WO2021027469A1 - 一种SiCf/SiC复合材料火焰筒及其自动化制备方法 - Google Patents

一种SiCf/SiC复合材料火焰筒及其自动化制备方法 Download PDF

Info

Publication number
WO2021027469A1
WO2021027469A1 PCT/CN2020/101903 CN2020101903W WO2021027469A1 WO 2021027469 A1 WO2021027469 A1 WO 2021027469A1 CN 2020101903 W CN2020101903 W CN 2020101903W WO 2021027469 A1 WO2021027469 A1 WO 2021027469A1
Authority
WO
WIPO (PCT)
Prior art keywords
sic
preform
layer
flame tube
sio
Prior art date
Application number
PCT/CN2020/101903
Other languages
English (en)
French (fr)
Inventor
阳海棠
郭小军
黄小忠
Original Assignee
中南大学
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中南大学 filed Critical 中南大学
Publication of WO2021027469A1 publication Critical patent/WO2021027469A1/zh
Priority to US17/474,091 priority Critical patent/US11591267B2/en

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/89Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62277Fibres based on carbides
    • C04B35/62281Fibres based on carbides based on silicon carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00Layered products essentially comprising ceramics, e.g. refractory products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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
    • C04B35/573Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/6269Curing of mixtures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/6286Carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/6286Carbides
    • C04B35/62863Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/62865Nitrides
    • C04B35/62868Boron nitride
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/62865Nitrides
    • C04B35/62871Silicon nitride
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/62873Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62884Coating the powders or the macroscopic reinforcing agents by gas phase techniques
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62894Coating the powders or the macroscopic reinforcing agents with more than one coating layer
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62897Coatings characterised by their thickness
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating 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
    • C04B41/4523Coating 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 molten state ; Thermal spraying, e.g. plasma spraying
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating 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
    • C04B41/4523Coating 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 molten state ; Thermal spraying, e.g. plasma spraying
    • C04B41/4527Plasma spraying
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating 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
    • C04B41/4529Coating 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
    • C04B41/4531Coating 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 by C.V.D.
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating 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
    • C04B41/455Coating 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4584Coating or impregnating of particulate or fibrous ceramic material
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/46Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
    • C04B41/49Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
    • C04B41/4905Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
    • C04B41/4922Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane
    • C04B41/4933Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane containing halogens, i.e. organohalogen silanes
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating 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
    • C04B41/5024Silicates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating 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
    • C04B41/5025Coating 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
    • C04B41/5027Oxide ceramics in general; Specific oxide ceramics not covered by C04B41/5029 - C04B41/5051
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/04Coating on selected surface areas, e.g. using masks
    • C23C16/045Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32Carbides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32Carbides
    • C23C16/325Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34Nitrides
    • C23C16/342Boron nitride
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34Nitrides
    • C23C16/345Silicon nitride
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23RGENERATING COMBUSTION PRODUCTS OF HIGH PRESSURE OR HIGH VELOCITY, e.g. GAS-TURBINE COMBUSTION CHAMBERS
    • F23R3/00Continuous combustion chambers using liquid or gaseous fuel
    • F23R3/007Continuous combustion chambers using liquid or gaseous fuel constructed mainly of ceramic components
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23RGENERATING COMBUSTION PRODUCTS OF HIGH PRESSURE OR HIGH VELOCITY, e.g. GAS-TURBINE COMBUSTION CHAMBERS
    • F23R3/00Continuous combustion chambers using liquid or gaseous fuel
    • F23R3/42Continuous combustion chambers using liquid or gaseous fuel characterised by the arrangement or form of the flame tubes or combustion chambers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40Metallic constituents or additives not added as binding phase
    • C04B2235/404Refractory metals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445Fluoride containing anions, e.g. fluosilicate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5244Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5268Orientation of the fibers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/614Gas infiltration of green bodies or pre-forms
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94Products characterised by their shape
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607Thermal properties, e.g. thermal expansion coefficient
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669Resistance against chemicals, e.g. against molten glass or molten salts
    • C04B2235/9684Oxidation resistance
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32Ceramic
    • C04B2237/36Non-oxidic
    • C04B2237/365Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32Ceramic
    • C04B2237/38Fiber or whisker reinforced
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23RGENERATING COMBUSTION PRODUCTS OF HIGH PRESSURE OR HIGH VELOCITY, e.g. GAS-TURBINE COMBUSTION CHAMBERS
    • F23R2900/00Special features of, or arrangements for continuous combustion chambers; Combustion processes therefor
    • F23R2900/00018Manufacturing combustion chamber liners or subparts

