WO2014168921A1 - Procédé de fabrication d'une matière céramique - Google Patents

Procédé de fabrication d'une matière céramique Download PDF

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Publication number
WO2014168921A1
WO2014168921A1 PCT/US2014/033283 US2014033283W WO2014168921A1 WO 2014168921 A1 WO2014168921 A1 WO 2014168921A1 US 2014033283 W US2014033283 W US 2014033283W WO 2014168921 A1 WO2014168921 A1 WO 2014168921A1
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Prior art keywords
mobilized
ceramic
glaze
recited
free metal
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PCT/US2014/033283
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English (en)
Inventor
Paul Sheedy
Wayde R. Schmidt
Tania Bhatia Kashyap
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United Technologies Corporation
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Publication date
Priority claimed from US13/859,093 external-priority patent/US9701591B2/en
Application filed by United Technologies Corporation filed Critical United Technologies Corporation
Priority to EP14782827.1A priority Critical patent/EP2984058A4/fr
Publication of WO2014168921A1 publication Critical patent/WO2014168921A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • C—CHEMISTRY; METALLURGY
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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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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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
    • C04B41/50—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
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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
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • 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
    • F01D5/282—Selecting composite materials, e.g. blades with reinforcing filaments
    • 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
    • F01D5/284—Selection of ceramic materials
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23R—GENERATING COMBUSTION PRODUCTS OF HIGH PRESSURE OR HIGH VELOCITY, e.g. GAS-TURBINE COMBUSTION CHAMBERS
    • F23R3/00—Continuous combustion chambers using liquid or gaseous fuel
    • F23R3/007—Continuous combustion chambers using liquid or gaseous fuel constructed mainly of ceramic components
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3891—Silicides, e.g. molybdenum disilicide, iron silicide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5244—Silicon carbide
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • 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
    • F05D2250/00—Geometry
    • F05D2250/60—Structure; Surface texture
    • F05D2250/62—Structure; Surface texture smooth or fine
    • F05D2250/621—Structure; Surface texture smooth or fine polished
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • 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
    • F05D2300/00—Materials; Properties thereof
    • F05D2300/20—Oxide or non-oxide ceramics
    • F05D2300/21—Oxide ceramics
    • F05D2300/2102—Glass
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • 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
    • F05D2300/00—Materials; Properties thereof
    • F05D2300/60—Properties or characteristics given to material by treatment or manufacturing
    • F05D2300/603—Composites; e.g. fibre-reinforced
    • F05D2300/6033—Ceramic matrix composites [CMC]

Definitions

  • Ceramic materials are known and used for components such as coatings, ceramic bodies and ceramic matrices. Ceramic materials may be fabricated using techniques such as powder processing and sintering, polymer impregnation and pyrolysis, or melt or slurry infiltration. However, these processing techniques can limit the chemistry and microstructure of the ceramic material.
  • a method for fabricating a ceramic material according to an example of the present disclosure includes providing a mobilized filler material capable of infiltrating a porous ceramic matrix composite.
  • the mobilized filler material includes at least one of a ceramic material and a free metal.
  • the mobilized filler material is infiltrated into pores of the porous ceramic matrix composite.
  • the mobilized filler material is then immortalized within the pores of the porous ceramic matrix composite.
  • the mobilized filler material is in a preceramic polymer carrier material.
  • the mobilized filler material is a heated melt.
  • the mobilized filler is the free metal, and the free metal is silicon.
  • the mobilized filler is the free metal
  • the free metal is selected from the group consisting of boron, titanium, vanadium, chromium, zirconium, niobium, molybdenum, ruthenium, rhodium, hafnium, tantalum, tungsten, rhenium, osmium, iridium and combinations thereof.
  • the mobilized filler material is the ceramic material.
  • a method for fabricating a ceramic material according to an example of the present disclosure includes infiltrating a surface zone of a porous ceramic matrix composite with a mobilized glaze material such that pores in the surface zone of the porous ceramic matrix composite, exclusive of an interior of the porous ceramic matrix composite, includes the mobilized glaze material and there is a layer of the mobilized glaze material on an exterior side of the porous ceramic matrix composite.
