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Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C
(2018)
Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far.
In order to reduce CO2 emissions fossil fuelled power stations with high combustion efficiency are being developed. The increase of the operating temperature, a common way to improve combustion efficiency, leads to enhanced corrosion of heat exchange steel tubes in the power plants. Within the framework of the European project “Production of Coatings for New Efficient and Clean Coal Power Plant Materials” (POEMA)", high temperature corrosion protection coatings are now under investigation.
Thin porous sol-gel alumina films are promising candidate coating materials. Coatings were prepared by applying boehmite sols on grinded steel P92 and subsequent heat treatments at temperatures up to 650 °C. Thus a porous layer of worm-like particles was formed consisting of nano-crystallites and amorphous alumina. A dense interface with satisfying adhesion resulted from diffusion of chromium and iron ions out of the steel into the porous coating. However, the film locally exhibited some cracks caused by steep edges in the grinded steel surface. An appropriate substrate pretreatment should avoid this problem.
The protection of the steel relies on the barrier function of the alumina coating and the formation of a dense chromia layer at the steel surface.
Al2O3 has been widely used as a coating in industrial applications due to its excellent chemical and thermal resistance. Considering high temperatures and aggressive mediums exist in geothermal systems, Al2O3 can be a potential coating candidate to protect steels in geothermal applications. In this study, γ-Al2O3 was used as a coating on martensitic steels by applying AlOOH sol followed by a heat treatment at 600 °C. To evaluate the coating application process, one-, two-, and three-layer coatings were tested in the artificial North German Basin (NGB), containing 166 g/L Cl−, at 150 °C and 1 MPa for 168 h. To reveal the stability of the Al2O3 coating in NGB solution, three-layer coatings were used in exposure tests for 24, 168, 672, and 1296 h, followed by surface and cross-section characterization. SEM images show that the Al2O3 coating was stable up to 1296 h of exposure, where the outer layer mostly transformed into boehmite AlOOH with needle-like crystals dominating the surface. Closer analysis of cross-sections showed that the interface between each layer was affected in long-term exposure tests, which caused local delamination after 168 h of exposure. In separate experiments, electrochemical impedance spectroscopy (EIS) was performed at 150 °C to evaluate the changes of coatings within the first 24 h. Results showed that the most significant decrease in the impedance is within 6 h, which can be associated with the electrolyte penetration through the coating, followed by the formation of AlOOH. Here, results of both short-term EIS measurements (up to 24 h) and long-term exposure tests (up to 1296 h) are discussed.
Sol-Gel-Aluminiumoxidschichten für den Oxidationsschutz von Hochtemperaturlegierungen, Teil 2
(2009)
Sol-Gel-Aluminiumoxidschichten für den Oxidationsschutz von Hochtemperaturlegierungen, Teil 1
(2009)
Alumosols in combination with well dispersed corundum were successfully used to form up to 2.5 ìm thick coatings on the Ni-base alloy SC16. These coatings withstood heat treatments at 700 °C in a water vapour containing atmosphere. The heat treatment caused formation of delta-alumina in the coating and diffusion of chromium and titanium into the coating.
The suitability of an Al2O3 coating for corrosion protection on X20Cr13 was evaluated in various artificial geothermal brines, focusing on the influence of different pH (4, 6 and 8) and their chemical compositions on the coating properties. All experiments were performed in the laboratory using autoclaves at 150 ◦C and 1 MPa in deaerated condition for 1 and 7 days. Results showed that the pH of geothermal waters is the most detrimental factor in the transformation of ɣ-Al2O3 and its protective abilities. Delaminations were found in the Coating exposed to geothermal brines with pH 4. FTIR spectra indicated a transformation of ɣ-Al2O3 to boehmite AlOOH after exposure to pH 4 and 6, and bayerite Al(OH)3 was formed after exposure to pH 8. Different Crystal structures of the hydrated Al2O3 also contribute to the stability of the coatings, observed by the SEM- EDX of the surface and cross-section of coatings. This study indicated that ɣ-Al2O3 sol-gel coating presents a promising aspect of corrosion protection in geothermal environment with a neutral pH.