TY - CONF A1 - Stephan-Scherb, Christiane T1 - Applied Crystallography as a tool for a better understanding of Fundamental Questions of high temperature corrosion phenomena N2 - Corrosion Science Meets X-Rays, Neutrons and Electrons. The presentation gives an overview on current research activities applying in-situ X-ray diffraction and spectroscopy for a better understanding of fundamental mechanisms of high temperature corrosion. Additionally the knowledge gain by applying neutron powder diffraction and EBSD analysis is presented. T2 - Joint meeting of german and polish crystallographic association 2020 CY - Wroclaw, Poland DA - 24.02.2020 KW - Corrosion KW - Oxidation KW - In situ KW - Diffraction PY - 2020 AN - OPUS4-50483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Unravelling high temperature oxidation phenomena by in situ x-ray techniques N2 - Unravelling high temperature oxidation phenomena by in situ x-ray techniques. A multi techqnique approach to study high temperature gas corrosion is presented. T2 - Gordon Research Conference on High Temperature Corrosion CY - New London, NH, USA DA - 20.07.2019 KW - Corrosion KW - High temperature KW - Diffraction KW - Spectroscopy PY - 2019 AN - OPUS4-48772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Novel insights into high temperature corrosion phenomena by advanced X-ray methods N2 - A variety of materials of technological interest change their properties through contact with reactive media. Solid-gas reactions lead to a variety of reaction products on the surfaces and internal interfaces. The observation of nucleation and growth processes in the environment where they occur (in situ) from a chemical-structural perspective is especially challenging for aggressive atmospheres. The talk presents innovative approaches to study corrosion mechanisms using advanced X-ray methods. Using energy dispersive X-ray diffraction and X-ray absorption spectroscopy in different tailor made environmental reaction chambers, valuable insights into high temperature oxidation and sulfidation processes were gained. Fe-based alloys were exposed to hot and reactive atmospheres containing gases like SO2, H2O and O2 at 650°C. During the gas exposure the tailor made reaction chambers were connected to a high energy diffraction end station at the synchrotron. The crystallization and growth of oxide and sulfide reaction products at the alloy surfaces were monitored by collecting full diffraction pattern every minute. Careful examination of shape and intensity of phase-specific reflections enabled to a detailed view on growth kinetics. These studies showed, oxides are the first phases occurring immediately after experimental start. As soon as reactive gas media enter the chamber, the conditions change and different reaction products, such as sulfides start to grow. A comparison of different gas environments applied, illustrated the differences in the type of reaction products. The in situ observation of high temperature material degradation by corrosion made it possible to study the contribution of phases, which are not stable at room temperature. For instance, wuestite (Fe1-xO), was frequently observed at high temperatures in humid gases on Fe with 2 wt.% and 9 wt.% chromium, but not at room temperature. The strength of the occurrence of this phase additionally explains why, despite a higher Cr content, ferritic alloys with 9 wt.% Cr in a challenging atmosphere prevent the intrinsic formation of protective layers. The in situ observations were supplemented by careful considerations of thermodynamic boundary conditions and detailed post characterization by classical metallographic analysis. Additionally, the structure and chemistry of the dominant oxide layers were evaluated using X-ray absorption near edge structure spectroscopy. The talk will give an overview about chances and challenges for studying high temperature corrosion phenomena by advanced X-ray methods. T2 - MRS Spring Meeting CT08.02.01 CY - Online Meeting DA - 18.04.2021 KW - XRD KW - Spectroscopy KW - Corrosion KW - High temperature KW - In-situ PY - 2021 AN - OPUS4-52486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Nützmann, Kathrin A1 - Falk, Florian A1 - de Oliveira Guilherme Buzanich, Ana A1 - Witte, Steffen A1 - Radtke, Martin T1 - Early stages of high temperature oxidation/sulfidation studied by synchrotron x-ray diffraction and spectroscopy N2 - Ferritic high temperature alloys are widely used as boiler tube and heat exchanger materials in coal, biomass and co-fired power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres that lead to a change of the material properties and a further degradation of the material. Material changes caused by aging in highly corrosive and toxic gases such as SO2 are mainly studied ex situ after the reaction is finished. The solid material is deposited in the atmosphere for a certain period of time, and