  • the mobilized glaze material is then immortilized.
  • the immobilized glaze material seals the surface zone and provides an exterior glaze layer on the ceramic matrix composite.
  • a further embodiment of any of the foregoing embodiments includes, prior to the infiltrating, applying the glaze material, mobilized or prior to mobilizing, onto one or more of the exterior sides of the porous ceramic matrix composite.
  • a further embodiment of any of the foregoing embodiments includes, prior to the infiltrating, applying the mobilized glaze material onto one or more of the exterior sides of the porous ceramic matrix composite, followed by infiltrating the mobilized glaze material into the surface zone.
  • a further embodiment of any of the foregoing embodiments includes, prior to the infiltrating, applying the glaze material, prior to mobilizing, onto one or more of the exterior sides of the porous ceramic matrix composite, followed by mobilizing the glaze material and then infiltrating the mobilized glaze material into the surface zone.
  • the mobilized glaze material is in a preceramic polymer carrier material and the mobilized glaze is a free metal in the preceramic polymer carrier material, and the free metal is silicon.
  • the mobilized glaze material is a heated melt.
  • the mobilized glaze is a free metal, and the free metal is silicon.
  • the mobilized glaze is a free metal
  • the free metal is selected from the group consisting of boron, titanium, vanadium, chromium, zirconium, niobium, molybdenum, ruthenium, rhodium, hafnium, tantalum, tungsten, rhenium, osmium, iridium and combinations thereof.
  • the mobilized glaze material is a ceramic material.
  • the ceramic material is at least partially amorphous.
  • the ceramic material includes a vitreous material.
  • the ceramic material is a silicate-based glass or glass-ceramic, including an element selected from the group consisting of boron, barium, calcium, magnesium, lithium, sodium, potassium, aluminum, phosphorus, strontium, zinc, the rare earth metals (La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, including Sc, Y, and Hf), and combinations thereof.
  • the rare earth metals La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, including Sc, Y, and Hf
  • the infiltrating of the surface zone is a final iteration in a polymer infiltration and pyrolysis (PIP) process, the PIP process including iteratively infiltrating a preceramic polymer into a porous reinforcement structure, curing the infiltrated preceramic polymer and then pyrolyzing the infiltrated preceramic polymer, the preceramic polymer being free of the mobilized glaze material in all but the final iteration of the PIP process.
  • PIP polymer infiltration and pyrolysis
  • a ceramic article according to an example of the present disclosure includes a ceramic matrix composite including a porous reinforcement structure and a ceramic matrix within pores of the porous reinforcement structure.
  • the ceramic matrix composite includes a surface zone and a glaze material within pores of the surface zone and on an exterior side of the surface zone as an exterior glaze layer on the ceramic matrix composite.
  • the glaze material is a free metal, and the free metal is silicon.
  • the glaze material is a free metal, and the free metal is selected from the group consisting of boron, titanium, vanadium, chromium, zirconium, niobium, molybdenum, ruthenium, rhodium, hafnium, tantalum, tungsten, rhenium, osmium, iridium and combinations thereof.
  • the glaze material is a ceramic material.
  • the glaze material is a Borosilicate glass (BSG) of composition, by weight, Boron Oxide, B2O 3 , 10- 30%; Aluminum Oxide, A1 2 0 3 , 0-4%; Sodium Oxide, Na 2 0, 0-8%; and Silicon Dioxide, Si0 2 , 65-85%.
  • BSG Borosilicate glass
  • the glaze material is a Barium Magnesium Alumino Silicate (BMAS) glass of composition, by weight, Barium Oxide, BaO, 12-16%; Magnesium Oxide, MgO, 5-10%; Boron Oxide, B 2 0 3 , 0-4%; Aluminum Oxide, A1 2 0 3 , 25-35%; and Silicon Dioxide, Si0 2 , 45-55%.
  • BMAS Barium Magnesium Alumino Silicate
  • Figure 1 illustrates a method for fabricating a ceramic material.
  • Figure 2 illustrates an example ceramic component fabricated according to the method of Figure 1.
  • Figure 3 illustrates an infiltration of a free metal into an internal pore.