Definitions

  • the invention relates to the technical field of structural materials for aviation, in particular to a SiC f /SiC composite flame tube and an automated preparation method thereof.
  • the combustion chamber is one of the core components of an aero engine. Its main function is to convert the chemical energy of the fuel into heat energy through combustion to improve the ability of the gas to expand in the turbine and nozzle.
  • the flame tube is The place where the combustion is organized is the key component to ensure air splitting, sufficient combustion, uniform mixing and effective cooling of the wall.
  • the reliability, economy and life of the combustion chamber depend to a large extent on the reliability and Temperature resistance, so the development of high-performance and long-life combustor flame tube plays a vital role in improving engine performance.
  • the existing silicon carbide fiber-reinforced ceramic matrix (SiC f /SiC) composite material has excellent performance and is the preferred material to replace superalloys as the material for the hot end components of aeroengines.
  • the stress in the service environment will promote the composite matrix Cracking accelerates the damage and corrosion of the material, affecting its long-life requirements in high-temperature gas environments, which severely restricts the application of SiC f /SiC composites in the flame tube of the engine combustion chamber; such as the patent of US20120076927A1, which provides an improvement
  • the method for the mechanical properties of fiber-reinforced silicon-carbon composites in the patent improves the fiber interface coating and ceramic matrix by controlling the heat treatment of the composite material, and at the same time can remove the excess silicon in the phase matrix, but the patent has a treatment time- The limitation of temperature-environmental conditions is very strict.
  • the heat treatment can even reach the treatment temperature of 1900°C, and the treatment holding time is as long as 100 hours in a vacuum or in an inert gas environment with a purity of more than 99%.
  • the ceramic substrate is prepared solely by the CVI process. It can effectively control free silicon, but cannot guarantee the high density of the material, which is not conducive to the market. Therefore, we have developed a high-performance SiC f /SiC composite flame tube that can produce high density at low cost and remove excess silicon.
  • the preparation method is particularly necessary;
  • the patent CN106966738B uses a three-dimensional four-step method to weave the preform of the combustion chamber flame tube, and the connection part adopts fiber stitching technology.
  • the flame tube is in a high-temperature gas environment, stress concentration and slight cracks will be formed at the connection, thereby accelerating material damage And corrosion, which seriously restrict the performance of the composite flame tube; and through the finite element method shown in Figure 1 to analyze the temperature field distribution of the flame tube, it can be seen that there is a temperature difference of about 240 °C between the cold and hot ends of the flame tube, and The temperature change gradient inside the flame tube is large, so the temperature difference will cause stress inside the material, and then cracks.
  • the flame tube must have a low thermal expansion coefficient to ensure the dimensional stability of the component during temperature changes. At the same time, it must have high heat.
  • Conductivity to avoid flame tube failure caused by thermal stress concentration; at the same time, the current three-dimensional four-step braiding method basically adopts manual weaving method, which has high cost, long construction period and uncontrollable quality. Therefore, automatic continuous preparation of flame tube prefabrication has been developed The body plays a vital role in the wide application of SiC f /SiC composites in the flame tube.
  • this application provides a SiC f /SiC composite flame tube and an automated preparation method thereof.
  • the prepared SiC f /SiC composite flame tube not only has the characteristics of high temperature resistance and long life, but also It also has the advantages of low thermal expansion coefficient, high thermal conductivity, high thermal shock resistance and excellent mechanical properties.
  • the preparation method has a high degree of automation, short production cycle, low cost and controllable quality.
  • the technical scheme of the present invention is as follows: an automatic preparation method of a SiC f /SiC composite flame tube, including the following steps:
  • the SiC fiber is prepared by chemical vapor deposition to prepare the interface layer to obtain the SiC fiber with a continuous interface layer;
  • the SiC fiber with the continuous interface layer obtained in step 1) is unidirectionally taped and wound to obtain a net-size molded preform;
  • step 2) The preform obtained in step 2) is densified by the reactive melt infiltration process and the chemical vapor deposition process successively, until the quality of the SiC matrix formed by the chemical vapor deposition process and the SiC matrix formed by the reactive melt infiltration process The ratio is 1 ⁇ 1:2;
  • step 5 Prepare a thermal barrier coating on the surface of the preform obtained in step 4), the thickness of the thermal barrier coating is 100-150um, and a high-density SiC f /SiC composite flame tube is obtained fully intelligently.
  • the simulation simulation of the present invention includes the finite element analysis method to analyze the temperature field, and the method of combining multi-scale analysis and finite element solid modeling, according to the temperature field analysis, guides the design of composite flame tube components, fiber volume, fiber direction and
  • the parameters such as the molding method of the composite material can be used to improve the efficiency and accuracy of the performance prediction of the SiC f /SiC composite flame tube, and to realize the automation and high efficiency of the preparation method.
  • the interface layer in step 1) of the present invention is one or more of PyC, SiC, B 4 C, ZrC, HfC, TaC, Si 3 N 4 , and BN.
  • the chemical vapor deposition process of the present invention specifically includes: selecting the precursor according to the introduced interface layer, hydrogen as the reaction gas, argon as the dilution gas, and introducing the gas into the chemical vapor deposition furnace by the bubbling method, and the deposition temperature is 500 ⁇ 1400°C, the deposition pressure is 0.5-12KPa, the deposition time is 60-600min, and the thickness of the deposited interface layer is 100nm-2 ⁇ m; the precursors are methane, trichloromethylsilane, boron chloride, zirconium chloride, and chlorinated One or more of tantalum, silicon chloride, boron halide, and ammonia gas.
  • the step 2) of the present invention includes the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, coat the surface of the flame tube mold evenly with epoxy resin release agent 2 to 3 times, and heat the flame tube mold to 30-50°C;
  • Step 2 Lay the SiC fiber with a volume content of 40-65% and the prepreg unidirectional tape with the balance being resin on the surface of the flame cylinder mold;
  • Step 3 Winding a prepreg unidirectional tape with a volume content of 50-70% SiC fiber and a balance of resin on the surface of the mold laid in Step 2 through a winding machine, and wind it from the inside to the outside in a way of decreasing winding tension gradient ,
  • the winding angle is 30 ⁇ 90°
  • the winding speed is 0.3 ⁇ 0.7m/s
  • the winding tension is 2 ⁇ 10N/cm
  • the winding thickness is 1 ⁇ 5mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and molding, the curing temperature is 90-165°C, and the curing time is 4-8h;
  • Step five demold the preform after curing and molding in step four. After demolding, the preform is processed by a combination of grinding processing and laser processing to obtain a net-size molded preform.
  • the step 3) reaction melt infiltration process of the present invention is specifically a molten silicon infiltration process: the equipment is a vacuum high temperature atmosphere deposition furnace and a vacuum high temperature silicon infiltration furnace, using silicon alloy as the silicon source, argon as the dilution gas, and the deposition temperature 1450 ⁇ 1800°C, the deposition pressure is 2Pa ⁇ normal pressure, and the siliconizing time is 30 ⁇ 300min; the silicon alloy is the binary or ternary of Si and Ta, Hf, Mo, W, Zr, Ti, B, Be alloy.
  • the chemical vapor deposition process of step 3) of the present invention specifically includes using trichloromethylsilane as the precursor, hydrogen as the reaction gas, and argon as the diluent gas, and introducing the gas into the chemical vapor deposition furnace by a bubbling method.
  • the deposition temperature is 900-1200°C
  • the deposition pressure is 0.5-5KPa
  • the deposition time is 60-6000min.
  • the environmental barrier coating in step 4) of the present invention includes a Si bonding layer, a rare earth monosilicate Re 2 SiO 5 surface layer, and Yb 2 Si 2 O 7 located between the bonding layer and the surface layer.
  • Intermediate layer; the thickness ratio of the Si bonding layer, the Yb 2 Si 2 O 7 intermediate layer and the rare earth monosilicate Re 2 SiO 5 surface layer is 1-2:1-2:1-3;
  • the silicate Re 2 SiO 5 is selected from at least one of Y 2 SiO 5 , Sc 2 SiO 5 , Gd 2 SiO 5 , Er 2 SiO 5 , Tm 2 SiO 5 , Yb 2 SiO 5 , and Lu 2 SiO 5 .
  • the preparation method of the environmental barrier coating of the present invention includes the following steps:
  • the rare earth monosilicate Re 2 SiO 5 powder is sprayed on the preform with the bonding layer and the intermediate layer to obtain the environmental barrier coating.
  • the parameters of the plasma spraying method include: plasma gas includes argon and helium, the flow rate of the argon gas is 60-80 slpm, the flow rate of the helium gas is 40-60 slpm, and the powder feeding rate is 10-35r/min, The spraying distance is 90 ⁇ 200mm.
  • the thermal barrier coating is R 2 O 3 , ZrO 2 , CeO 2 , Al 2 O 3 .2SiO 2 , SrZrO 3 , La 2 Zr 2 O 7 , La 2 Ce 2 O 7 At least one of.
  • the invention also provides a SiC f /SiC composite flame tube.
  • the present invention introduces a uniform interface layer between the fiber and the matrix, so that the fiber and the matrix will not be integrated.
  • the layered fiber-interface layer-matrix structure can absorb the energy required for crack propagation and effectively improve the composite material.
  • the existence of the ceramic interface layer can protect the SiC fiber from corrosion by oxygen, water vapor, fuel, acid, etc., thereby increasing the use temperature and use environment.
  • the present invention combines the chemical vapor deposition process (CVI) and the reactive infiltration process (MI) to densify the ceramic matrix composite material.
  • CVI chemical vapor deposition process
  • MI reactive infiltration process
  • the MI process is simple and the cycle is short, and MI-SiC/SiC has higher Density and lower apparent porosity, so the composite material has higher thermal conductivity, especially the thermal conductivity perpendicular to the fiber direction.
  • MI-SiC/SiC is more than twice that of CVI-SiC/SiC composite material, which is beneficial
  • the improvement of thermal shock resistance on the other hand, according to the experimental data, it is known that the thermal expansion coefficient of the MI-SiC/SiC composite is greater than that of the CVI-SiC/SiC composite.
  • the composite matrix composition and structure are adjusted to achieve The controllability of the thermal expansion coefficient of the material, and obtaining materials with low thermal expansion coefficient and supporting members for space optics, effectively reducing the degree of deformation caused by uneven heating of the material, and improving the service life of the SiC f /SiC composite flame tube; at the same time, the present invention
  • the processing temperature in the reactive infiltration process is lower than the conventional temperature, which can effectively reduce the silicon content on the surface of the composite material, thereby improving the high temperature resistance of the composite material.
