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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).
During carbon sequestration the CO2-induced corrosion of injection pipe steels is a relevant safety issue when emission gasses are compressed into deep geological layers. The reliability of the high alloyed steel X35CrMo17 suitable as injection pipe for the geological onshore CCS-site (Carbon Capture and Storage) in the Northern German Basin, is demonstrated in laboratory experiments in equivalent corrosive environment (T = 60 °CC, p = 1–100 bar, aquifer water, CO2-flow rate of 9 L/h, 700–8000 h exposure time). Corrosion kinetics and microstructure were characterized and compared to other potential injection pipe steels (42CrMo4, X46Cr13, X20Cr13 and X5CrNiCuNb16-4).
X5CrNiCuNb16-4 has been proven to be sufficient resistant in corrosive environments, but shows rather unusual corrosion behaviour in CCS environment. Therefore a series of 30 specimens was tested at stress amplitudes between 150 MPa and 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ∼ 30 Hz). Due to the rather heterogeneous fine machined surfaces (Rz=4) the specimens are comparable with prefabricated parts. X5CrNiCuNb16-4 reached the maximum number of cycles (10 x 106) at a stress amplitude of 150 MPa and lies 60% below the stress amplitude measured in air. The scatter range TN = 1:34 is disproportionately large. Although the fracture surface exhibited the typical striations and corroded surface areas no significant differences were found. The hardness was found to be homogeneous in all specimens tested at 335 HV10. Non-metallic inclusions were found within the microstructure, but no correlation could be found between the inclusions and early rupture. Still specimens that showed inclusions at the fracture surface and its cross section endured lower number of cycles. Additionally Aluminium was analysed in specimens with low number of cycles and may be cause for early rupture during corrosion fatigue tests. These findings reveal a very high sensitivity on a homogeneous microstructure upon the corrosion and corrosion fatigue behaviour of X5CrNiCuNb16-4 and needs to be taken into account when regarding this steel as pipe steel during injection of CO2 into saline aquifers.
Unusual Corrosion Behavior of 1.4542 Exposed a Laboratory Saline Aquifer Water CCS-Environment
(2017)
Differently heat treated coupons of 1.4542 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. Surface corrosion layers are homogeneous but unusually discontinuously ellipsoidal. After 8000 h at 100 bar maximum corrosion rate in the liquid phase is approximately 0.014 mm/year, with normalizing providing best corrosion resistance and approximately 0.003 mm/year in the supercritical phase where hardening+tempering at 670 °C leads to lowest corrosion rates.
Samples of differently heat treated high alloyed stainless injection-pipe steels AISI 420 X46Cr13, AISI 420J X20Cr13 as well as X5CrNiCuNb16-4 AISI 630 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CO2- saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Corrosion rates and scale growth are lowest after long term exposure for steels hardened and tempered at 600 to 670 °C and pits - indicating local corrosion- decrease in diameter but increase in number as a function of carbon content of the steel. Martensitic microstructure is preferred with respect to this particular CCS-site.
During carbon dioxide storage technology (carbon capture and storage, CCS) components are exposed to a corrosive environment and mechanical stress, which results in corrosion fatigue and inevitably followed by the a lifetime reduction of these components. In order to gain knowledge upon the corrosion fatigue strength of materials, Samples of high alloyed stainless injection-pipe steels AISI 420 X46Cr13, and X5CrNiCuNb16-4 AISI 630 were tested in a at T=60 °C and ambient pressure in a CO2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Therefore a corrosion chamber applied to a resonant testing machine allowing for “in situ” test conditions was designed and successfully tested. In-situ tension compression experiments were established using a resonant testing machine at a frequency as low as 30 – 40 Hz. In addition technical CO2 was introduced into the closed system at a rate close to 9 L/h to keep stable environmental conditions. Simultaneously electrochemical testing was performed to get information on failure causes and the mechanism of failure during the injection of CO2 into deep geological layers. S-N plots, micrographic analysis, and surface analysis of the fracture surface were applied to obtain sustainable information on the corrosion fatigue behavior of injection pipe steels. Samples used have a surface roughness of Rz = 4, to simulate technically machined surfaces. X46Cr13 reached the maximum number of cycles (12.5 x 106) at a stress amplitude of 173 MPa. X5CrNiCuNb16-4 reached the maximum number of cycles (10 x 106) at a stress amplitude at 150 MPa. The scatter range of X5CrNiCuNb16-4 is very high (1:34); by comparison the scatter range of X46Cr13 is only 1:3.5.
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.
In geothermal power plants the materials used in pumps are loaded cyclically and
exposed constantly to the highly corrosive hot thermal water. The lifetime reduction
of AISI 420C (X46Cr13, 1.4034) is demonstrated in in-situ-laboratory experiments
(T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/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 may be identified as failure
cause.
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 CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, CO2-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 X46Cr13 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 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 CO 2 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 3 in both types of steel.