  • Figure 4 illustrates an example wherein a ceramic component includes ceramic particles and a free metal or free metal-derived compound that coats the ceramic particles.
  • Figure 5 illustrates an example ceramic article.
  • Figure 6 illustrates an example method for fabricating a ceramic material.
  • Figure 7 illustrates a micrograph of a ceramic matrix composite prior to the method of Figure 6.
  • Figure 8 illustrates a micrograph of the ceramic matrix composite of Figure 7 after the method of Figure 6.
  • Figure 1 illustrates a method 20 for fabricating a ceramic material.
  • the method 20 allows fabrication of ceramic materials with new compositions and/or microstructures that are not heretofore available. Furthermore, the method 20 can be used to enhance densification and/or thermal conductivity of ceramic materials for end use components such as turbine engine components.
  • the method 20 generally includes steps 22, 24 and 26. Any or all of steps 22, 24 and 26 can be repeated for a desired number of iterations in the method 20 to modify porosity and properties, for example.
  • a mixture is infiltrated into a porous structure.
  • the mixture includes a preceramic material and a filler material.
  • the filler material includes at least one free metal.
  • a "metal” refers to elements conventionally identified as metals and also to semi-metals or metalloids, such as silicon.
  • a “free metal” refers to a metal or metals that are metallically bonded.
  • free metals include elemental forms of metals and metal-containing compounds that provide a source of metal, such as through decomposition of an organometallic compound.
  • the preceramic material is rigidized, such as by curing, to form a green body.
  • the green body is thermally treated to convert the rigidized preceramic material into a ceramic matrix within the pores of the porous structure.
  • the same thermal treatment or a second, further thermal treatment is used to cause the at least one free metal to move into pores of the thermally treated green body.
  • the pores include internal porosity defined by the ceramic matrix as well as pores defined within or at least partially by the porous structure. In one example, the pores range in size from nanometer size to a few hundred micrometers.
  • the method 20 thus utilizes the infiltration in step 22 to deliver the free metal into the porous structure and the thermal treatment (or subsequent thermal treatment(s)) to infiltrate the free metal into the internal pores of the ceramic matrix as well as pores defined within or at least partially by the porous structure.
  • the internal pores of the ceramic matrix and/or the pores defined within or at least partially by the porous structure include pores that are not interconnected or surface connected.
  • the internal pores are voids, micro-cracks or other open regions that are formed during the conversion of the preceramic material to ceramic.
  • the green body is treated at a temperature that is below the melting temperature of the at least one free metal.
  • the selected thermal treatment temperature is slightly below the melting temperature (e.g., within 10%) of the at least one free metal such that the free metal softens and thereby mobilizes within the ceramic matrix.
  • the mobilized free metal is able to flow and/or diffuse to the internal porosity of the ceramic matrix.
  • the free metal thereby at least partially fills the internal porosity to increase densification of the ceramic matrix and overall ceramic component.
  • the thermal treatment that converts the preceramic material into the ceramic matrix can be followed by a second, further thermal treatment to mobilize the free metal to move to the internal porosity defined by the ceramic matrix.
  • the second thermal treatment is conducted at a temperature that is approximately equivalent to the first thermal treatment temperature or, alternatively, at a higher temperature that is above the melting temperature of the free metal.
  • the free metal liquefies and flows into the internal porosity of the ceramic matrix.
  • the silicon expands upon re- solidification and thereby further enhances densification of the final ceramic component.
  • the porous structure includes or is a fibrous structure having ceramic, metallic and/or carbon fibers.
  • the ceramic fibers include oxide or non-oxide ceramic fibers.
  • the fibers are silicon carbide-containing fibers.
  • the fibers are coated, prior to the method 20, with a suitable protective coating that serves to chemically protect the fibers and allow for the desired composite mechanical behavior.
  • the protective coating includes an oxide or non-oxide coating and can be a monolayer coating or a multilayer coating.
  • the preceramic material is a material that converts from a non-ceramic material to a ceramic material.
  • the preceramic material is a carbosilane-, carbonitride-, silazane-, silane-, or siloxane-based polymer, oligomer or mixture thereof.