  • the present invention adopts the automatic method of unidirectional tape laying and winding to prepare the preform, so that while obtaining the three-dimensional preform, the fiber cloth is extended in the thickness direction.
  • the distance between the fibers is minimized, and the fiber cloth is kept flat, which not only increases the fiber volume content, but also ensures the uniformity of the fiber distribution.
  • the composite flame tube made by this method has light weight, high strength, and no micro cracks. At the same time, it also has the characteristics of high temperature resistance, abrasion resistance, and anti-leakage. At the same time, it has high automation, short production cycle, low cost and controllable quality.
  • the environmental barrier coating in the present invention is a Si layer, considering that Si has a higher melting point, so it can ensure that the environmental barrier coating has a higher ambient applicable temperature;
  • the intermediate layer material is Yb 2 Si 2 O 7 , considering that The thermal expansion coefficient of Yb 2 Si 2 O 7 is small, which is significantly lower than the thermal expansion coefficient of the rare earth monosilicate Re 2 SiO 5 surface layer, which makes it difficult to be penetrated by cracks during the thermal cycle, which is beneficial to improve the resistance of the coating.
  • Thermal shock performance on the other hand, the rare earth silicate Re 2 SiO 5 surface layer of the present invention has excellent water vapor corrosion resistance, which can further improve the protective performance of the coating system.
  • the present invention adopts a high temperature reaction heat treatment method to form the Si layer, which can further reduce the silicon content on the surface of the composite material, thereby improving the high temperature resistance of the composite material.
  • the silicon carbide can be improved by optimizing the heat treatment temperature. The grain size of the coating and the density of the coating, so as to obtain a high-temperature resistant, high-density composite flame tube.
  • the present invention first analyzes the temperature field of the composite flame tube through the finite element method, and then uses the method of combining multi-scale analysis and finite element solid modeling to combine the meso and macro to obtain the deterministic load of the structure and The state of the fiber matrix at the load, the design of the composite flame tube component, the fiber volume, the fiber direction, and the molding method of the composite material are guided to improve the efficiency and accuracy of the performance prediction of the SiC f /SiC composite flame tube, and realize the preparation The automation and efficiency of the method.
  • Figure 1 is a schematic diagram of the temperature field calculated by the finite element method of the SiC f /SiC composite flame tube of the present invention.
  • Figure 2 is a schematic diagram of the preparation process of the SiC f /SiC composite flame tube of the present invention.
  • Example 3 is a scanning electron microscope image of the PyC/Si 3 N 4 /BN multilayer interface layer of Example 3.
  • Figure 4 is a scanning electron micrograph of the MI SiC/CVI SiC substrate of the present invention.
  • Figure 5 is a scanning electron micrograph of the EBC environmental barrier layer of the present invention.
  • Figure 6 is an enlarged view of the surface of the EBC environmental barrier layer of the present invention.
  • Figure 7 is a design diagram of the thermal protection coating structure of the present invention.
  • Fig. 8 is a schematic diagram of the structure of laying and winding the unidirectional tape of the present invention.
  • Fig. 9 is a perspective view of the flame tube of the SiC f /SiC composite material of the present invention.
  • Figure 10 shows the apparent state and cross-sectional morphology of Example 1 after different times of thermal shock at 1100°C ⁇ 20min.
  • Figure 11 shows the apparent state and cross-sectional morphology of Example 1 after different times of thermal shock at 1200°C ⁇ 20min.
  • Figure 12 shows the apparent state and cross-sectional morphology of Example 1 after different times of thermal shock at 1300°C ⁇ 20 min.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly coat the epoxy resin release agent on the surface of the flame tube mold twice, and heat the flame tube mold to 30°C;
  • Step 2 Lay the SiC fiber with a volume content of 40% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Winding a prepreg unidirectional tape with a volume content of 50% SiC fiber and a balance of resin on the surface of the mold laid in Step 2 by a winding machine, with a winding angle of 30° and a winding speed of 0.3m/s. Winding tension is 2N/cm, winding thickness is 1mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and molding, the curing temperature is 90°C, and the curing time is 4 hours;
  • Step five demold the preform after curing and molding in step four, and after demolding, perform product finishing on the preform by laser processing to obtain a net-size molded preform;
  • the preform obtained in step 2) is densified by using a reactive melt infiltration process and a chemical vapor deposition process successively.
  • the low-temperature vacuum silicon infiltration is performed first.
  • the binary alloy of Si and Ta is used as the silicon source, and argon is used as the silicon source.
  • Dilution gas the deposition temperature is 1400°C
  • the deposition pressure is normal pressure
  • the siliconizing time is 300min
  • Argon is the diluent gas.
  • the gas is introduced into the chemical vapor deposition furnace by bubbling.
  • the deposition temperature is 900°C
  • the deposition pressure is 5KPa
  • the deposition time is 6000min. Cooling with the furnace is used and repeated once until the chemical vapor deposition process.
  • the mass ratio of the formed SiC matrix to the SiC matrix formed by the reactive melt infiltration process is 1:1;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the plasma gas includes argon and helium
  • the flow of the argon is 60 slpm
  • the flow of the helium is 40 slpm
  • the powder feeding rate is 10r/min
  • the spraying distance is 90mm
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -Al 2 O 3 and has a thickness of 100 ⁇ m. It is fully intelligent to obtain a high-density SiC f /SiC composite Material flame tube.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly apply 3 times of epoxy resin release agent on the surface of the flame tube mold, and heat the flame tube mold to 50°C;
  • Step 2 Lay the SiC fiber with a volume content of 65% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Wind the prepreg unidirectional tape with a volume content of 70% of SiC fiber and the balance of resin on the surface of the mold laid in Step 2 by a winding machine, with a winding angle of 90° and a winding speed of 0.7m/s.
  • the winding tension is 10N/cm, and the winding thickness is 5mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing, the curing temperature is 165°C, and the curing time is 8 hours;
  • Step five demold the preform after curing and molding in step four, and perform product finishing on the preform by laser processing after demolding to obtain a net-size molded preform.
  • the preform obtained in step 2) is densified by using a chemical vapor deposition process and a reactive melt infiltration process successively.
  • the low-temperature vacuum silicon infiltration is performed first.
  • the binary alloy of Si and Ta is used as the silicon source, and argon is used as the silicon source.
  • Dilution gas, deposition temperature is 1800°C, deposition pressure is 2Pa, siliconizing time is 30min, using furnace cooling, repeat once; then chemical vapor deposition is performed with trimethylsilane as precursor, hydrogen as reaction gas, argon
  • the gas is the diluent gas.
  • the gas is introduced into the chemical vapor deposition furnace by bubbling method.
  • the deposition temperature is 1200°C
  • the deposition pressure is 0.5KPa
  • the deposition time is 60min.
  • the furnace is cooled and repeated once until the chemical vapor deposition process.
  • the mass ratio of the formed SiC matrix to the SiC matrix formed by the reactive melt infiltration process is 1:2;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the plasma gas includes argon and helium
  • the flow of the argon is 80 slpm
  • the flow of the helium is 60 slpm
  • the powder feeding rate is 35r/min
  • the spraying distance is 200mm
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -Al 2 O 3 and has a thickness of 150 ⁇ m. It is fully intelligent to obtain a high-density SiC f /SiC composite Material flame tube.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly coat the epoxy resin release agent on the surface of the flame tube mold twice, and heat the flame tube mold to 40°C;
  • Step 2 Lay the SiC fiber with a volume content of 55% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Wrap a prepreg unidirectional tape with a volume content of 60% of SiC fiber and a balance of resin on the surface of the mold laid in step 2 through a winding machine, with a winding angle of 60° and a winding speed of 0.5m/s.
  • the winding tension is 6N/cm, and the winding thickness is 3mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and forming, the curing temperature is 120°C, and the curing time is 6 hours;
  • Step five demold the preform after curing and molding in step four, and perform product finishing on the preform by laser processing after demolding to obtain a net-size molded preform.
  • the preform obtained in step 2) is densified by using a chemical vapor deposition process and a reactive melt infiltration process successively.
  • the low-temperature vacuum silicon infiltration is performed first.
  • the binary alloy of Si and Ta is used as the silicon source, and argon is used as the silicon source.
  • Dilution gas, deposition temperature is 1600°C, deposition pressure is 1Pa, siliconizing time is 180min, using furnace cooling, repeated once; then chemical vapor deposition is performed with trimethylsilane as precursor, hydrogen as reaction gas, argon
  • the gas is the diluent gas, and the gas is introduced into the chemical vapor deposition furnace by bubbling method.
  • the deposition temperature is 1000°C
  • the deposition pressure is 3KPa
  • the deposition time is 4800min.
  • the furnace is cooled and repeated once until the chemical vapor deposition process is formed.
  • the mass ratio of SiC matrix to the SiC matrix formed by the reaction melt infiltration process is 1:1.5;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the thickness ratio of the Si bonding layer, Yb 2 Si 2 O 7 intermediate layer and rare earth monosilicate Re 2 SiO 5 surface layer of 1:2:1, prepare the intermediate layer and the surface layer, and the preparation process
  • Plasma spraying method is used in both, and the plasma gas includes argon and helium, the flow of the argon is 70 slpm, the flow of the helium is 50 slpm, the powder feeding rate is 20r/min, and the spraying distance is 120mm,
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -Al 2 O 3 and has a thickness of 120 um. It is fully intelligent to obtain a high-density SiC f /SiC composite Material flame tube.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the PyC interface layer uses methane as the precursor, hydrogen as the reaction gas, and argon as the dilution gas.
  • the gas is introduced into the chemical vapor deposition furnace by the bubbling method.
  • the deposition temperature is 500°C
  • the deposition pressure is 12KPa
  • the deposition time is 600min.
  • the thickness of the deposited interface layer is 100nm; the specific introduction of the Si 3 N 4 interface layer uses trichloromethylsilane and ammonia as the precursors, hydrogen as the reaction gas, and argon as the dilution gas. The gas is introduced into the chemical by bubbling method.
  • the deposition temperature is 500°C
  • the deposition pressure is 0.5KPa
  • the deposition time is 600min
  • the thickness of the deposited interface layer is 100nm
  • the specific introduction of the BN interface layer uses boron chloride and ammonia as precursors, and hydrogen as the reaction
  • the gas, argon is the diluent gas
  • the gas is introduced into the chemical vapor deposition furnace by bubbling method
  • the deposition temperature is 500°C
  • the deposition pressure is 12KPa
  • the deposition time is 600min
  • the thickness of the deposited interface layer is 100nm
  • after cooling with the furnace That is, SiC fiber with multiple continuous interface layers is obtained;
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly coat the epoxy resin release agent on the surface of the flame tube mold twice, and heat the flame tube mold to 30°C;
  • Step 2 Lay the SiC fiber with a volume content of 40% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Winding a prepreg unidirectional tape with a volume content of 50% SiC fiber and a balance of resin on the surface of the mold laid in Step 2 by a winding machine, with a winding angle of 30° and a winding speed of 0.3m/s. Winding tension is 2N/cm, winding thickness is 1mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and molding, the curing temperature is 90°C, and the curing time is 4 hours;
  • Step five demold the preform after curing and molding in step four, and perform product finishing on the preform by laser processing after demolding to obtain a net-size molded preform.
  • step 2) The preform obtained in step 2) is densified using a chemical vapor deposition process and a reactive melt infiltration process successively, and first is subjected to low-temperature vacuum silicon infiltration, using a binary alloy of Si and Mo as the silicon source, and argon as the source Dilution gas, deposition temperature is 1400°C, deposition pressure is 2Pa, siliconizing time is 300min, using furnace cooling, repeated once; then chemical vapor deposition is performed with trimethylsilane as precursor, hydrogen as reaction gas, argon The gas is the diluent gas, and the gas is introduced into the chemical vapor deposition furnace by bubbling.
  • the deposition temperature is 900°C
  • the deposition pressure is 5KPa
  • the deposition time is 60min.
  • the furnace is cooled and repeated once until the chemical vapor deposition process is formed.
  • the mass ratio of SiC matrix to the SiC matrix formed by the reactive melt infiltration process is 1:1;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the plasma gas includes argon and helium
  • the flow of the argon is 60 slpm
  • the flow of the helium is 40 slpm
  • the powder feeding rate is 10r/min
  • the spraying distance is 90mm
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -ZrO 2 -CeO 2 and has a thickness of 100 um. It is fully intelligent to obtain high-density SiC f /SiC Composite flame tube.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the PyC interface layer uses methane as the precursor, hydrogen as the reaction gas, and argon as the dilution gas.
  • the gas is introduced into the chemical vapor deposition furnace by the bubbling method.
  • the deposition temperature is 1400°C
  • the deposition pressure is 0.5KPa
  • the deposition time is 60min.
  • the thickness of the deposited interface layer is 2um;
  • the specific introduction of the Si 3 N 4 interface layer uses trichloromethyl silane and ammonia as precursors, hydrogen as the reaction gas, argon as the dilution gas, and the gas is introduced into the In the chemical vapor deposition furnace, the deposition temperature is 1400°C, the deposition pressure is 0.5KPa, the deposition time is 60min, and the thickness of the deposited interface layer is 2um;
  • the specific introduction of the BN interface layer uses boron chloride and ammonia as precursors, and hydrogen as the precursor
  • the reaction gas, argon is the diluent gas
  • the gas is introduced into the chemical vapor deposition furnace by bubbling method, the deposition temperature is 1400°C, the deposition pressure is 0.5KPa, the deposition time is 60min, and the thickness of the deposited interface layer is 2um; After cooling, SiC fibers with multiple continuous interface layers are obtained;
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly coat the epoxy resin release agent on the surface of the flame tube mold twice, and heat the flame tube mold to 50°C;
  • Step 2 Lay the SiC fiber with a volume content of 65% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Wind the prepreg unidirectional tape with a volume content of 70% of SiC fiber and the balance of resin on the surface of the mold laid in Step 2 by a winding machine, with a winding angle of 90° and a winding speed of 0.7m/s.
  • the winding tension is 10N/cm, and the winding thickness is 5mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and molding, the curing temperature is 90°C, and the curing time is 4 hours;
  • Step five demold the preform after curing and molding in step four, and perform product finishing on the preform by laser processing after demolding to obtain a net-size molded preform.
  • step 2) The preform obtained in step 2) is densified by chemical vapor deposition process and reactive melt infiltration process successively, and then low-temperature vacuum silicon infiltration is performed first.
  • the binary alloy of Si and Mo is used as the silicon source, and argon is used as the silicon source.
  • Dilution gas deposition temperature is 1800°C
  • deposition pressure is normal pressure
  • silicon infiltration time is 30min
  • cooling with furnace repeated once
  • chemical vapor deposition is carried out with trimethylsilane as precursor and hydrogen as reaction gas
  • Argon is the diluent gas.
  • the gas is introduced into the chemical vapor deposition furnace by bubbling.
  • the deposition temperature is 1200°C
  • the deposition pressure is 0.5KPa
  • the deposition time is 6000min.
  • the furnace is cooled and repeated once until the chemical vapor deposition.
  • the mass ratio of the SiC matrix formed by the process to the SiC matrix formed by the reactive melt infiltration process is 1:2;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the plasma gas includes argon and helium
  • the flow of the argon is 80 slpm
  • the flow of the helium is 60 slpm
  • the powder feeding rate is 35r/min
  • the spraying distance is 200mm
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -ZrO 2 -CeO 2 and has a thickness of 150 um. It is fully intelligent to obtain high-density SiC f /SiC Composite flame tube.
  • This embodiment provides an automated preparation method of a SiC f /SiC composite flame tube, which is characterized in that it includes the following steps:
  • the PyC interface layer uses methane as the precursor, hydrogen as the reaction gas, and argon as the dilution gas.
  • the gas is introduced into the chemical vapor deposition furnace by the bubbling method.
  • the deposition temperature is 1000°C
  • the deposition pressure is 8KPa
  • the deposition time is 300min.
  • the thickness of the deposited interface layer is 1um; the specific introduction of the Si 3 N 4 interface layer uses trichloromethylsilane and ammonia as precursors, hydrogen as the reaction gas, and argon as the dilution gas.
  • the gas is introduced into the chemical by bubbling method In the vapor deposition furnace, the deposition temperature is 1000°C, the deposition pressure is 8KPa, the deposition time is 300min, and the thickness of the deposited interface layer is 1um; the specific introduction of the BN interface layer uses boron chloride and ammonia as precursors, and hydrogen as the reaction gas , Argon is the diluent gas.
  • the gas is introduced into the chemical vapor deposition furnace by bubbling.
  • the deposition temperature is 1000°C
  • the deposition pressure is 8KPa
  • the deposition time is 300min
  • the thickness of the deposited interface layer is 1um; after the furnace is cooled, The SiC fiber with multiple continuous interface layers is obtained;
  • the SiC fiber with continuous interface layer obtained in step 1) is unidirectionally taped and wound, including the following steps:
  • Step 1 Use acetone to clean the surface of the flame tube mold to a state where no impurities are attached, and evenly coat the epoxy resin release agent on the surface of the flame tube mold twice, and heat the flame tube mold to 40°C;
  • Step 2 Lay the SiC fiber with a volume content of 55% and the prepreg unidirectional tape with the balance being resin on the surface of the flame tube mold respectively;
  • Step 3 Wrap a prepreg unidirectional tape with a volume content of 60% of SiC fiber and a balance of resin on the surface of the mold laid in step 2 through a winding machine, with a winding angle of 60° and a winding speed of 0.5m/s.
  • the winding tension is 6N/cm, and the winding thickness is 3mm;
  • Step 4 Put the material layer wound on the surface of the mold in step 3 into a curing furnace for curing and forming, the curing temperature is 120°C, and the curing time is 6 hours;
  • Step five demold the preform after curing and molding in step four, and perform product finishing on the preform by laser processing after demolding to obtain a net-size molded preform.
  • step 2) The preform obtained in step 2) is densified by chemical vapor deposition process and reactive melt infiltration process successively, and then low-temperature vacuum silicon infiltration is performed first.
  • the binary alloy of Si and Mo is used as the silicon source, and argon is used as the silicon source.
  • Dilution gas deposition temperature is 1600°C, deposition pressure is 1Pa, siliconizing time is 180min, using furnace cooling, repeated once; then chemical vapor deposition is performed with trimethylsilane as precursor, hydrogen as reaction gas, argon
  • the gas is the diluent gas.
  • the gas is introduced into the chemical vapor deposition furnace by bubbling method.
  • the deposition temperature is 1000°C
  • the deposition pressure is 3KPa
  • the deposition time is 4800min.
  • the furnace is cooled and repeated once until the chemical vapor deposition process is formed.
  • the mass ratio of SiC matrix to the SiC matrix formed by the reaction melt infiltration process is 1:1.5;
  • the preparation method of the environmental barrier coating includes the following steps:
  • the thickness ratio of the Si bonding layer, Yb 2 Si 2 O 7 intermediate layer and rare earth monosilicate Re 2 SiO 5 surface layer of 1:2:1, prepare the intermediate layer and the surface layer, and the preparation process
  • Plasma spraying method is used in both, and the plasma gas includes argon and helium, the flow of the argon is 70 slpm, the flow of the helium is 50 slpm, the powder feeding rate is 20r/min, and the spraying distance is 150mm,
  • the Yb 2 Si 2 O 7 powder and the Yb 2 Si 2 O 5 powder are sprayed on the preform in sequence to obtain a high-density and fully intelligent SiC f /SiC composite flame tube.
  • the thermal barrier coating is R 2 O 3 -ZrO 2 -CeO 2 and has a thickness of 120 um. It is fully intelligent to obtain high-density SiC f /SiC Composite flame tube.
  • Measurement method take samples of the SiC f /SiC composite flame tube prepared in Example 1 to Example 6 to make a mechanical property piece with a size of 3 ⁇ 4 ⁇ 40 (mm), and perform 500h aerobic Environment, normal temperature and high temperature environment treatment, among which the high temperature environment is 1400°C and 1600°C respectively.
  • Test results The test results of bending strength are shown in Table 1 below:
  • the volume density of the prepared SiC f /SiC composite flame tube is 2.75 g/m 3 , and the apparent porosity is 0.65%.
  • Measurement method Cut the specimens on the SiC f /SiC composite flame tube prepared in Examples 1 to 6, and place them in a completely enclosed space, respectively, and heat to 1100°C, 1200°C, 1300°C, and then place them at 20 In °C water, repeated heating and cooling treatments, visually check for cracking.
  • the thermal shock resistance performance is represented by the number of heating and cooling treatments. The more the number, the better the thermal shock resistance. It can be seen from Table 2 that the thermal shock resistance of Examples 1 to 6 is more excellent.
  • the average thermal conductivity of the prepared SiC f /SiC composite flame tube is 30 W/(m ⁇ K).
  • the average thermal expansion coefficient of the prepared SiC f /SiC composite flame tube is 3.65 ⁇ 10 -6 m/K.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Ceramic Products (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

一种SiCf/SiC复合材料火焰筒的自动化制备方法,包括如下步骤:将SiC纤维采用化学气相沉积法制备界面层,得到带连续界面层的SiC纤维;根据仿真模拟计算得到纤维体积和纤维走向,将得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,获得净尺寸成型的预制体;对得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理;然后在得到的预制体表面制备环境障碍涂层;最后继续在表面制备热障涂层,全智能化得到高致密度SiCf/SiC复合材料火焰筒。制备得到的SiCf/SiC复合材料火焰筒不仅具有耐高温、长寿命的特点,还具有低热膨胀系数、高热导率和高抗热震性能以及力学性能优异等优势,同时制备方法自动化程度高、生产周期短、成本低且质量可控。

Description

一种SiC f/SiC复合材料火焰筒及其自动化制备方法 技术领域
本发明涉及航空用结构材料技术领域,具体涉及一种SiC f/SiC复合材料火焰筒及其自动化制备方法。
背景技术
燃烧室是航空发动机的核心部件之一,其主要功能是将燃料的化学能经过燃烧转变为热能,以提高燃气在涡轮和喷管中膨胀的能力,在燃烧室的结构组成中,火焰筒是组织燃烧的场所,是保证空气分股、燃烧充分、掺混均匀并使壁面得到有效冷却的关键部件,燃烧室的可靠性、经济性和寿命在很大程度上取决于火焰筒的可靠性和耐温程度,因此研制高性能长寿命的燃烧室火焰筒对于提高发动机性能起着至关重要的作用。
现有的碳化硅纤维增强陶瓷基(SiC f/SiC)复合材料具有优异的性能,是代替高温合金作为航空发动机热端构件用材料的首选材料,然而服役环境中的应力作用会促使复合材料基体开裂,加速材料的损伤和腐蚀,影响其在高温燃气环境下服役长寿命的要求,从而严重制约SiC f/SiC复合材料在发动机燃烧室火焰筒的应用;如US20120076927A1的专利,提供了一种改善纤维增强硅碳复合材料的机械性能的方法,专利中通过对复合材料进行控制热处理,改进了纤维界面涂层和陶瓷基体,同时可以除去相基质中多余的硅,但是该专利中对处理时间-温度-环境条件的限定十分苛刻,热处理甚至达到1900℃的处理温度,在真空中或在纯度大于99%的惰性气体环境中处理保持时间长达100小时,另 外单纯采用CVI工艺制备陶瓷基,虽然能有效控制游离硅,但是不能保证材料的高致密性,不利于应用于市场,所以研发一种可低成本制备高致密度,同时还能除去多余硅的高性能SiC f/SiC复合材料火焰筒的制备方法显得尤为必要;
另外专利CN106966738B中采用三维四步法编织燃烧室火焰筒预制体,而连接部分采用纤维缝合技术,当火焰筒处于高温燃气环境中,会在连接处形成应力集中和轻微开裂,从而加速材料的损伤和腐蚀,严重制约着复合材料火焰筒性能的发挥;而且通过图1所示有限元法分析火焰筒温度场分布图可以看出,火焰筒冷、热端之间具有约240℃的温差,并且火焰筒内部的温度变化梯度较大,所以温差会使材料内部产生应力,进而产生裂纹,所以要求火焰筒必须具有低的热膨胀系数,以保证温度变化时构件尺寸的稳定性,同时,必须具有高热导率,避免因为热应力集中而造成的火焰筒失效;同时目前三维四步的编织方法基本全部采用手工编织的方式,成本高、工期长、质量不可控,因此研制自动化的连续制备火焰筒预制体对于SiC f/SiC复合材料在火焰筒的广泛应用有至关重要的作用。
发明内容
针对现有技术存在的上述问题,本申请提供了一种SiC f/SiC复合材料火焰筒及其自动化制备方法,制备得到的SiC f/SiC复合材料火焰筒不仅具有耐高温、长寿命的特点,还具有低热膨胀系数、高热导率和高抗热震性能以及力学性能优异等优势,同时制备方法自动化程度高、生产周期短、成本低且质量可控。
本发明的技术方案如下:一种SiC f/SiC复合材料火焰筒的自动化制备方法,包括如下步骤:
1)将SiC纤维采用化学气相沉积法制备界面层,得到带连续界面层的SiC 纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,获得净尺寸成型的预制体;
3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1~1∶2;
4)在步骤3)得到的预制体表面制备环境障碍涂层,所述环境障碍涂层的厚度为60~150um;
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层的厚度为100~150um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
本发明仿真模拟包括有限元分析法分析温度场、以及联合采用多尺度分析与有限元实体建模相结合的方法,根据温度场分析、指导复合材料火焰筒构件的设计、纤维体积、纤维走向以及复合材料的成型方式等参数,以达到提高SiC f/SiC复合材料火焰筒性能预测的效率和精度,实现制备方法的自动化和高效性的目的。
本发明所述步骤1)中的界面层为PyC、SiC、B 4C、ZrC、HfC、TaC、Si 3N 4、BN中的一种或多种。
本发明所述化学气相沉淀工艺具体为:根据引入的界面层选择前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500~1400℃,沉积压力为0.5~12KPa,沉积时间为60~600min,沉积的界面层厚度为100nm~2μm;所述前驱体为甲烷、三氯甲基硅烷、氯化硼、氯化锆、氯化钽、氯化硅、卤化硼、氨气中的一种或几种。
本发明所述步骤2)单向带铺带、缠绕成型包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2~3次的环氧树脂脱模剂,并对火焰筒模具加热到30~50℃;
步骤二、将体积含量为40~65%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为50~70%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,由内向外以缠绕张力梯度递减的方式进行缠绕,缠绕角度为30~90°,缠绕速度为0.3~0.7m/s,缠绕张力为2~10N/cm,缠绕厚度为1~5mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为90~165℃,固化时间为4~8h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用磨削加工及激光加工相结合方式进行产品精加工,即得到净尺寸成型的预制件。
本发明所述步骤3)反应熔体浸渗工艺具体为熔融渗硅工艺:设备为真空高温气氛沉积炉和真空高温渗硅炉,以硅合金为硅源,氩气为稀释气体,沉积温度为1450~1800℃,沉积压力为2Pa~常压,渗硅时间为30~300min;所述硅合金为Si与Ta、Hf、Mo、W、Zr、Ti、B、Be的二元或三元的合金。
本发明所述步骤3)的化学气相沉积工艺具体为,以三氯甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度900~1200℃,沉积压力为0.5~5KPa,沉积时间为60~6000min。
本发明所述步骤4)中的环境障碍涂层包括Si粘结层、稀土单硅酸盐Re 2SiO 5面层、以及位于所述粘结层和面层之间的Yb 2Si 2O 7中间层;所述Si粘结层、 Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1~2:1~2:1~3;所述稀土单硅酸盐Re 2SiO 5选自Y 2SiO 5、Sc 2SiO 5、Gd 2SiO 5、Er 2SiO 5、Tm 2SiO 5、Yb 2SiO 5、Lu 2SiO 5中的至少一种。
本发明所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Re 2SiO 5分别进行球磨处理,直至粒径为20~80um;
(2)将预制件置于惰性保护气氛中,在1450~1800℃下热处理1~4h,形成Si粘结层;
(3)采用等离子体喷涂法,将Yb 2Si 2O 7粉体喷涂在带有Si粘结层的预制件上,形成中间层;
(4)采用等离子体喷涂法,将稀土单硅酸盐Re 2SiO 5粉体喷涂在带有粘结层和中间层的预制件上,得到所述环境障碍涂层。
所述等离子喷涂法的参数包括:等离子气体包括氩气与氦气,所述氩气的流量为60~80slpm,所述氦气的流量为40~60slpm,送粉速率为10~35r/min,喷涂距离为90~200mm。
本发明所述步骤5)所述热障涂层为R 2O 3、ZrO 2、CeO 2、Al 2O 3·2SiO 2、SrZrO 3、La 2Zr 2O 7、La 2Ce 2O 7中的至少一种。
本发明还提供了一种SiC f/SiC复合材料火焰筒。
本发明有益的技术效果在于:
(1)本发明在纤维与基体之间引入均匀界面层,使得纤维与基体不会融为一体,层次分明的纤维-界面层-基体结构能够吸收裂纹扩散所需要的能量,有效提高了复合材料的力学强度;同时陶瓷界面层的存在,能够保护SiC纤维遭受氧气、水蒸气、燃油、酸等的腐蚀,从而提高使用温度与使用环境。
(2)本发明联合采用化学气相沉积工艺(CVI)和反应熔渗工艺(MI)对 陶瓷基复合材料进行致密化处理,一方面MI工艺简单,周期短,MI-SiC/SiC具有更高的密度和更低的显气孔率,因此复合材料具有更高的热导率,尤其是垂直纤维方向的热导率,MI-SiC/SiC是CVI-SiC/SiC复合材料的2倍多,有利于抗热震性能的改善,另一方面根据实验数据得知MI-SiC/SiC复合材料的热膨胀系数大于CVI-SiC/SiC复合材料,而通过优化工艺参数,调控复合材料基体组成与结构,从而实现材料热膨胀系数的可调控性,并获得具有低热膨胀系数的材料和空间光学用支撑构件,有效降低材料受热不均产生的形变程度,提高SiC f/SiC复合材料火焰筒的使用寿命;同时本发明采用反应熔渗工艺中的处理温度低于常规温度,可有效降低复合材料表面的硅含量,从而提高复合材料的耐高温性能。
(3)本发明根据仿真模拟计算得到的纤维体积和纤维走向,采用单向带铺带、缠绕成型的自动化方式进行预制件的制备,使得在获得三维预制体的同时,延厚度方向,纤维布间的距离达到最低,且纤维布都保持平整性,这样既提高了纤维体积含量,还保证了纤维的分布均匀性,该方法制成的复合材料火焰筒具有轻质、强度高、无微裂纹的优势,同时还具有耐高温、抗磨损、防渗漏的特点,同时自动化程度高、生产周期短、成本低且质量可控。
(4)本发明中的环境障碍涂层选用Si层,考虑Si具有更高的熔点,因此可以保证环境障碍涂层具有更高的环境适用温度;中间层材料采用Yb 2Si 2O 7,考虑Yb 2Si 2O 7的热膨胀系数较小,显著低于稀土单硅酸盐Re 2SiO 5面层的热膨胀系数,使得在热循环过程中,不容易被裂纹贯穿,有利于提高涂层的抗热震性能,另一方面本发明稀土硅酸盐Re 2SiO 5面层具有优异的耐水蒸气腐蚀性能,可以进一步提高涂层体系的防护性能。
(5)本发明在制备Si层中,采用高温反应热处理的方法形成Si层,可以 进一步降低复合材料表面的硅含量,从而提高复合材料的耐高温性能,另一方面通过优化热处理温度提高碳化硅涂层的晶粒尺寸和涂层致密度,从而获得耐高温、致密度高的复合材料火焰筒。
(6)本发明首先通过有限元法分析复合材料火焰筒的温度场,然后采用多尺度分析与有限元实体建模相结合的方法,将细观、宏观相结合,获取结构的确定性载荷以及载荷处的纤维基体状态,进行指导复合材料火焰筒构件的设计、纤维体积、纤维走向以及复合材料的成型方式等参数,提高了SiC f/SiC复合材料火焰筒性能预测的效率和精度,实现制备方法的自动化和高效性。
附图说明
图1为本发明SiC f/SiC复合材料火焰筒有限元计算的温度场示意图。
图2为本发明SiC f/SiC复合材料火焰筒的制备流程示意图。
图3为实施例3的PyC/Si 3N 4/BN多层界面层的扫描电镜图。
图4为本发明MI SiC/CVI SiC基体的扫描电镜图。
图5为本发明EBC环境障碍层的扫描电镜图。
图6为本发明EBC环境障碍层的表面放大图。
图7为本发明的热防护涂层结构设计图。
图8为本发明单向带铺放、缠绕成型的结构示意图。
图9为本发明SiC f/SiC复合材料火焰筒的立体图。
图10为实施例1经1100℃×20min热震不同次数后的表观状态和截面形貌。
图11为实施例1经1200℃×20min热震不同次数后的表观状态和截面形貌。
图12为实施例1经1300℃×20min热震不同次数后的表观状态和截面形貌。
下面结合附图和实施例,对本发明进行具体描述,显然,所描述的实施例 仅是本发明一部分实施例,而不是全部的实施例,基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下结合具体优选实施例对本发明一种SiC f/SiC复合材料火焰筒的制备方法进行详细阐述。
实施例1:
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中,以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500℃,沉积压力为12KPa,沉积时间为600min,沉积的界面层厚度为100nm;随炉冷却后,即得到带连续PyC界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂,并对火焰筒模具加热到30℃;
步骤二、将体积含量为40%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为50%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为30°,缠绕速度为0.3m/s,缠绕张力为2N/cm,缠绕厚度为1mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为90℃,固化时间为4h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件;
3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理,先进行低温真空渗硅,以Si与Ta的二元合金作为硅源,氩气为稀释气体,沉积温度为1400℃,沉积压力为常压,渗硅时间为300min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为900℃,沉积压力为5KPa,沉积时间为6000min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:1;
4)在步骤3)得到的预制体表面制备60um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为20um;
(2)将预制件置于惰性保护气氛中,在1450℃下热处理4h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1:1:1,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为60slpm,所述氦气的流量为40slpm,送粉速率为10r/min,喷涂距离为90mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-Al 2O 3,厚度为100um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
实施例2:
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中,以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1400℃,沉积压力为0.5KPa,沉积时间为60min,沉积的界面层厚度为2um;随炉冷却后,即得到带连续界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆3次的环氧树脂脱模剂,并对火焰筒模具加热到50℃;
步骤二、将体积含量为65%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为70%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为90°,缠绕速度为0.7m/s,缠绕张力为10N/cm,缠绕厚度为5mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为165℃,固化时间为8h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理,先进行低温真空渗硅,以Si与Ta的二元合金作为硅源,氩气为稀释气体,沉积温度为1800℃,沉积压力为2Pa,渗硅时间为30min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1200℃,沉积压力为0.5KPa,沉积时间为60min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:2;
4)在步骤3)得到的预制体表面制备150um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为80um;
(2)将预制件置于惰性保护气氛中,在1800℃下热处理1h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为2:2:3,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为80slpm,所述氦气的流量为60slpm,送粉速率为35r/min,喷涂距离为200mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-Al 2O 3,厚度为150um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
实施例3
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征 在于,包括如下步骤:
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中,以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1000℃,沉积压力为8KPa,沉积时间为300min,沉积的界面层厚度为1um;随炉冷却后,即得到带连续界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂,并对火焰筒模具加热到40℃;
步骤二、将体积含量为55%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为60%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为60°,缠绕速度为0.5m/s,缠绕张力为6N/cm,缠绕厚度为3mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为120℃,固化时间为6h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理,先进行低温真空渗硅,以Si与Ta的二元合金作为硅源,氩气为稀释气体,沉积温度为1600℃,沉积压力为1Pa,渗硅时间为180min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中, 沉积温度为1000℃,沉积压力为3KPa,沉积时间为4800min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:1.5;
4)在步骤3)得到的预制体表面制备100um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为50um;
(2)将预制件置于惰性保护气氛中,在1600℃下热处理3h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1:2:1,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为70slpm,所述氦气的流量为50slpm,送粉速率为20r/min,喷涂距离为120mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-Al 2O 3,厚度为120um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
实施例4
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
1)将SiC纤维先后置于PyC界面层、Si 3N 4界面层和BN界面层相应的化学气相沉积温度的电阻炉中,引入PyC/Si 3N 4/BN多层界面层,具体的引入PyC界面层以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500℃,沉积压力为12KPa,沉积时 间为600min,沉积的界面层厚度为100nm;具体的引入Si 3N 4界面层以三氯甲基硅烷和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500℃,沉积压力为0.5KPa,沉积时间为600min,沉积的界面层厚度为100nm;具体的引入BN界面层以氯化硼和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500℃,沉积压力为12KPa,沉积时间为600min,沉积的界面层厚度为100nm;随炉冷却后,即得到带多层连续界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂,并对火焰筒模具加热到30℃;
步骤二、将体积含量为40%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为50%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为30°,缠绕速度为0.3m/s,缠绕张力为2N/cm,缠绕厚度为1mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为90℃,固化时间为4h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理,先进行低温真空渗硅,以Si与Mo的二元合金作为硅源, 氩气为稀释气体,沉积温度为1400℃,沉积压力为2Pa,渗硅时间为300min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为900℃,沉积压力为5KPa,沉积时间为60min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:1;
4)在步骤3)得到的预制体表面制备60um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为20um;
(2)将预制件置于惰性保护气氛中,在1450℃下热处理4h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1:1:1,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为60slpm,所述氦气的流量为40slpm,送粉速率为10r/min,喷涂距离为90mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-ZrO 2-CeO 2,厚度为100um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
实施例5
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
1)将SiC纤维先后置于PyC界面层、Si 3N 4界面层和BN界面层相应的化学气相沉积温度的电阻炉中,引入PyC/Si 3N 4/BN多层界面层,具体的引入PyC界面层以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1400℃,沉积压力为0.5KPa,沉积时间为60min,沉积的界面层厚度为2um;具体的引入Si 3N 4界面层以三氯甲基硅烷和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1400℃,沉积压力为0.5KPa,沉积时间为60min,沉积的界面层厚度为2um;具体的引入BN界面层以氯化硼和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1400℃,沉积压力为0.5KPa,沉积时间为60min,沉积的界面层厚度为2um;随炉冷却后,即得到带多层连续界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂,并对火焰筒模具加热到50℃;
步骤二、将体积含量为65%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为70%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为90°,缠绕速度为0.7m/s,缠绕张力为10N/cm,缠绕厚度为5mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为90℃,固化时间为4h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理,先进行低温真空渗硅,以Si与Mo的二元合金作为硅源,氩气为稀释气体,沉积温度为1800℃,沉积压力为常压,渗硅时间为30min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1200℃,沉积压力为0.5KPa,沉积时间为6000min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:2;
4)在步骤3)得到的预制体表面制备150um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为80um;
(2)将预制件置于惰性保护气氛中,在1800℃下热处理1h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为2:2:3,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为80slpm,所述氦气的流量为60slpm,送粉速率为35r/min,喷涂距离为200mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-ZrO 2-CeO 2,厚度为150um,全智能化得到高致密度SiC f/SiC复合材料火 焰筒。
实施例6
本实施例提供了一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
1)将SiC纤维先后置于PyC界面层、Si 3N 4界面层和BN界面层相应的化学气相沉积温度的电阻炉中,引入PyC/Si 3N 4/BN多层界面层,具体的引入PyC界面层以甲烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1000℃,沉积压力为8KPa,沉积时间为300min,沉积的界面层厚度为1um;具体的引入Si 3N 4界面层以三氯甲基硅烷和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1000℃,沉积压力为8KPa,沉积时间为300min,沉积的界面层厚度为1um;具体的引入BN界面层以氯化硼和氨气为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1000℃,沉积压力为8KPa,沉积时间为300min,沉积的界面层厚度为1um;随炉冷却后,即得到带多层连续界面层的SiC纤维;
2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,包括如下步骤:
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂,并对火焰筒模具加热到40℃;
步骤二、将体积含量为55%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
步骤三、通过缠绕机将体积含量为60%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,缠绕角度为60°,缠绕速度为0.5m/s,缠绕张力为6N/cm,缠绕厚度为3mm;
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为120℃,固化时间为6h;
步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用激光加工方式进行产品精加工,即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理,先进行低温真空渗硅,以Si与Mo的二元合金作为硅源,氩气为稀释气体,沉积温度为1600℃,沉积压力为1Pa,渗硅时间为180min,采用随炉冷却,重复1次;再进行化学气相沉积,以三甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为1000℃,沉积压力为3KPa,沉积时间为4800min,采用随炉冷却,重复1次,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1:1.5;
4)在步骤3)得到的预制体表面制备100um厚的环境障碍涂层,所述环境障碍涂层的制备方法,包括以下步骤:
(1)对Yb 2Si 2O 7和Yb 2Si 2O 5分别进行球磨处理,直至粒径为60um;
(2)将预制件置于惰性保护气氛中,在1600℃下热处理2h,形成Si粘结层;
(3)按照Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1:2:1,对中间层和面层进行制备,制备过程中均采用等离子体喷涂法,具体为等离子气体包括氩气与氦气,所述氩气的流量为70slpm,所述氦气的流 量为50slpm,送粉速率为20r/min,喷涂距离为150mm,依次将Yb 2Si 2O 7粉体和Yb 2Si 2O 5粉体喷涂在预制件上,得到高致密度全智能化的SiC f/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层为R 2O 3-ZrO 2-CeO 2,厚度为120um,全智能化得到高致密度SiC f/SiC复合材料火焰筒。
测试例
将实施例一到实施例六制备得到的SiC f/SiC复合材料火焰筒进行性能测试,并且将常规的火焰筒作为对比例,具体如下:
1、高温耐氧化性能
测定方法:将实施例一到实施例六制备的SiC f/SiC复合材料火焰筒截取试样,制成尺寸为3×4×40(mm)的力学性能件,对试件进行500h的有氧环境、常温和高温环境处理,其中高温环境分别为1400℃和1600℃。
测试结果:测试的弯曲强度结果如下表1所示:
表1不同温度下SiC f/SiC复合材料火焰筒的弯曲强度
Figure PCTCN2020101903-appb-000001
Figure PCTCN2020101903-appb-000002
2、密度和孔隙率
测定方法:将实施例一至六制备得到的SiC f/SiC复合材料火焰筒根据GB/T1966-1996《多孔陶瓷显气孔率、容量试验方法》进行检测。
测定结果:制备得到的SiC f/SiC复合材料火焰筒的体积密度为2.75g/m 3,显孔隙率为0.65%。
3、抗热震性能
测定方法:将实施例一至六制备得到的SiC f/SiC复合材料火焰筒上切割试样件,分别放置在完全密闭的空间内,分别加热至1100℃、1200℃、1300℃,接着置于20℃水中,反复的升温、冷却处理,目测有无开裂现象。
测定结果:测试的抗震性能如下表2所示:
表2不同温度下SiC f/SiC复合材料火焰筒的抗热震性能
Figure PCTCN2020101903-appb-000003
抗热震性能的优劣通过升温、冷却处理的次数表示,次数越多,抗热震性能越好;从表2中可以看出实施例一至六的抗热震性能更加优异。
4、热导率
测定方法:将实施例一至六制备得到的SiC f/SiC复合材料火焰筒根据GB/T17911.8-2002《耐火陶瓷纤维制品导热系数试验方法》进行检测。
测定结果:制备得到的SiC f/SiC复合材料火焰筒的平均热导率为30W/(m·K)。
5、热膨胀系数
测定方法:将实施例一至六制备得到的SiC f/SiC复合材料火焰筒根据GB/T16535-1996《工程陶瓷线热膨胀系数试验方法》进行检测。
测定结果:制备得到的SiC f/SiC复合材料火焰筒的平均热膨胀系数为3.65×10 -6m/K。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,对于本领域的普通技术人员而言,在不脱离本发明的原理的情况下可以对这些实施例进行多种变化、修改、替换和变型,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。

Claims (8)

  1. 一种SiC f/SiC复合材料火焰筒的自动化制备方法,其特征在于,包括如下步骤:
    1)将SiC纤维采用化学气相沉积法制备界面层,得到带连续界面层的SiC纤维;
    2)根据仿真模拟计算得到的纤维体积和纤维走向,将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型,获得净尺寸成型的预制体;
    3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理,直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1~1∶2;
    4)在步骤3)得到的预制体表面制备环境障碍涂层,所述环境障碍涂层的厚度为60~150um;
    5)在步骤4)得到的预制体表面制备热障涂层,所述热障涂层的厚度为100~150um,全智能化得到高致密度SiC f/SiC复合材料火焰筒;
    所述步骤2)单向带铺带、缠绕成型包括如下步骤:
    步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态,在火焰筒模具表面均匀涂覆2~3次的环氧树脂脱模剂,并对火焰筒模具加热到30~50℃;
    步骤二、将体积含量为40~65%的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上;
    步骤三、通过缠绕机将体积含量为50~70%的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上,由内向外以缠绕张力梯度递减的方 式进行缠绕,缠绕角度为30~90°,缠绕速度为0.3~0.7m/s,缠绕张力为2~10N/cm,缠绕厚度为1~5mm;
    步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型,固化温度为90~165℃,固化时间为4~8h;
    步骤五、将经步骤四固化成型后的预制体进行脱模,脱模后对预制体采用磨削加工及激光加工相结合方式进行产品精加工,即得到净尺寸成型的预制件;
    所述步骤3)反应熔体浸渗工艺具体为熔融渗硅工艺:设备为真空高温气氛沉积炉和真空高温渗硅炉,以硅或硅合金为硅源,氩气为稀释气体,沉积温度为1400~1800℃,沉积压力为2Pa~常压,渗硅时间为30~300min;
    所述硅合金为Si与Ta、Hf、Mo、W、Zr、Ti、B、Be的二元或三元的合金。
  2. 根据权利要求1所述的制备方法,其特征在于,所述步骤1)中的界面层为PyC、SiC、B 4C、ZrC、HfC、TaC、Si 3N 4、BN中的一种或多种。
  3. 根据权利要求1所述的制备方法,其特征在于,所述步骤1)中,所述化学气相沉积工艺具体为:根据引入的界面层选择前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度为500~1400℃,沉积压力为0.5~12KPa,沉积时间为60~600min,沉积的界面层厚度为100nm~2μm;
    所述前驱体为甲烷、三氯甲基硅烷、氯化硼、氯化锆、氯化钽、氯化硅、卤化硼、氨气中的一种或几种。
  4. 根据权利要求1所述的制备方法,其特征在于,所述步骤3)的化学气相沉积工艺具体为,以三氯甲基硅烷为前驱体,氢气为反应气体,氩气为稀释气体,通过鼓泡法将气体引入到化学气相沉积炉中,沉积温度900~1200℃,沉积压力为0.5~5KPa,沉积时间为60~6000min。
  5. 根据权利要求1所述的制备方法,其特征在于,所述步骤4)中的环境障碍涂层包括Si粘结层、稀土单硅酸盐Re 2SiO 5面层、以及位于所述粘结层和面层之间的Yb 2Si 2O 7中间层;
    所述Si粘结层、Yb 2Si 2O 7中间层和稀土单硅酸盐Re 2SiO 5面层的厚度比为1~2:1~2:1~3;
    所述稀土单硅酸盐Re 2SiO 5选自Y 2SiO 5、Sc 2SiO 5、Gd 2SiO 5、Er 2SiO 5、Tm 2SiO 5、Yb 2SiO 5、Lu 2SiO 5中的至少一种。
  6. 根据权利要求7所述的制备方法,其特征在于,所述环境障碍涂层的制备方法,包括以下步骤:
    (1)对Yb 2Si 2O 7和Re 2SiO 5分别进行球磨处理,直至粒径为20~80um;
    (2)将预制件置于惰性保护气氛中,在1450~1800℃下热处理1~4h,形成Si粘结层;
    (3)采用等离子体喷涂法,将Yb 2Si 2O 7粉体喷涂在带有Si粘结层的预制件上,形成中间层;
    (4)采用等离子体喷涂法,将稀土单硅酸盐Re 2SiO 5粉体喷涂在带有粘结层和中间层的预制件上,得到所述环境障碍涂层。
    所述等离子喷涂法的参数包括:等离子气体包括氩气与氦气,所述氩气的流量为60~80slpm,所述氦气的流量为40~60slpm,送粉速率为10~35r/min,喷涂距离为90~200mm。
  7. 根据权利要求1所述的制备方法,其特征在于,所述步骤5)所述热障涂层为R 2O 3、ZrO 2、CeO 2、Al 2O 3·2SiO 2、SrZrO 3、La 2Zr 2O 7、La 2Ce 2O 7中的至少一种。
  8. 根据权利要求1~9任一项所述的方法制备得到的SiC f/SiC复合材料火焰筒。
PCT/CN2020/101903 2019-08-15 2020-07-14 一种SiCf/SiC复合材料火焰筒及其自动化制备方法 WO2021027469A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US17/474,091 US11591267B2 (en) 2019-08-15 2021-09-14 Automated preparation method of a SiCf/SiC composite flame tube