material changes are then examined by various microscopic techniques such as optical microscopy (OM), electron microprobe analysis (EMPA), scanning electron microscopy (SEM and TEM) and X-ray diffraction (XRD). Nevertheless, extensive efforts were made to study material changes of high temperature alloys under oxidizing and reducing atmospheres by environmental scanning electron microscopy or in situ TEM techniques However, the possibilities of microscopic in situ techniques are very limited for the use of highly corrosive and toxic gases such as SO2. Since Sulfur induced corrosion at temperatures relevant for coal and biomass fired power plants, which is causing breakaway oxidation and sulfide precipitation at grain boundaries, is still of scientific interest, the current work focuses on the effect of SO2 in an initial stage of corrosion of ferritic alloys. For the analysis of early stages of combined oxidation and sulphidation processes of Fe-Cr model alloys the usage of a light furnace to conduct a rapid reactive annealing experiment is feasible. Previous studies presented distinct results of the influence of chromium on early high temperature corrosion by SO2 by this technique and subsequent classical metallographic analyses. However, it is still not possible to trace the corrosion mechanism in real time by conducting single aging experiments. The current work introduces two different approaches to study the initial stages of high temperature oxidation processes by applying above state of the art X-ray diffraction and spectroscopy methods. One part focuses on the real time observation of the formation of corrosion products such as oxides and sulfides by energy dispersive X-ray diffraction (EDXRD). The potential of this technique to study crystallization and growth processes of thin films in a reactive environment in real time was previously shown for different compound semiconductors. This approach was now applied to follow oxidation and sulphidation processes of ferritic model alloys in SO2 and SO2/H2O environments. The diffraction signals of the X-rays were detected during the corrosion process and the peak area and positions were analyzed as a function of time. This procedure enables monitoring external oxide growth and material loss in real time in an early stage of corrosion. The other part of the current work presents the possibilities of X-ray absorption near edge structure spectroscopy (XANES) to characterize oxide scales and their growth mechanisms. Precise phase identification and quantification of corrosion products in a multi-phase oxide/sulfide scale is a pre-requisite to understand diffusion paths of metal ions and gas components. It is a challenging task to distinguish structurally similar reaction products such as Fe3O4 and FeCr2O4 especially in thin films with texture effects by diffraction. To illustrate for example Cr-out diffusion of an alloy throughout an inner and external oxide scale the differentiation of Fe3O4 and FeCr2O4 is indispensable. XANES uses the photoionization effect at the metal absorption edge in an aging product and accesses by this structural and chemical information. The current work uses XANES at the Fe-K and Cr-K absorption edge to identify various aging products grown as thin layers on alloys after short time aging experiments. A reaction chamber for combining high temperature oxidation experiments with surface sensitive X-ray absorption near edge structure spectroscopy will be introduced and first results of XANES on scales at high temperatures will be presented. T2 - ISHOC 2018 CY - Matsue, Japan DA - 22.10.2018 KW - Corrosion KW - Sulfidation KW - In situ KW - Diffraction KW - XANES PY - 2018 AN - OPUS4-47278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rütters, R. A1 - Fisher, S. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Maßmann, J. A1 - Ostertag-Henning, C. A1 - Lennard Wolf, J. A1 - Pumpa, M. A1 - Lubenau, U. A1 - Knauer, S. A1 - Jaeger, P. A1 - Neumann, A. A1 - Svensson, K. A1 - Pöllmann, H. A1 - Lempp, C. A1 - Menezes, F. A1 - Hagemann, B. T1 - Towards defining reasonable minimum composition thresholds – impacts of variable CO2 stream compositions on transport, injection and storage N2 - The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on: Corrosion of pipeline steel, pipeline network design and related transport costs, alteration of well bore cements, pressure evelopment and rock integrity, geochemical reactions, and petrophysical and geomechanical rock properties. All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein. The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for eachindividual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv)impurity combinations to be avoided. T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 CY - Online meeting DA - 15.03.2021 KW - Corrosion KW - Impurities KW - CO2 quality KW - Pipeline network KW - Whole-chain CCS scenario