  • the preceramic material is a carbosilane -based material that converts, in the absence of oxygen, to silicon carbide.
  • the preceramic material is a silazane -based material that converts, in the absence of oxygen, to silicon carbide and silicon nitride.
  • the preceramic material includes heteroatom modifications such as boron, aluminum, zirconium, gadolinium, hafnium or titanium. Given this description, one of ordinary skill in the art will recognize other types of preceramic materials to meet their particular needs.
  • the at least one free metal includes silicon.
  • additional metals are included with the silicon.
  • the free metal or metals are selected from refractory metals, which include boron, titanium, vanadium, chromium, zirconium, niobium, molybdenum, ruthenium, rhodium, hafnium, tantalum, tungsten, rhenium, osmium, iridium and mixtures thereof.
  • the filler within the mixture includes multiple free metals, such as any of those listed in the above examples.
  • the thermal treatment or, alternatively, the second, further thermal treatment not only mobilizes the free metals but also causes the free metals to react together to form a free metal-derived compound within the internal pores of the ceramic matrix.
  • the free metal-derived compound is molybdenum disilicide (M0S1 2 ) which forms from silicon and molybdenum as the free metals.
  • the filler may range in size from sub-nanometer size to tens or hundreds of micrometers.
  • the filler includes the at least one free metal and further includes ceramic particles that have a different thermal conductivity than the ceramic matrix material produced from conversion of the preceramic material.
  • the filler includes the at least one free metal and further includes ceramic particles that have a higher thermal conductivity than the ceramic matrix material produced from conversion of the preceramic material.
  • the ceramic particles include silicon carbide and the ceramic matrix comprises carbonitride.
  • the at least one free metal forms a continuous phase or region within the ceramic matrix.
  • the continuous phase facilitates the enhancement of thermal conductivity of the final ceramic material by providing a continuous thermal conduction path.
  • FIG. 2 illustrates an example ceramic component 30 fabricated according to the method 20 described above.
  • the ceramic component 30 includes a porous structure 32 and a polymer-derived ceramic matrix 34 within pores 36 of the porous structure 32.
  • the porous structure 32 is a fibrous structure.
  • the fibrous structure includes two or more parallel sets or tows of fibers that are transversely oriented.
  • the fibrous structure is a woven structure, non-woven structure, braided structure, unidirectional fiber lay-up, tape, a two-dimensional structure or three-dimensional structure or other cloth and weave architectures.
  • the fibrous structure can contain continuous, non- continuous or chopped fibers. Given this description, one of ordinary skill in the art will recognize other fibrous structures to meet their particular needs.
  • the polymer-derived ceramic matrix 34 defines internal pores 38 that result from the conversion of the rigidized material to ceramic during the above-described thermal treatment to form the ceramic matrix 34.
  • the internal pores 38 are interconnected, non-interconnected, surface connected or non-surface connected.
  • At least one of a free metal or a free metal-derived compound 40 is located within the internal pores 38 of the polymer-derived ceramic matrix 34 and the residual pores 32a.
  • the free metal can include silicon and/or refractory metals. If multiple free metals are used, the metals may react to form the free metal-derived compound.
  • multiple free metals are used and include at least silicon in combination with one or more of the refractory metals described above.
  • the silicon reacts with the one or more of the refractory metals to form a silicide.
  • the silicide includes titanium silicide, chromium silicide, zirconium silicide, hafnium silicide, niobium silicide, tantalum silicide, tungsten silicide, molybdenum silicide or combinations thereof.
  • the composition of the ceramic component 30, by volume percentage is:
  • FIG. 3 shows the infiltration of a free metal 50 into a pore 52 during thermal treatment in the method 20.
  • the pore 52 may be an internal pore of the preceramic material-derived ceramic matrix 34 or a pore defined within or at least partially by the porous structure 32. This example is based on using silicon as the free metal.
  • stage (A) the free metal 50 is initially located adjacent the pore 52 at the beginning of the thermal treatment.
  • stage (B) the thermal treatment mobilizes the free metal 50 such that the free metal can move by flowing, diffusion or both into a portion of the pore 52.
  • stage (C) upon cooling, the free metal 50 expands within the pore 52 to further fill the pore 52.
  • the free metal facilitates the densification of the ceramic component 30.
  • Figure 4 shows another example wherein the preceramic material-derived ceramic matrix 34 includes ceramic particles 60, such as silicon carbide particles.
  • the free metal 52 migrates and coats the ceramic particles 60 such that there is a continuous region 62 or phase of the free metal or free metal-derived compound that extends through the ceramic matrix 34.
  • the ceramic particles 60 are coated with the one or more free metals prior to mixing with the preceramic material in the method 20. During the thermal treatment to mobilize the free metal or metals, the free metal moves through internal pores of the ceramic matrix 34 and interconnects to form the continuous region 62 or phase.
  • the ceramic particles 60 are not initially coated with the one or more free metals in the mixture with the preceramic material in the method 20. During the thermal treatment to mobilize the free metal or metals, the free metal moves through internal pores of the ceramic matrix 34, coats the ceramic particles 60 and interconnects to form the continuous region 62 or phase.
  • the selected free metal, or at least one of the free metals is chemically compatible with the selected ceramic particles 60 such that the free metal or metals have an affinity to the ceramic particles 60.
  • the ceramic particles 60 include, as a constituent element, the same element as the free metal or at least one of the free metals.
  • the ceramic particles 60 are silicon carbide and the free metal or metals include silicon.
  • the ceramic particles 60 are a carbide of the selected free metal or at least one of the selected free metals.
  • FIG. 5 illustrates an example ceramic article 130 that can be fabricated according to the method 20 described above or by using another method that will be described below.
  • like reference numerals designate like elements where appropriate and reference numerals with the addition of one-hundred or multiples thereof designate modified elements that are understood to incorporate the same features and benefits of the corresponding elements.
  • the ceramic article 130 is shown with an indistinct geometry. It is to be understood, however, that the ceramic article 130 can be any end-use article.
  • the ceramic article 130 can be an article, or portion of an article, of a gas turbine engine, such as but not limited to, combustor liners, turbine blade outer air seals, vanes, and blades.
  • the ceramic article 130 in this example includes a ceramic matrix composite 131 that has a porous reinforcement structure 132.
  • the porous reinforcement structure is a continuous fiber reinforcement (generically shown as a grid).
  • the porous reinforcement structure 132 can alternatively be another type of fiber structure, or a non- fibrous structure.
  • the ceramic matrix composite 131 also includes a ceramic matrix 134 within pores 136 (between the grid lines) of the porous reinforcement structure 132.
  • the ceramic matrix 134 can have internal pores 138.
  • the internal pores 138 can be voids, micro- cracks or other open regions.
  • the ceramic matrix composite 131 includes a surface zone 139 that extends inward from one or more exterior sides 141 of the ceramic matrix composite 131 to a boundary 143 (dashed line) that demarks an interior zone 145.
  • the surface zone 139 extends completely around the ceramic matrix composite 131, although in other examples the surface zone 139 may be at only one or selected exterior sides 141 of the ceramic matrix composite 131.
  • a glaze material 147 is located within pores 136 and/or pores 138 in the surface zone 139 and on one or more of the exterior sides 141 of the surface zone 139 as an exterior glaze layer 147a on the ceramic matrix composite 131.
  • the interior zone 145 is free of any of the glaze material 145 and thus has a greater porosity than the surface zone 139.
  • the boundary 143 is thus a distinct border between the interior zone that has no glaze material 145 and the surface zone 139 that has the glaze material 145 (i.e., the glaze material 145 indicates the boundary 143).
  • the exterior glaze layer 147a is a solid, continuous layer.
  • the exterior glaze layer 147a can be discontinuous. Whether the exterior glaze layer 147a is continuous or discontinuous, at least the glaze material 147 in the surface zone 139 seals the pores 136 and/or pores 138 that open to, or are connected to, the exterior sides 141. The glaze material 147 seals the surface zone 139.
  • the glaze material 147 in the surface zone 139 can also modify porosity and properties, such as mechanical properties or thermal conductivity, at the surface zone 139, for example.
  • a continuous exterior glaze layer 147a can provide additional sealing, as well as enhanced aesthetics of the ceramic component 130.
