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Eingeladener Vortrag
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Comprehensive insights into the early stages of corrosion mechanisms provide fundamental knowledge to further understand and model long time material behaviour. The present work studies the early stages of combined oxidation and sulphidation of ferritic model alloys for time scales up to 250 h at 650 °C to observe the influence of chromium during the corrosion under SO2. Model alloys were used to focus on the reaction of the intended elements: Fe, Cr, S, and O. Pure iron simultaneously forms magnetite and iron sulphide in an early stage of corrosion, covered by a pure oxide layer after 100 h. Iron with 13 wt% Cr shows hematite and mixed Fe-Cr-oxides first, before sulphides nucleate in the inner corrosion zone. With increasing ageing time a magnetite layer is observed below the hematite layer. Quantitative phase fractions of all corrosion products observed were determined from cross section images. Characterization of the Fe13Cr corrosion scale by FIB revealed a highly porous structure in the inner corrosion zone where Cr-rich (Fe, Cr)-sulphides are present, and caused the scale to spall easily.
Basic research on the corrosive effect of flue gases has been performed at the BAM Federal Institute for Materials Research and Testing (Germany). Conditions at both high and low temperatures were simulated in specially designed experiments. Carburization occured in flue gases with high CO2 content and temperatures higher than 500 °C. In SO2 containing flue gases sulphur was detected in the oxide scale. At lower temperatures no corrosion was observed when gases with low humidity were investigated. Humidity higher than 1500 ppm was corrosive and all steels with Cr contents lower than 12% revealed corroded surfaces. At low temperatures below 10 °C a mixture of sulphuric and nitric acid condensed on metal surfaces. Acid condensation caused severe corrosion. Humidity, CO2, O2, and SO2 contents are the important factors determining corrosion. Below 300 °C acid condensation is the primary reason for corrosion. Low humidity and low temperatures are conditions which can be expected in the CO2 separation and treatment process. This work includes major conditions of the flue gas and CO2 stream in CCS plants and CCS technology.
Der Klimaschutz erfordert die Reduzierung des Ausstoßes von Kohlendioxid. Neue Kraftwerke mit Sauerstoffverbrennung und möglicherweise CO2-Abscheidung sollen eine Reduktion des CO2 im Bereich der Energietechnik ermöglichen. Die heute üblichen Hochtemperaturwerkstoffe werden anderen Umgebungsbedingungen ausgesetzt, und es sind andere Korrosionsraten und Korrosionsreaktionen zu erwarten. In diesem Beitrag werden die Kraftwerkstechnologien kurz vorgestellt und an einem Beispiel erläutert, dass die Oxidation an Luft mit der Oxidation in Wasser nicht direkt vergleichbar ist.
The CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, C02-corrosion of the injection pipe steels has to be given special attention when engineering CCSsites. To get to know the corrosion behaviour samples of the heat treated Steel 1.72252CrMo4, used for casing, and the stainless injection-pipe Steel 1.4034 X46Cr 13 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a C02-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. The isothermal corrosion behaviour obtained by mass gain of the steels in the gas phase, the liquid phase and the intermediate phase gives surface corrosion rates around 0.1 to 0.8 mm/year at ambient pressure and much lower about 0.02 to 0.2 mm/year at 100 bar where the C02 is in its supercritical state. Severe pit corrosion with pit heights around 4.5 mm are only located on the 42CrMo4 Steel. Main phase of the continuous complicated multi-layered carbonate/oxide structure is siderite FeCO} in both types of Steel.
The CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, CC>2-corrosion of the injection pipe steels has to be given special attention when engineering CCS-sites. To get to know the corrosion behaviour samples of the heat treated Steel 1.72252CrMo4, used for casing, and the stainless injection-pipe Steel 1.4034 X46Crl3 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CC>2-saturated synthetic aquifer environment similar to possible geological onshore CCS-sites in the northern German Basin. The isothermal corrosion behaviour obtained by mass gain of the steels in the gas phase, the liquid phase and the intermediate phase gives surface corrosion rates around 0.1 to 0.8 mm/year at ambient pressure and much lower about 0.02 to 0.2 mm/year at 100 bar where the CO2 is in its supercritical state. Severe pit corrosion with pit heights around 4.5 mm are only located on the 42CrMo4 Steel. Main phase of the continuous complicated multi-layered carbonate/oxide structure is siderite FeCCh in both types of Steel.
Dealing with first corrosion screening experiments to predict the reliability and safety of Germanys first Carbon Capture and Storage site in the northern Bassin of Germany, northwest of the Capital Berlin, laboratory experiments have been established to simulate the particular conditions at T=60 °C, highly saline aquifer water similar to 'Stuttgart Aquifer', but only at ambient pressure. With mounting 2 independent full 2-grade titanium autoclave systems (running up to 250 bar and 300 °C) pressures up to p=100 bar are possible. In 2010 a specific corrosion chamber of 2-grade titanium working up to 100 °C, flowing aqui fer water with different gas mixtures was designed to fit to a high cycle fatigue testing machine. Long term fatigue experiments simulating fatigue crack growth under corrosive environments will soon start. These experiments may not only help engineering a CCS site, but results can be used to improve the maintenance of geothermal energy production sites, especially moved parts such as pumps and shafts.
The combustion of coal in CO2-reduced Oxyfuel power plants requires creep resistant and corrosion
resistant materials, which can withstand high temperatures up to 600°C and CO2 rich atmospheres.
Among the heat resistant materials, the 9-12% chromium steels are proven to resist high wall
temperatures in conventional power plants and are suitable as membrane wall, superheaters and steam
piping.
During Oxyfuel combustion a flue gas is generated, which consists mainly of H2O (30 mol %) and
CO2 (70 mol %). The present paper is focused on the corrosion of 9-12% chromium steels under
oxyfuel conditions in a temperature range between 550 and 625°C.
Depending on Chromium content of the 9-12%chromium steels, carburization of the base material,
perlite formation and carbide formation were observed. Alloys with lower chromium content form a
non protective oxide scale with perlite at the scale-alloy interface. Steels with 12% chromium have a
small growing oxide scale with enlarged M23C6-particles at the scale-alloy interface. The carburization
of the base material is found to be increased for the 9% Cr-steel. Higher pressure of the flue gas results
in the formation of less resistant scales and cause accelerated carburization of the base materials.
However, the carburization has an impact on the mechanical properties at the surface and leads to an
embrittlement, which is deleterious during thermal cycling.
Oxidation kinetics, phase analysis of the scale (transmission electron microscope) and carburization
depths (microprobe) of the base materials are presented.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
During the compression of emission gasses into deep geological layers (Carbon Dioxide Capture and Storage, CCS) CO2-corrosion will become a relevant safety issue. The reliability of the steels used at a geological onshore CCS-site in the Northern German Bassin 42CrMo4 (1.7225, AISI 4140) used for casing, and the injection pipe steels X46Cr13 (1.4034, AISI 420 C), X20Cr13 (1.4021, AISI 420 J) as well as X35CrMo17 (1.4122) is demonstrated in laboratory experiments. Samples were kept in a synthetic aquifer environment at T = 60 °C. This corrosive environment is then saturated with technical CO2 at a flow rate of 3 l/h. Microstructures were characterized by X-ray diffraction, light microscopy, scanning electron microscopy, and energy dispersive X-ray analysis, after a series of heat treatments (700 h to 2 years). The non-linear isothermal surface corrosion behaviour of the steels reveals surface corrosion rates around 0.10.8 mm/year, when obtained by mass gain. Severe pit corrosion (pit heights ca. 4.5 mm) are only located on the injection pipe steels. Main phases of the continuous scales are siderite FeCO3 and goethite α-FeOOH. The formation of the non-protective layer is likely to form via a
transient Fe(OH)2-phase.