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Alumina thin films
(2016)
This chapter gives an overview over preparation, properties and applications of alumina thin films. The preparation of polymeric and colloidal alumina sols and their deposition on diverse substrate materials with different geometries are described first. Consideration of properties (surface tension, particle size, viscosity, aging of the sols and their optimization by using certain additives) is included, too. A description of post-treatments of the coatings, which initiate phase transformations and also determine their microstructure, completes the part on coating preparation. Data on adhesion, thickness, surface roughness and mechanical, textural as well as optical properties of alumina thin films are provided in a further paragraph. In a third main part experience concerning possible applications, such as (i) membranes for catalysis, separation and filtration, (ii) barrier layers against electrochemical and high temperature corrosion or inter-diffusion of ions between different phases, (iii) mechanical protection, (iv) sensor construction, (v) improvement of optical properties, as well as (vi) achieving water repellency is summarized.
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.
The objective of the present work was the investigation and demonstration of the potential of sol-gel alumina layers as corrosion protection of commercial power plant steels under oxyfuel conditions. The starting points of this work were modified Yoldas-sols which were developed in the BAM-department 5.6. These sols were suitable for the spin-coating method only. The application of coatings on tubes by spin-coating is impossible. Therefore, the chemical composition of the modified Yoldas-sol had to be adapted to the dip- and spray-coating techniques.
Exclusively the sol with the composition s-0.52-6-1.5 with a nitrate/aluminium ratio of 0.52; a solid content of 6 wt.% and a PVP (binder) content of 1.5 wt.% could fulfill the necessary criteria: long-term stability; formation of a dense, crack-free and well adhered layer on polished metal surfaces; as well as high protective abilities against corrosion in H2O-CO2-O2-SO2.
The commercial power plant steel X20CrMoV12-1 (X20) and the steel X12Cr13 were successfully coated with the sol s-0.52-6-1.5 by means of the dip-coating method. An at least 400 nm thick alumina layer (δ-Al2O3) is necessary to ensure the corrosion protection of these steels. The corrosion of the coated samples compared to that of the uncoated ones was significantly reduced, even after 1000 h of exposure in a H2O-CO2-O2-SO2 atmosphere at 600°C. Sulfur and carbon were not detected at the substrate surface or beneath the coating. Hence the transport of the flue gas components SO2 and CO2 into as well as through the alumina layer could be hindered. The diffusion of the alloying elements (Cr, Mn, Si) into the alumina layer resulted in the formation of mixed oxides like δ-(Al,Cr)2O3. Formation of such phases considerably contributed to the corrosion protection.
The long-term stability of the sol s-0.52-6-1.5 and the high protective abilities of the alumina layer on commercial power plant steels provide a good basis for an industrial application.
The martensitic steels X30CrMoN15-1 and 100Cr6 did not show any hydrogen enhanced wear in sliding friction tests against alumina balls in hydrogen gas environment. However, depending on the purity of the environment, unexpected high wear occurred at the alumina ball. The results of a tests series with a broad variation of test parameters are presented.
Sliding wear of martensitic steels in hydrogen – X30CrMoN15-1 and 100Cr6 – the role of water traces
(2016)
Initially the primary objective of the project has been the investigation of the influence of gaseous hydrogen on the wear of martensitic steels under heavy tribological stress. As a counter body an Al2O3 ball has been used because the material is inert and hard so that a low amount of wear was expected. If only the gas pressure is responsible for the absorption of hydrogen from the gas to pure α-iron it would require 15·105 MPa (~15 Mbar) to press 1 ppm into the material.
In the test series the Al2O3 balls showed in N2 and H2 atmosphere a higher wear compared to aerial experiments which showed a smaller wear track and a severer wear for the disc. Because of scattering and thereof following investigations it was shown that hydrogen has no noticeable influence but water traces in the gas are manipulating the outcome of the tests distinctly.
The wear rates of self-amted alumina couples show that friction as well as wear is largely determined by the above mentioned hydro-thermal conditions. The presence of water and ist amount available in the surrounding system either in liquid or in gaseous from plays a key role for friction and wear behavior and cabe benefical for the tribological profile of steam degradation resistant materials. Hot steam enhances the tribo-chemical formations of oxides and hydroxides on MgO-ZrO2, alumina and antimony impregnated carbon.
The wear rates of self-mated alumina couples show that friction as well as wear is largely determined by the above-mentioned hydro-thermal conditions. The presence of water and its amount available in the surrounding system either in liquid or in gaseous form plays a key role for friction and wear behavior and can be beneficial for the tribological profile of steam degradation resistant materials. Hot steam enhances the tribo-chemical formations of oxides and hydroxides on MgO-ZrO2 alumina and antimony impregnated carbon.
In the present work an approach is presented which combines various aspects of the former models with probability considerations. It is used to simulate the impact of more than one billion Alumina particles onto a steel substrate. This approach permits the simulation of an entire erosion experiment on an average PC within about six hours.
Powder based Additive Manufacturing (AM) processes are widely used for metallic and polymeric materials, but rarely commercially used for ceramic materials, especially for technical ceramics. This seemingly contradicting observation is explained by the fact that in powder based AM, a dry flowable powder needs to be used. Technical ceramics powders are in fact typically very fine and poorly flowable, which makes them not suitable for AM. The layerwise slurry deposition (LSD) is an innovative process for the deposition of powder layers with a high packing density for powder based AM. In the LSD process, a ceramic slurry is deposited to form thin powder layers, rather than using a dry powder This allows the use of fine powders and achieves high packing density (55-60%) in the layers after drying. When coupled with a printing head or with a laser source, the LSD enables novel AM technologies which are similar to *Denotes Presenter 42nd International Conference & Exposition on Advanced Ceramics & Composites 127 Abstracts the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder bed. The LSD -3D printing, in particular, offers the potential of producing large (> 100 mm) and high quality ceramic parts, with microstructure and properties similar to traditional processing. This presentation will give an overview of the milestones in the development of this technology, with focus on the latest results applied both to silicate and to technical ceramics.
Dielectric strength testing of ceramics is simple and yet challenging. The execution of a breakthrough voltage measurement of a given sample is fast and straightforward. ASTM D149 describes the standardized procedure. But, there are versatile effects of test conditions and sample properties that affect the result of such a measurement. As one example, ASTM D149 allows different sizes of test electrodes and does not unambiguously prescribe the condition of the electrodes. Thus, different electrode configurations are used in the field. We conducted several test series on alumina samples to comprehensively quantify the effect of test conditions and sample properties on dielectric strength results. In our study, testing of alumina substrates using different electrode configurations resulted in differences of mean values of up to 20%. Further test series on alumina focused on the effect of voltage ramp rate. The results are complemented by calculations of failure probability at different voltage levels and corresponding withstand voltage tests. We conclude that a communication and comparison of single dielectric strength values is insufficient and may be misleading. A meaningful comparison of dielectric strength studies from different sources requires a thorough consideration of test conditions.