  • the exterior glaze layer 147a can provide a smoother (i.e., lower surface roughness) exterior surface than the exterior sides 141 of the ceramic matrix composite 131.
  • the glaze material 147 is a free metal, but could also include a ceramic material.
  • the free metal is silicon.
  • the free metal is selected from refractory metals, which include boron, titanium, vanadium, chromium, zirconium, niobium, molybdenum, ruthenium, rhodium, hafnium, tantalum, tungsten, rhenium, osmium, iridium and mixtures thereof.
  • the glaze material 147 is a ceramic material, but can also include the free metal or metals from above.
  • the ceramic material is at least partially amorphous, such as a glass material.
  • the ceramic material includes a vitreous material.
  • the ceramic material is a refractory glass or glass/ceramic composition.
  • the glass or glass-ceramic material is silicate-based.
  • the silicate-based glass or glass-ceramic includes boron, barium, calcium, magnesium, lithium, sodium, potassium, aluminum, phosphorus, strontium, zinc, the rare earth metals (La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, including Sc, Y, and Hi), or combinations thereof.
  • the silicate-based glass or glass/ceramic additionally includes a nucleating agent that serves to precipitate crystalline phases from the amorphous phase with the application of thermal treatment.
  • the nucleating agent includes zirconium or a compound containing zirconium.
  • glass-ceramic systems e.g., the Li 2 0 x - AI2O 3 y - nSi0 2 -System (LAS-System), the MgO x - AI2O 3 y - nSi0 2 -System (MAS-System), the ZnO x - A1 2 0 3 y - nSi0 2 -System (ZAS-System), the CaO x - A1 2 0 3 y - nSi0 2 -System (CAS), the BaO x - MgO y - A1 2 0 3 z - nSi0 2 -System (BMAS-System), the CaO x - MgO y - A1 2 0 3 z - nSi0 2 -System (CMAS-System), the BaO x - A1 2 0 3 y - nSi0 2 -System (BAS-System), the SrO
  • the glaze material 147 can be selected based upon the composition of the ceramic matrix composite 131 and use environment of the end-use ceramic article 130.
  • a Borosilicate glass (BSG) is used as the glaze material 147, with the following oxide compositions, by weight: Boron Oxide, B 2 C>3, 10-30%; Aluminum Oxide, A1 2 0 3 , 0-4%; Sodium Oxide, Na 2 0, 0-8%; and Silicon Dioxide, Si0 2 , 65- 85%.
  • a Barium Magnesium Alumino Silicate (BMAS) glass is used as the glaze material 147, with the following oxide composition ranges by weight: Barium Oxide, BaO, 12-16%; Magnesium Oxide, MgO, 5-10%; Boron Oxide, B 2 0 3 , 0-4%; Aluminum Oxide, A1 2 0 3 , 25-35%; and Silicon Dioxide, Si0 2 , 45-55%.
  • BMAS Barium Magnesium Alumino Silicate
  • FIG. 6 illustrates a method 170 for fabricating a ceramic material, such as the ceramic article 130.
  • the method 170 will be described with reference to the structure of the ceramic article 130.
  • the method 170 includes an infiltration step 172 and an immobilization step 174.
  • the infiltration step 172 includes infiltrating the surface zone 139 of the porous ceramic matrix composite 131 with a mobilized glaze material 147 such that pores 136 and/or 138 in the surface zone 139, exclusive of the interior zone 145, include the mobilized glaze material 147 and there is a layer of the mobilized glaze material (exterior glaze layer 147a) on the exterior side 141 of the porous ceramic matrix composite 131.
  • the term "mobilized” or variations thereof refers to the ability of the glaze material 147 to infiltrate into the pores 136 and/or 138 under temperatures and/or environment conditions that do not chemically alter the ceramic matrix composite 131.
  • the immobilization step includes immobilizing the mobilized glaze material 147.
  • the immobilized glaze material 147 seals the surface zone 139 and provides the exterior glaze layer 147a on the ceramic matrix composite 131.
  • the glaze material 147 is mobilized thermally, non- thermally, or a combination thereof.
  • the glaze material 147 can be thermally mobilized to a heated melt by thermal melting or softening to a flowable state.
  • the glaze material 147 can be non-thermally mobilized by inclusion of the glaze material 147 in a carrier material.
  • the carrier material is a preceramic material as described above, but could alternatively be a solvent that is later removed by evaporation.
  • the infiltration of the infiltration step 172 can first include application of the glaze material 147, mobilized or prior to mobilizing, onto one or more of the exterior sides 141 of the ceramic matrix composite 131.
  • the application can include one or more of spraying the glaze material 147 onto one or more of the exterior sides 141, submerging or partially submerging the ceramic matrix composite 131 in the glaze material 147, or applying a powderized form of the glaze material 147 onto one or more of the exterior sides 141.
  • the application is not limited to any particular technique and other techniques can be used.
  • the glaze material 147 can then be mobilized, such as by thermal mobilization. If already mobilized, thermally or non-thermally, the glaze material 147 can then be infiltrated into the surface zone 139. For example, the infiltration can occur from flow of the mobilized glaze material 147 into the pores 136 and/or 138. A low pressure, vacuum environment can be used for assistance. Additionally or alternatively, the infiltration can occur from capillary action in the pores 136 and/or 138.
  • the immobilization step 174 includes immobilizing the glaze material 147 in the pores 136 and/or 138.
  • the term “mobilized” or variations thereof refers to the ability of the glaze material 147 to infiltrate into the pores 136 and/or 138
  • the term “immobilized” or variations thereof refers to the inability of the glaze material 147 to exfiltrate from the pores 136 and/or 138.
  • the glaze material 147 can be immobilized by cooling to a lower temperature (for a thermally mobilized glaze material 147) or by conversion or removal of the carrier material (for non-thermally mobilized glaze material 147).
  • the infiltration step 172 is part of a polymer infiltration and pyrolysis (PIP) process.
  • PIP polymer infiltration and pyrolysis
  • the PIP process includes iteratively infiltrating a preceramic polymer material into the porous reinforcement structure 132, curing the infiltrated preceramic polymer material and then pyrolyzing the infiltrated preceramic polymer material.
  • the preceramic polymer material is free of the glaze material 147 in all but the final iteration of the PIP process.
  • the preceramic polymer material is mixed with a free silicon metal glaze material 147 and infiltrated into the porous reinforcement structure 132 in the final iteration of the PIP process.
  • the infiltrated porous reinforcement structure 132 is then processed at an elevated temperature in an inert environment that is free of oxygen.
  • the elevated temperature can the pyrolysis temperature of the preceramic polymer material and, in one example, can be greater than 1400°C.
  • the free silicon metal melts and further infiltrates into the pores 136 and/or 138. Upon cooling, as indicated above, the silicon expands and thus further enhances densification.
  • Figure 7 illustrates a micrograph of a ceramic matrix composite 231 prior to the method 170.
  • Figure 8 illustrates a micrograph of the ceramic matrix composite 231 after the method 170, wherein the glaze material 147 fills many of the pores 136 and/or 138.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Composite Materials (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne un procédé de fabrication d'une matière céramique qui comprend la disposition d'une matière de charge mobilisée apte à infiltrer un composite à matrice céramique poreuse. La matière de charge mobilisée comprend au moins l'un d'une matière céramique et d'un métal libre. La matière de charge mobilisée est infiltrée dans les pores du composite à matrice céramique poreuse. La matière de charge mobilisée est ensuite immobilisée à l'intérieur des pores du composite à matrice céramique poreuse.
PCT/US2014/033283 2013-04-09 2014-04-08 Procédé de fabrication d'une matière céramique WO2014168921A1 (fr)

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US13/859,093 US9701591B2 (en) 2011-10-12 2013-04-09 Method for fabricating a ceramic material
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CN106587621A (zh) * 2016-11-11 2017-04-26 广东道氏技术股份有限公司 一种超耐磨立体装饰效果晶钢釉
WO2018072970A1 (fr) * 2016-10-17 2018-04-26 Siemens Aktiengesellschaft Écran thermique céramique à infiltration de surface servant à éviter la corrosion et les attaques par érosion

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