KW - Recommendations PY - 2021 AN - OPUS4-52419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rütters, H. A1 - Fischer, S. A1 - Le, Quynh A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Maßmann, J. A1 - Ostertag-Henning, C. A1 - Wolf, J. Lennard A1 - Pumpa, M. A1 - Lubenau, U. A1 - Knauer, S. A1 - Jaeger, P. A1 - Neumann, A. A1 - Svensson, K. A1 - Lempp, C. A1 - Menezes, F. A1 - Hagemann, B. T1 - Towards defining reasonable minimum composition thresholds – impacts of variable CO2 stream compositions on transport, injection and storage T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 N2 - The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on: Corrosion of pipeline steel, pipeline network design and related transport costs, alteration of well bore cements, pressure development and rock integrity, geochemical reactions, and petrophysical and geomechanical rock properties. All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein. The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided. T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 CY - Online meeting DA - 15.03.2021 KW - Corrosion KW - Impurities KW - CO2 quality KW - Pipeline network KW - Whole-chain CCS scenario KW - Recommendations PY - 2021 DO - https://doi.org/10.2139/ssrn.3816427 SP - 1 EP - 18 AN - OPUS4-52418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rütters, H A1 - Fischer, S A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Maßmann, J A1 - Ostertag-Henning, C A1 - Lennard Wolf, J A1 - Pumpa, M A1 - Lubenau, U A1 - Knauer, S A1 - Jaeger, P A1 - Neumann, A A1 - Svensson, K A1 - Pöllmann, H A1 - Lempp, C A1 - Menezes, F A1 - Hagemann, B T1 - Towards Defining Reasonable Minimum Composition Thresholds – Impacts of Variable CO2 Stream Compositions on Transport, Injection and Storage T2 - Proceedings of the 15th Greenhouse Gas Control Technologies Conference 15-18 March 2021 N2 - The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on: • corrosion of pipeline steel, • pipeline network design and related transport costs, • alteration of well bore cements, • pressure development and rock integrity, • geochemical reactions, and • petrophysical and geomechanical rock properties. All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein. The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided. T2 - The 15th Greenhouse Gas Control Technologies Conference CY - Online meeting DA - 15.03.2021 KW - Corrosion KW - Impurities KW - CO2 quality KW - Pipeline network KW - Whole-chain CCS scenario KW - Recommendations PY - 2021 DO - https://doi.org/10.2139/ssrn.3816427 SP - 1 EP - 18 PB - Elservier AN - OPUS4-52940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Wolf, Marcus A1 - Kranzmann, Axel T1 - Corrosion and corrosion fatigue of steels in downhole CCS environment - A summary JF - Processes N2 - Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60 °C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO₃ and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60 °C, brine: Stuttgart Aquifer and NGB, flowing CO₂: 30 L/h, +/- applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied. KW - Steel KW - High alloyed steel KW - Corrosion KW - Corrosion fatigue KW - Carbon capture and storage PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531391 DO - https://doi.org/10.3390/pr9040594 SN - 2227-9717 VL - 9 IS - 4 SP - 1 EP - 33 PB - MDPI CY - Basel AN - OPUS4-53139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja A1 - Wolf, Marcus A1 - Kranzmann, Axel T1 - Evaluating corrosion and corrosion fatigue behavior via laboratory testing techniques in highly corrosive CCS-environment T2 - Proceedings of the 15th Greenhouse Gas Control Technologies Conference 15-18 March 2021 N2 - In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO₂). T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 CY - Abu Dhabi, United Arab Emirates DA - 15.03.2021 KW - Steel KW - Supercritical CO2 KW - Pipeline KW - Corrosion KW - CO2-storage PY - 2021 DO - https://doi.org/10.2139/ssrn.3812193 SP - 1 EP - 11 PB - SSRN CY - Rochester, NY AN - OPUS4-53142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Wolf, M. A1 - Kranzmann, Axel T1 - Corrosion and Corrosion Fatigue of Steels in Downhole CCS Environment—A Summary JF - Processes N2 - Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60°C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO2-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO3 and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60°C , brine: Stuttgart Aquifer and NGB, flowing CO2: 30 L/h, +/- applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied. KW - Carbon capture and storage KW - Steel KW - High alloyed steel KW - Corrosion KW - Corrosion fatigue KW - CCS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523948 DO - https://doi.org/10.3390/pr9040594 VL - 9 IS - 4 SP - 594 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -