WO2020233832A1 - Verfahren zum aufbringen einer beschichtung auf eine oberläche eines mullitmaterials, mullitmaterial mit einer beschichtung und gasturbinenbauteil - Google Patents
Verfahren zum aufbringen einer beschichtung auf eine oberläche eines mullitmaterials, mullitmaterial mit einer beschichtung und gasturbinenbauteil Download PDFInfo
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- WO2020233832A1 WO2020233832A1 PCT/EP2020/000096 EP2020000096W WO2020233832A1 WO 2020233832 A1 WO2020233832 A1 WO 2020233832A1 EP 2020000096 W EP2020000096 W EP 2020000096W WO 2020233832 A1 WO2020233832 A1 WO 2020233832A1
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- WIPO (PCT)
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- aluminum oxide
- mullite material
- containing layer
- mullite
- layer
- Prior art date
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4529—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/0054—Plasma-treatment, e.g. with gas-discharge plasma
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/455—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction
- C04B41/4558—Coating or impregnating involving the chemical conversion of an already applied layer, e.g. obtaining an oxide layer by oxidising an applied metal layer
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5031—Alumina
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
- C04B41/5338—Etching
- C04B41/5346—Dry etching
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
- F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
- F01D5/12—Blades
- F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
- F01D5/288—Protective coatings for blades
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02C—GAS-TURBINE PLANTS; AIR INTAKES FOR JET-PROPULSION PLANTS; CONTROLLING FUEL SUPPLY IN AIR-BREATHING JET-PROPULSION PLANTS
- F02C7/00—Features, components parts, details or accessories, not provided for in, or of interest apart form groups F02C1/00 - F02C6/00; Air intakes for jet-propulsion plants
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
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- F05D2220/00—Application
- F05D2220/30—Application in turbines
- F05D2220/32—Application in turbines in gas turbines
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- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
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- F05D2230/00—Manufacture
- F05D2230/90—Coating; Surface treatment
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- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
- F05D2300/00—Materials; Properties thereof
- F05D2300/20—Oxide or non-oxide ceramics
- F05D2300/21—Oxide ceramics
- F05D2300/2112—Aluminium oxides
Definitions
- the invention relates to a method for applying a coating to a surface of a mullite material, a mullite material with a coating and a gas turbine component.
- mullite In modern gas turbines, materials containing silicon and aluminum are used in the area of the combustion chamber as combustion chamber bricks and also for other gas turbine components. These materials are mostly referred to as mullite, although in addition to phases of actual mullite with the chemical composition 3 (Al 2 O) 3 x 2 (SiO 2 ), they also contain phases of other Al 2 O 3 -SiO 2 compounds, but also phases of may contain pure Al 2 O 3 in corundum structure (aA ⁇ Oa). In addition, many ceramic fiber composite materials contain fibers containing mullite. In the following, the term “mullite material” is therefore used for all materials containing Al 2 O 3 —SiO 2 , right through to materials that consist almost exclusively of Al 2 O 3. The term mullite material also includes so-called Ox-Ox materials which are alumina-based ceramic matrix composite materials
- FIG. 1 shows an optical microscope image of a section of a mullite material, in which different phases, which can occur in different grain sizes, are identified.
- the mullite material has excellent mechanical strength and chemical stability even at very high temperatures, as can occur in the area of a combustion chamber of a turbine.
- mullite materials have the disadvantage that they are attacked by hot water vapor, because this can form volatile compounds with the silicon contained in the mullite material.
- the consequence of this is that because of the loss of silicon from the surface, for example the combustion chamber bricks or another component made of mullite material, particles can be released from the mullite material because they lose their adhesion and become detached. These detached particles lead to wear of the turbine blades and other components such as B. of guide ring segments in the following turbine area.
- the object of the present invention is to provide a coating method and a coating with which the disadvantages described above can at least be reduced.
- Another problem is the adaptation of the layer material to the mullite material in such a way that a chemical bond is made possible.
- the different phases of the mullite material also have a negative effect in this regard, since different chemical reactions would have to take place in each case.
- the current application methods for the protective layers by means of spraying in order to achieve good adhesion, have a heating step which is intended to cause diffusion of elements in the boundary area between the mullite material and the sprayed-on protective layer. It is known, however, that at least one component of the mullite material, namely corundum, is a good diffusion barrier and thus prevents the common way of improving adhesion via a diffusion process.
- a method according to the invention for applying a coating to a surface of a mullite material includes pretreating the surface of the mullite material by means of a plasma-chemical process in which molecular hydrogen is excited in such a way that plasma-activated hydrogen, e.g. B. atomic hydrogen and / or ionized hydrogen molecules, and an application of an aluminum oxide-containing layer by means of a PVD process on the pretreated surface of the mullite material.
- plasma-activated hydrogen e.g. B. atomic hydrogen and / or ionized hydrogen molecules
- mullite material represents the substrate on whose surface the coating is applied after pretreatment.
- the coating can have further layers, e.g. B. Adhesive layers, cover layers, thermal insulation layers.
- the aluminum oxide-containing layer is preferably applied directly, that is to say without intermediate layers, to the pretreated surface of the mullite material.
- the mullite material To pretreat the surface of the mullite material, it is subjected to a plasma-chemical process in a vacuum (pressure range between 0.001 mbar and 1 mbar, preferably between 0.05 mbar and 0.1 mbar). In this plasma-chemical process, molecular hydrogen is excited in such a way that atomic hydrogen and ionized hydrogen molecules are created.
- a vacuum pressure range between 0.001 mbar and 1 mbar, preferably between 0.05 mbar and 0.1 mbar.
- This plasma removes silicon very gently and only in the uppermost atomic layers of the mullite material from the silicon-containing phases of the mullite material by forming volatile Si — H compounds. These are then pumped out of the vacuum using a pump system. At the same time, impurities such as carbon, hydrocarbons or other elements are deposited on the pure Al-O- Phases and in all other areas of the surface of the multi-material removed and pumped out.
- a pretreated surface of the mullite material is obtained which essentially only has only a-Al 2 O, 3 that is aluminum oxide with a corundum structure.
- the surface of the mullite material is pretreated by means of the plasma-chemical process
- infiltration of the surface with an aluminum-containing material e.g. B. YAG (yttrium aluminum garnet)
- an aluminum-containing material e.g. B. YAG (yttrium aluminum garnet)
- the porosity of the surface can advantageously be reduced by at least partially filling existing pores with the aluminum-containing material.
- a more homogeneous surface is achieved, so that the subsequently applied aluminum oxide-containing
- the method according to the invention is also suitable for applying a coating to the surface of a material which has previously been infiltrated with an aluminum-containing material.
- Both PVD processes use a target from which material is removed and deposited on the surface of the mullite material.
- the target comprises aluminum and optionally other elements, such as. B. chromium, titanium, hafnium, yttrium, erbium, silicon and / or zirconium, which should be included in the layer to be applied.
- B. chromium, titanium, hafnium, yttrium, erbium, silicon and / or zirconium which should be included in the layer to be applied.
- the aluminum oxide-containing layer can be applied from an aluminum oxide-containing target by means of high-frequency sputtering.
- the aluminum oxide-containing layer is preferably applied to the pretreated surface of the mullite material by means of reactive cathodic spark evaporation, with the target material being evaporated which is connected as the cathode in the spark evaporation.
- the evaporation takes place in a vacuum under controlled oxygen partial pressure, which can be adjusted by an appropriate oxygen gas flow.
- the application of the aluminum oxide-containing layer to the pretreated surface of the mullite material is preferably carried out at a substrate temperature in the range between 550 ° C. and 650 ° C., particularly preferably at a substrate temperature of 600 ° C.
- the temperature can also be lowered below 300 ° C. or the layer can also be applied at higher temperatures.
- PVD processes advantageously enable the application of a homogeneous aluminum oxide-containing layer in just one process step.
- Layer thicknesses in the range between 0.5 ⁇ m and 50 ⁇ m can be achieved with high accuracy.
- the reactive cathodic spark evaporation is also characterized by a high level of robustness. There is normally no need for any special regulation to avoid target poisoning.
- the metallic vapor generated during reactive cathodic spark evaporation is ionized to a high degree, which contributes to well-adhering layers.
- the boundary area created by the method between the mullite material and the aluminum oxide-containing layer has spike-like structures made of an aluminum oxide-containing material, preferably aluminum oxide, whereby the adhesion or Binding of the aluminum oxide-containing layer on the mullite material is improved.
- the target preferably also has the metal chromium.
- a target with an element distribution of 70/30 Al / Cr
- the proportion of chromium in the target promotes the formation of a corundum structure in a forming Al-Cr-O mixed crystal, even at relatively low temperatures of 500 ° C. and below.
- the lattice constant of the Al-Cr-O mixed crystal structure in the aluminum oxide-containing layer to be applied can be adapted in a range between corundum and eskolaite.
- the corundum structure is characterized by high thermal stability.
- the Al-Cr-O mixed crystal structure can be present in various crystallite sizes, which are determined by the process conditions of the PVD process, e.g. B. Chromium content in the target, oxygen partial pressure, substrate temperature can be influenced and controlled accordingly. This has the consequence that the applied aluminum oxide-containing layer, depending on the process conditions, for. B. can be X-ray amorphous or can clearly show the corundum structure in an X-ray analysis, the positions of the Bragg peaks corresponding to the chromium content being between those of pure corundum and those of escolaite.
- the aluminum oxide-containing layer is preferred as im
- the mixed crystal structure is thermally stable. More preferably, the crystal structure of the aluminum oxide-containing single-phase layer corresponds to the corundum structure or changes to the corundum structure at higher temperatures. If the layer containing aluminum oxide also contains chromium, it is preferably applied as a single-phase layer with a corundum mixed crystal structure.
- the aluminum oxide-containing layer can have metallic macroparticles, so-called droplets, which can arise, for example, during reactive cathodic spark evaporation.
- the macroparticles can have a higher chromium content than the target; H. Chromium accumulates in the macroparticles.
- the droplets can pass directly into the mixed crystal upon oxidation. This oxidation process can advantageously close any grain boundaries.
- the aluminum oxide-containing layer can have chromium, titanium, hafnium, yttrium, erbium, silicon and / or zirconium.
- the aluminum oxide-containing layer can preferably have chromium.
- the mentioned elements can be present in the target that is used to apply the layer. Other elements can also be included to promote certain properties.
- the elements can serve, for example, to adapt the layer properties to the mullite material to be coated or to influence further layer properties.
- the solubility limit of the said additional elements in aluminum should not be significantly exceeded.
- the proportion of the elements can be so high that their solubility limit in aluminum is approximately reached, but not exceeded, or at most slightly exceeded.
- the proportions of the additional elements can also be higher in order to adapt the properties of the material to specific requirements, e.g. B. in order to adapt the thermal expansion coefficients of the layer to be applied and the substrate material to one another.
- the aluminum oxide-containing layer can be applied with a layer thickness between 0.5 mm and 50 mm.
- the thickness may, for example, depending on the quality, e.g. B. roughness, the surface of the mullite material can be selected so that the properties of the coated mullite material can be improved.
- the method can include a heat treatment of the applied aluminum oxide-containing
- the heat treatment can improve the bond between the applied layer and the substrate. If the applied layer contains chromium, diffusion of the chromium to the layer surface and evaporation of the chromium oxide that is formed can also occur.
- the applied aluminum oxide-containing layer can be post-treated by means of an oxygen plasma.
- plasma oxidation of the applied layer can take place in an oxygen atmosphere, the oxygen being activated by the plasma.
- Such a post-treatment can be advantageous directly after the application of the aluminum Umoxid Anlagenn layer take place on the surface of the mullite material without the vacuum having to be interrupted.
- Another aspect of the invention relates to a mullite material with an aluminum oxide-containing layer arranged on a surface of the mullite material, spike-like structures with tips directed into the aluminum oxide-containing layer being formed in a boundary region between the mullite material and the aluminum oxide-containing layer.
- the mullite material of the present invention can be obtained, for example, by the method explained above.
- the spike-like structures have a substantially triangular shape in cross section (parallel to the layer thickness), e.g. B. the shape of an isosceles triangle.
- a spike-like structure can, for example, approximately have the geometry of a cone with im
- the essentially triangular shape can be detected, for example, by means of scanning electron microscopy images or transmission electron microscopy images after sample preparation that is customary in the art.
- the spike-like structures essentially begin at the interface between the mullite material and the aluminum oxide-containing layer, ie the surface of the mullite material before the coating, and taper as the layer thickness of the aluminum oxide-containing layer increases, ie a point directed into the aluminum oxide-containing layer is formed.
- Typical dimensions of a spike-like structure are a width b (measured parallel to the interface between the mullite material and the aluminum oxide-containing layer) between 50 nm and 200 nm and a height h (measured parallel to the layer thickness of the aluminum-containing layer) between 100 nm and 500 nm.
- the dimensions can, for example, by evaluating Ras- terelectron microscope images or transmission electron microscope images are determined.
- spike-like structures result in a very good bond between the aluminum oxide-containing layer and the mullite material.
- the coated mullite material is characterized by very high thermal stability and a long service life. It can therefore be advantageous for high temperature applications, e.g. B. in the field of gas turbines.
- the layer containing aluminum oxide acts as a protective layer, so that the mullite material can no longer be attacked by hot water vapor. This makes it possible to prevent the release of particles from the surface and consequently erosion caused by the released particles.
- the spike-like structures preferably have an aluminum-containing material or consist of aluminum oxide.
- the layer thickness of the aluminum oxide-containing layer can be between 0.5 mm and 50 mm, preferably between 5 mm and 20 mm. With a layer thickness in this range, particularly good protection of the mullite material under high temperatures can be achieved.
- the aluminum oxide-containing layer is essentially single-phase.
- the aluminum oxide-containing layer can have metallic macroparticles.
- Another aspect of the invention relates to a gas turbine component, e.g. B. a combustion chamber stone with a mullite material according to the Invention.
- the gas turbine component can be part of a gas turbine.
- the use of the mullite material according to the invention has a particularly advantageous effect, since otherwise damage caused by particle-related erosion can lead to long downtimes and high repair costs. Maintenance intervals can be shortened since the gas turbine component according to the invention has a longer service life than a gas turbine component without the mullite material according to the invention.
- Figure 1 is a light microscope image of a section of a
- Figure 2 is a schematic representation of a coated
- FIG. 3 shows an exemplary flow diagram of a coating process
- FIG. 4 is a scanning electron microscope image of a
- Section of a mullite material with a coating (low magnification);
- FIG. 5 shows a schematic representation of the limit area
- FIG. 6 shows a schematic illustration of the proportions of the spike-like structures in cross section
- FIG. 7 is a scanning electron microscope image of a
- FIG. 1 shows a light microscope image of a section of a mullite material 3, in which different phases, which can occur in different grain sizes, are designated. Seen, the triangular formation of a phase having a corundum structure, in Figure 1 as "a-alumina” is referred to, and refers to an elongated configuration with mullite phase, in Figure 1 as "Mullite (3Al 2 O 3 x2SiO 2)". As already mentioned, such a material is referred to herein as a mullite material 3.
- the mullite material 3 can be used, for example, to manufacture combustion chamber bricks for a gas turbine.
- a coated mullite material 3 is shown schematically, as it can be obtained with the method according to the invention.
- a layer 4 containing aluminum oxide, which forms the coating 1 is arranged directly on the surface 2 of the mullite material 3 that has been pretreated by means of a plasma-chemical process.
- the coating 1 can optionally have further layers (not shown in FIG. 2).
- the aluminum oxide-containing layer 4 can for example consist of aluminum oxide. However, other elements, such as. B. contain chromium.
- the aluminum oxide-containing layer 4 was applied by means of a PVD process, preferably by means of reactive cathodic spark evaporation.
- a first method step S1 the surface 2 of the mullite material 3 is pretreated.
- a plasma-chemical process is used for this, in which molecular hydrogen is excited in such a way that plasma-activated hydrogen is produced, which acts on the surface 2.
- This makes silicon from the top atomic layers of phases containing silicon removed so that a surface 2 results, which is in
- the pretreatment can be carried out, for example, as described below.
- the substrate is introduced into a coating chamber with a coating device.
- the coating chamber contains, in addition to a coating device, a further device with which an arc discharge can be generated and which consists of a cathode and an anode.
- the anode can be isolated from the coating chamber, i.e. also isolated from ground (or earth), or at the same potential as the coating chamber, or the anode can be realized by the conductive substrate holder.
- the arc discharge is operated with a noble gas, typically argon. This is let into the space between the cathode and anode, preferably near the cathode, and the flow of argon is chosen so that a pressure in the coating chamber of between 1x10 -4 mbar and 1x10 -2 mbar is established.
- the arc discharge is then ignited by a suitable ignition device.
- Such an arc discharge is characterized by high discharge currents (10A - 400A) and low discharge voltages (20V - 40V).
- the reactive gas to be activated hydrogen is added to it, the flow of the hydrogen gas being chosen so that a total pressure of between 5 ⁇ 10 -3 mbar and 5 ⁇ 10 -2 mbar is established in the coating chamber.
- the attached hydrogen gas is dissociated, atomized, excited and ionized. This creates highly reactive hydrogen, which can react with elements of the substrate surface to be coated and with elements such as Si or C forms volatile, gaseous compounds that can be pumped out.
- the result of this surface pretreatment in the hydrogen plasma is a surface from which both silicon, which is located in the surface of the mullite material, and undesired carbon-based impurities are removed.
- the cleaning depth of such a process is limited to the depth of attack of the activated hydrogen, ie to typical penetration depths in the range of 10 nm - 100 nm.
- These modifications of the surface near the substrate are of course not sufficient to achieve, for example, permanent protection against the volatilization of silicon under water vapor at high temperatures (over 1000 ° C).
- the mullite material is protected by an additional layer after the hydrogen plasma treatment, which is inert to reactive hydrogen.
- a layer 4 containing aluminum oxide is therefore applied to the pretreated surface 2.
- the coating is preferably carried out directly after the pretreatment without interrupting the vacuum in the same coating chamber.
- a PVD process e.g. B. reactive cathodic spark evaporation or sputtering used.
- the applied aluminum oxide-containing layer 4 can be post-treated. There are two ways of doing this. Either the aluminum oxide-containing layer 4 is subjected to a heat treatment in process step S3, e.g. B. for 30 min at 1200 ° C, or the aluminum oxide-containing layer 4 is oxidized in process step S4 by means of an oxygen plasma.
- FIG. 4 shows a scanning electron microscope image of a section of an exemplary mullite material 3 with an aluminum oxide-containing layer 4, which is applied to the surface 2 of the mullite material by means of reactive cathodic spark evaporation. rials 3 was applied.
- the layer thickness 5 is about 2mm.
- the white area above the aluminum oxide-containing layer 4 was caused by over-exposure of the border area (caused by the substrate preparation) when the scanning electron microscope image was made and has no physical significance.
- FIG. 5 shows the area outlined in black in FIG. 4 in the boundary area 7 between mullite material 3 and aluminum oxide-containing layer 4 in a schematic enlarged illustration.
- the spike-like structures 6 lead to a significantly improved connection or adhesion between the mullite material 3 and the aluminum oxide-containing layer 4.
- FIG. 6 illustrates the size relationships of the spike-like structures 6.
- Spike-like structures 6 can be seen in the boundary area 7 between the mullite material 3 and the aluminum oxide-containing layer 4, those at the interface between the mullite material 3 and the aluminum-oxide-containing layer 4, the surface 2 before coating corresponds, begin and the tips 8 are directed into the aluminum oxide-containing layer 4.
- the spike-like structures 6 essentially have the shape of isosceles triangles in the cross section shown.
- the width b of a spike-like structure 6 is between 50 nm and 200 nm, while the height h is between 100 nm and 500 nm.
- the layer thickness 5 of the aluminum oxide-containing layer 4 can for example be approximately 1.5 mm.
- FIG. 7 shows a scanning electron microscope image of a mullite material 3 with an aluminum oxide-containing layer 4 arranged on the surface 2.
- the aluminum oxide-containing layer 4 is essentially single-phase and, in addition to aluminum and oxygen, also has chromium.
- spike-like structures 6 can be seen which begin at the interface between the mullite material 3 and the aluminum oxide-containing layer 4 or the surface 2.
- the tips 8 of the spike-like structures 6 are directed into the layer 4 containing aluminum oxide.
- the width b of a spike-like structure 6 is between 50 nm and 200 nm, while the height h is between 100 nm and 500 nm.
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Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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US17/613,426 US11964921B2 (en) | 2019-05-20 | 2020-05-19 | Method for applying a coating to a surface of a mullite material, mullite material having a coating, and gas turbine component |
CN202080037658.3A CN113874542A (zh) | 2019-05-20 | 2020-05-19 | 施加涂层至莫来石材料表面的方法、具有涂层的莫来石材料和燃气轮机部件 |
CA3138444A CA3138444A1 (en) | 2019-05-20 | 2020-05-19 | A method for applying a coating to a surface of a mullite material, mullite material having a coating and gas turbine component |
JP2021568977A JP2022533406A (ja) | 2019-05-20 | 2020-05-19 | ムライト材料の表面にコーティングを塗布する方法、コーティングを有するムライト材料およびガスタービンモジュール |
EP20739263.0A EP3973087A1 (de) | 2019-05-20 | 2020-05-19 | Verfahren zum aufbringen einer beschichtung auf eine oberläche eines mullitmaterials, mullitmaterial mit einer beschichtung und gasturbinenbauteil |
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DE102019207367.0A DE102019207367A1 (de) | 2019-05-20 | 2019-05-20 | Verfahren zum Aufbringen einer Beschichtung auf eine Oberfläche eines Mullitmaterials, Mullitmaterial mit einer Beschichtung und Gasturbinenbauteil |
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US (1) | US11964921B2 (de) |
EP (1) | EP3973087A1 (de) |
JP (1) | JP2022533406A (de) |
CN (1) | CN113874542A (de) |
CA (1) | CA3138444A1 (de) |
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WO2006099754A1 (de) * | 2005-03-24 | 2006-09-28 | Oerlikon Trading Ag, Trübbach | Hartstoffschicht |
EP1780294A1 (de) | 2005-10-25 | 2007-05-02 | Siemens Aktiengesellschaft | Legierung, Schutzschicht zum Schutz eines Bauteils gegen Korrosion und Oxidation bei hohen Temperaturen und Bauteil |
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DE69924065T2 (de) * | 1998-04-27 | 2006-04-13 | General Electric Co. | Formkörper mit einem überzug aus modifiziertem mullit und verfahren zu dessen herstellung |
US6129954A (en) * | 1998-12-22 | 2000-10-10 | General Electric Company | Method for thermally spraying crack-free mullite coatings on ceramic-based substrates |
US6607852B2 (en) * | 2001-06-27 | 2003-08-19 | General Electric Company | Environmental/thermal barrier coating system with silica diffusion barrier layer |
US20060166019A1 (en) * | 2005-01-21 | 2006-07-27 | Irene Spitsberg | Thermal/environmental barrier coating for silicon-comprising materials |
US20060280955A1 (en) * | 2005-06-13 | 2006-12-14 | Irene Spitsberg | Corrosion resistant sealant for EBC of silicon-containing substrate and processes for preparing same |
DE102007047590A1 (de) * | 2007-10-05 | 2009-04-09 | Robert Bosch Gmbh | Keramischer Schichtverbund sowie Verfahren zu seiner Herstellung |
DE102008004532A1 (de) * | 2008-01-15 | 2009-07-16 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Verfahren zur Herstellung von Mullitfasern mit nanoskaliger Korngröße |
CN104609892B (zh) * | 2015-01-14 | 2017-01-18 | 中国人民解放军国防科学技术大学 | 外表沉积SiBCN涂层的莫来石纤维及其制备方法 |
US20170121232A1 (en) * | 2015-10-30 | 2017-05-04 | Rolls-Royce Corporation | Coating interface |
CN106966763B (zh) * | 2016-06-03 | 2018-07-13 | 北京航空航天大学 | 一种发动机环境下纤维增强的复合材料表面涂层及其制备方法 |
WO2019053257A1 (en) | 2017-09-15 | 2019-03-21 | Oerlikon Surface Solutions Ag, Pfäffikon | AL-CR-O COATINGS HAVING SUPERIOR THERMAL STABILITY AND PROCESS FOR PRODUCING THE SAME |
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- 2020-05-19 WO PCT/EP2020/000096 patent/WO2020233832A1/de unknown
- 2020-05-19 JP JP2021568977A patent/JP2022533406A/ja active Pending
- 2020-05-19 CN CN202080037658.3A patent/CN113874542A/zh active Pending
- 2020-05-19 CA CA3138444A patent/CA3138444A1/en active Pending
- 2020-05-19 US US17/613,426 patent/US11964921B2/en active Active
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WO2006099754A1 (de) * | 2005-03-24 | 2006-09-28 | Oerlikon Trading Ag, Trübbach | Hartstoffschicht |
EP1780294A1 (de) | 2005-10-25 | 2007-05-02 | Siemens Aktiengesellschaft | Legierung, Schutzschicht zum Schutz eines Bauteils gegen Korrosion und Oxidation bei hohen Temperaturen und Bauteil |
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US11964921B2 (en) | 2024-04-23 |
EP3973087A1 (de) | 2022-03-30 |
CA3138444A1 (en) | 2020-11-26 |
US20220213000A1 (en) | 2022-07-07 |
DE102019207367A1 (de) | 2020-11-26 |
JP2022533406A (ja) | 2022-07-22 |
CN113874542A (zh) | 2021-12-31 |
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