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Oxidation of a Fe –13Cr alloy under water vapor at 600°C produced a zone of nano-sized precipitation underneath the outside scale formed by iron oxides and Fe–Cr spinel. The majority of the spinel layer shows a fixed orientation relationship to the ferritic matrix: {1 0 0}α || {1 0 0}sp & <0 1 1>α || <0 0 1>sp . However, also the discovered precipitated particles are characterized by the same crystallographic orientation relationship to the respective ferritic parent grain. The habit of the precipitates is best described by a lath morphology with their main axis parallel to <1 0 0> of ferrite. Energy dispersive X-ray spectroscopy (EDX) and electron backscatter diffraction (EBSD) in scanning electron microscope (SEM) have been applied to characterize the oxide layer in micrometer scale. The clearly smaller precipitates were subsequently investigated by transmission electron microscopy (TEM). Specimens have been prepared by focused ion-beam (FIB) milling at an area previously characterized by EBSD. They cover the ferritic base material, but mainly the precipitation zone and the Fe–Cr spinel layer. Energy filtered selected area diffraction (SAD) in the conventional (C)TEM and high-angle annular dark field (HAADF) imaging in the scanning (S)TEM mode were employed in the characterization of the specimens.
Microstructure, smoothening effect, and local defects of alumina sol-gel coatings on ground steel
(2017)
Porous alumina films with thicknesses of a few microns were prepared via a dip-coating technique on steel P92. The coating is shown to protect the steel against massive corrosion, which is typical in the hot reactive environment of coal fired power plants. To mimic real conditions ground steel plates were coated with a boehmite-sol. This leads to an overall smoothing of the formerly rough surface. In the following short annealing step the inner porous construction with worm-like particles consisting of nano-crystallites and amorphous alumina is formed. Due to the simultaneous diffusion of chromium and iron ions out of the bulk steel material into the porous alumina coating, a dense interface with satisfactory adhesion is formed. However, the film exhibits few local defects like cracks or dense alumina nodules caused by steep edges in the ground surface or agglomeration of boehmite-sol components, respectively. Cracks especially have to be avoided. This problem can be overcome so far by slight modifications in the sol preparation process and surface treatment of the substrates. Nevertheless the results demonstrate the potential of sol-gel based alumina coatings as a time- and cost-saving protection type for commercial steel P92.
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.