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- Transmission electron microscopy (3)
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- Aluminiumoxid (2)
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Organisationseinheit der BAM
The transformation of doped or seeded pseudoboehmite to corundum was studied by combining thermal analysis, X-ray diffraction, transmission electron microscopy, and electron paramagnetic resonance spectroscopy. The temperature of phase transformation to corundum was lowered by about 130 °C when Fe3+ or corundum seeds were added to the sols. Action of Fe3+ ions depends on the actual degree of thermally induced transformation of pseudoboehmite via transition aluminas to corundum and the ability of these alumina phases to incorporate Fe3+ ions. These ions tend to aggregate with increasing iron concentration of the alumina phases and can work as nucleation centers. Small (not, vert, similar20 nm) corundum particles act as active nucleation sites whereas larger grains (200400 nm) also present in the samples are less effective. For the first time trapping and stabilization of NO2 molecules in transition aluminas formed by a solgel route was shown.
Future coal power plants will in case of oxyfuel combustion be operated with altered atmospheres. Hence, corrosion attack might become more severe and steels have to be protected. An alumina-sol was used to coat X20CrMoV12-1 (X20) with alumina to test the protection. Testing was performed at 600 °C in flowing H2O–CO2–O2 and static laboratory air for 1000 h. Oxidation under air is minor compared to exposure in oxyfuel atmosphere. In both cases a multilayered oxide (hematite, magnetite, spinel) was formed on uncoated steels. Carburization appeared on uncoated X20 in H2O–CO2–O2. The coating demonstrates a high protection.
Up to ~ 3 µm thick alumina coatings on corundum ceramic, sodalimesilica glass and Inconel718 were produced from mixtures of boehmite sols and corundum suspensions.
Transmission electron micrographs in combination with electron diffraction and energy dispersive X-ray spectroscopy served to identify crystallographic phases and to characterize the microstructure of the coatings. Using corundum ceramic as substrate the initially deposited boehmite transforms via transition aluminas to corundum while heating to 1200 °C. In the cases of glass and Inconel718 thermal treatments up to 520 °C and 1100 °C, respectively, cause diffusion of ions from the substrates into the coatings. Thus additional oxide phases were formed.
All coatings are free of cracks or delaminations and do not show any directed crystal growth.
Modified Yoldas sols can be used to prepare crack-free well adherent layers on different substrate materials such as sodalime glass, corundum and metal (IN-718). These layers having thicknesses of 0.6 µm are strain tolerant and withstand thermal cycling between 810 °C and room temperature. Introducing alpha-Al2O3 filler particles into modified Yoldas sols allows the preparation of thicker layers of 1.6 µm, which as well can be thermally cycled without noticeable delaminations. Chemical bonding seems to be the predominant layer bonding mechanism.
Alumina coatings with differing phase compositions were deposited on Inconel-718 (IN-718) Ni-base
superalloy substrates using solgel processing. Mass gain measurements served for studying the oxidation
behavior of coated metal surfaces if exposed to 800°C and 900°C for up to 4000 h in static air. Itwas found, that
alumina coatings significantly reduce the oxidation related mass gain of IN-718 even after heating to 900°C
for 4000 h. Transmission electron microscopy (TEM) studies revealed diffusion of elements from the metal
substrate (IN-718) into the alumina coatings and to a much lower degree from the coating into the
substrate. These diffusion processes are greatly influenced by the phase composition of the coatings, especially
by the presence of alpha-alumina.
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.
Diffusion of Cr, Fe, and Ti ions from Ni-base alloy inconel-718 into a transition alumina coating
(2012)
Heat treating metals at high temperatures trigger diffusion processes which may lead to the formation of oxide layers. In this work the diffusion of Cr, Fe and Ti into an alumina coating applied to Inconel-718 is being investigated. Mass gain measurements, UV–vis spectroscopy and transmission electron microscopy were applied in order to study the evolution of the diffusion process. It was found that mainly Cr as well as minor amounts of Fe and Ti are being incorporated into the alumina coating upon prolonged heat treatment at 700 °C. It could be shown that alumina coatings being void of Cr have the same oxidation related mass gain as uncoated samples. However, incorporation of Cr into the alumina coating decreased their mass gain below that of uncoated substrates forming a Cr oxide scale only.
The need for a more efficient coal power plant generation (e.g. oxyfuel technology) results in modified process parameters and enhanced corrosion. To reach the necessary service life of high temperature parts protective coatings may be a sufficient technical solution. A modified Yoldas sol (Al2O3 based) was used to coat X20CrMoV12-1 by spin coating. After appropriate heat treatments transition alumina coatings being about 400 nm thick were obtained. Oxidation studies were carried out in laboratory air at temperatures up to 650 °C for up to 500 h exposure time. In case of the uncoated sample a rough oxide layer formed on the surface and a remarkable weight gain (2.62 mg/cm²) were detected. The sol–gel alumina layer (mainly δ-Al2O3) demonstrated a high protection, i.e. a very low weight gain (0.05 mg/cm²). Diffusion of alloying elements into the coating was observed. No indication of spallation of the coating occurred. Local defects (2 µm–30 µm) in the coating led to the formation of iron-oxide islands.