional digital image correlations were conducted to investigate the stress and strain effected transformation behavior during tensile loading of low alloyed TRansformation Induced Plasticity (TRIP) steel. This technique allowed for phase specific stress measurement during certain tensile load steps in the elastic and also plastic regime. Additionally the simultaneous determination of the load dependent phase content was realized. The results show that the martensite transformation starts only after exceeding the overall yield point and is finished before reaching the uniform elongation, whereas a large portion of the austenite remains unchanged in the structure. Furthermore, the martensite transformation related to the stress in the γ-phase and α-phase was analyzed and quantified.
Energy-dispersive x-ray diffraction offers the possibility for measurement and evaluation of diffraction spectra containing information of various diffraction lines of all contributing crystalline phases of a material. Combined strain imaging and diffraction analysis was conducted during the tensile test of a low alloyed transformation-induced plasticity (TRIP) steel in order to investigate the transformation induced plasticity, strain hardening, and load partitioning effects. Optical strain imaging allowed for determination of localized true strains from three-dimensional deformations measured in situ. High-energy synchrotron radiation has permitted diffraction analysis in transmission mode to gather information from the material interior. Phase-specific stress evolution during loading could be observed applying the sin2ψ technique during certain load steps. The strains of the individual lattice planes were determined in different locations under varying angles between loading and perpendicular direction. Using energy-dispersive methods it was also possible to determine the transformation behaviour during elastic and plastic regime taking into account a large number of diffraction lines. The results show that the approach practised here enables one to pull together macroscopic and phase-specific microscopic material behaviour in order to improve existing models for prediction of complex load situations.