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Eingeladener Vortrag
- nein (2)
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.
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.
When engineering a Carbon Capture and Storage site (CCS) local corrosion (pitting) of the injection pipe steel may become an issue when emission gasses from oxyfuel power plants are compressed into deep geological layers. This highly corrosive environment arises when the flue gasses, mainly composed of CO2 , are injected into saline aquifer water. Immediately carbonic acid is formed causing corrosive attack of the injection steels. The influence of heat treatment on the local corrosion resistance was demonstrated in laboratory experiments at 60 °C and ambient pressure for three steels X46Cr13 (1.4034), X20Cr13 (1.4021) and X5CrNiCuNb16-4 (1.4543) under a similar liquid corrosive environment as found at a geological onshore CCS-site in the Northern German Bassin.
We present a new method for the complete three-dimensional (3D) calibration of scanning probe microscopes (SPM) and other high-resolution microscopes, e.g., scanning electron microscopes (SEM) and confocal laser scanning microscopes (CLSM), by applying a 3D micrometre-sized reference structure with the shape of a cascade slope-step pyramid. The 3D reference structure was produced by focused ion beam induced metal deposition. In contrast to pitch featured calibration procedures that require separate lateral and vertical reference standards such as gratings and step height structures, the new method includes the use of landmarks, which are well established in calibration and measurement tasks on a larger scale. However, the landmarks applied to the new 3D reference structures are of sub-micrometre size, the so-called 'nanomarkers'. The nanomarker coordinates are used for a geometrical calibration of the scanning process of SPM as well as of other instrument types such as SEM and CLSM. For that purpose, a parameter estimation routine involving three scale factors and three coupling factors has been developed that allows lateral and vertical calibration in only one sampling step. With this new calibration strategy, we are able to detect deviations of SPM lateral scaling errors as well as coupling effects causing, e.g., a lateral coordinate shift depending on the measured height position of the probe.
Oxidation of a single crystal nickel-base superalloy at 950 °C - a kinetic and microstructure study
(2008)
The nickel-base single crystal alloy investigated is a widely used material for first and second row blades in stationary gas turbines. Nickel-base superalloys are especially designed to resist high temperature oxidation by process gases. To determine this high temperature behaviour oxidation testing was carried out using samples cut perpendicular to (001)-direction. Microstructures were characterized by X-ray diffraction XRD, Light Microscopy LM, Scanning Electron Microscopy SEM, and X-ray energy dispersive spectroscopy (EDS), after a series of heat treatments (950 °C, 0 h - 1000 h). Mass gain and the respective thicknesses of the different oxide layers were measured to determine oxidation kinetics. In general, the isothermal oxidation behaviour at 950 °C, as defined by weight gain, follows a parabolic law with a parabolic rate constant around 1.4 · 10-2 mg2/(cm4 · h). A short incubation time is followed by the constitution of a multi-layered oxide scale. The oxide scale consists of a three layer structure. An outer scale contains a Ti-bearing thin film associated as TiO2 and NiTiO3 but mostly Cr attributed to Cr2O3, (Ni/Co)Cr2O4 beside NiTaO4. This outer scale is connected to a discontinuous layer of inner oxidation consisting mainly of Al2O3, which is followed by an area of γ´-depletion within the base material.
The process chain for Carbon Capture and Sequestration (CCS) includes tubing for injection of CO2 into saline aquifers. The compressed CO2 is likely to contain specific impurities; small concentrations of SO2 and NO2 in combination with oxygen and humidity are most harmful. In addition, CO2 saturated brine is supposed to rise in the well when the injection process is interrupted. The material selection has to ensure that neither CO2 nor brine or a combination of both will leak out of the inner tubing. In this comprehensive paper the investigated materials range from low-alloy steels and 13% Cr steels up to high-alloy materials. Electrochemical tests as well as long term exposure tests were performed in CO2, in brine and combination of both; pressure was up to 100 bar, temperature up to 60 °C. Whereas the CO2 stream itself can be handled using low alloy steels, combinations of CO2 and brine require more resistant materials to control the strong tendency to pitting corrosion. The corrosion behavior of heat-treated steels depends on factors such as microstructure and carbon content. For different sections of the injection tube, appropriate materials should be used to guarantee safety and consider cost effectiveness.
In corrosive environments such as CCS bore holes or geothermal power plants the materials loaded cyclically are also exposed constantly to the highly corrosive hot thermal water. The lifetime reduction of (X46Cr13, AISI 420C) is demonstrated in in-situ-laboratory experiments (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 Nl/h, CO2). S-N plots, micrographic-, phase-, fractographic- and surface analysis were applied to obtain sustainable information on the corrosion fatigue behavior. Maximum number of cycles (here 12.5 x 106 cycles to failure) is reached at σa =173 MPa. No typical fatigue strength exists and passive corrosion fatigue is most likely failure cause.