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910688219.8 2019-08-15
CN201910688219.8A CN110330353B (zh) 2019-08-15 2019-08-15 一种SiCf/SiC复合材料火焰筒及其自动化制备方法

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US17/474,091 Continuation US11591267B2 (en) 2019-08-15 2021-09-14 Automated preparation method of a SiCf/SiC composite flame tube

Publications (1)

Publication Number Publication Date
WO2021027469A1 true WO2021027469A1 (zh) 2021-02-18

Family

ID=68147938

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2020/101903 WO2021027469A1 (zh) 2019-08-15 2020-07-14 一种SiCf/SiC复合材料火焰筒及其自动化制备方法

Country Status (3)

Country Link
US (1) US11591267B2 (zh)
CN (1) CN110330353B (zh)
WO (1) WO2021027469A1 (zh)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114853480A (zh) * 2022-04-17 2022-08-05 西北工业大学 一种高温透波氮化物复合材料天线罩的低成本快速制备方法
CN116253584A (zh) * 2023-02-15 2023-06-13 中国航发北京航空材料研究院 一种用于陶瓷基复合材料的全氧化物热/环境障涂层及其制备方法
CN117003572A (zh) * 2023-08-01 2023-11-07 上海大学 一种沉积PyC/SiC界面相的制备方法、陶瓷基复合材料
CN117285362A (zh) * 2023-11-23 2023-12-26 中国航发北京航空材料研究院 SiC/SiC复合材料耐高温抗氧化界面层及制备方法

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330353B (zh) * 2019-08-15 2020-03-13 中南大学 一种SiCf/SiC复合材料火焰筒及其自动化制备方法
CN110985134B (zh) * 2019-12-13 2022-06-21 西安鑫垚陶瓷复合材料有限公司 航空发动机陶瓷基复合材料固定导向器叶片结构及其成型
CN111606715A (zh) * 2020-05-14 2020-09-01 湖南太子新材料科技有限公司 一种碳化硅纤维增强碳化硅复合材料的制备方法
CN111704468A (zh) * 2020-06-19 2020-09-25 宜兴市新立织造有限公司 一种三维机织航空火焰筒及其制备方法
CN112430111A (zh) * 2020-11-19 2021-03-02 航天特种材料及工艺技术研究所 一种自愈合改性SiC/SiC复合材料及其制备方法
CN112784401B (zh) * 2020-12-31 2024-08-09 南京玻璃纤维研究设计院有限公司 一种纤维预制体cvi致密化过程的仿真方法
US12006269B2 (en) * 2021-08-25 2024-06-11 Honeywell International Inc. Multilayer protective coating systems for gas turbine engine applications and methods for fabricating the same
CN114169186B (zh) * 2021-11-03 2024-09-20 南京航空航天大学 一种SiC纤维增强陶瓷基复合材料氧化-力学耦合本构模型建立及计算方法
CN114484505B (zh) * 2022-01-27 2023-05-16 西安鑫垚陶瓷复合材料有限公司 陶瓷基复合材料全环型火焰筒、定型模具及其制备方法
CN114582445B (zh) * 2022-03-10 2024-06-21 湖南大学 一种超材料的优化方法、系统及设备
CN114671710B (zh) * 2022-03-10 2023-04-07 西北工业大学 一种双周期多层TaC/HfC超高温陶瓷抗烧蚀涂层及制备方法
CN115536416B (zh) * 2022-08-28 2023-07-28 西北工业大学 一种高温高强高致密SiC/SiC复合材料及制备方法
CN115677385B (zh) * 2022-10-25 2023-09-08 哈尔滨工业大学 一种陶瓷基复合材料表面耐温达1300℃的可磨耗复合涂层的制备方法
CN116969764A (zh) * 2023-07-05 2023-10-31 西安鑫垚陶瓷复合材料股份有限公司 一种热模压结合CVI制备Diamond/SiC复合材料的方法
CN117902899B (zh) * 2024-03-18 2024-06-04 中南大学 一种稀土一体化改性C/C-UHTCs复合材料及其制备方法
CN118005418B (zh) * 2024-04-07 2024-08-13 西北工业大学宁波研究院 一种陶瓷基复合材料及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104010992A (zh) * 2011-12-29 2014-08-27 通用电气公司 制造陶瓷基质复合材料的方法和由此形成的陶瓷基质复合材料
CN105189932A (zh) * 2013-03-15 2015-12-23 通用电气公司 抗凹陷陶瓷基体复合物和环境阻隔涂层
CN106977219A (zh) * 2016-11-25 2017-07-25 北京航空航天大学 连续纤维增强陶瓷基复合材料火焰稳定器及其制备方法与应用
WO2018216816A1 (ja) * 2017-05-25 2018-11-29 イビデン株式会社 SiC/SiC複合材の製造方法
CN110330353A (zh) * 2019-08-15 2019-10-15 中南大学 一种SiCf/SiC复合材料火焰筒及其自动化制备方法

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5015540A (en) * 1987-06-01 1991-05-14 General Electric Company Fiber-containing composite
US5336350A (en) * 1989-10-31 1994-08-09 General Electric Company Process for making composite containing fibrous material
US5290491A (en) * 1990-04-02 1994-03-01 Societe Europeenne De Propulsion Process for the manufacture of a thermostructural composite material having a carbon interphase between its reinforcement fibers and its matrix
KR101101244B1 (ko) * 2009-05-14 2012-01-04 한국원자력연구원 고밀도 탄화규소 섬유강화 탄화규소 복합체(SiCf/SiC)의 제조방법
CN101555139B (zh) * 2009-05-20 2011-09-21 中国人民解放军国防科学技术大学 化学气相沉积碳与气相渗硅工艺联合制备SiCf/SiC复合材料的方法
US10807912B1 (en) * 2012-06-22 2020-10-20 United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration Advanced high temperature environmental barrier coating systems for SiC/SiC ceramic matrix composites
EP3010024B1 (en) * 2013-06-12 2017-11-08 Hitachi, Ltd. Tubular body and method for manufacturing tubular body
CN103979993B (zh) * 2014-05-27 2015-07-29 西安超码科技有限公司 一种大尺寸炭/碳化硅复合材料隔热底板的制备方法
CN203980349U (zh) 2014-06-04 2014-12-03 中国航空动力机械研究所 用于航空发动机燃烧室的火焰筒及航空发动机
GB2540769A (en) * 2015-07-27 2017-02-01 Rolls Royce Plc Combustor for a gas turbine engine
US10604454B1 (en) * 2016-06-16 2020-03-31 United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration Advanced high temperature environmental barrier coating for SiC/SiC ceramic matrix composites
EP3385407A3 (en) * 2017-04-03 2019-03-13 Rolls-Royce Corporation Cmas-resistant environmental barrier and thermal barrier coatings
CN109468568B (zh) * 2017-09-07 2021-02-12 中国科学院上海硅酸盐研究所 一种抗裂纹扩展的稀土硅酸盐环境障碍涂层及制备方法
CN108794040B (zh) * 2018-06-29 2021-02-09 航天材料及工艺研究所 一种基于熔融渗硅工艺的复合材料、碳/碳多孔体及其制备方法
CN113365963B (zh) * 2018-12-18 2023-10-31 欧瑞康美科(美国)公司 用于保护ebc和cmc层的涂层及其热喷涂方法
US20210017090A1 (en) * 2019-07-19 2021-01-21 Rolls-Royce Corporation Thermal spray deposited coating
CN111561713B (zh) 2020-04-16 2021-08-06 中国航发湖南动力机械研究所 直流燃烧室火焰筒
CN212029598U (zh) 2020-04-22 2020-11-27 上海慕帆动力科技有限公司 一种火焰筒双层壁间隙支撑件及火焰筒

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104010992A (zh) * 2011-12-29 2014-08-27 通用电气公司 制造陶瓷基质复合材料的方法和由此形成的陶瓷基质复合材料
CN105189932A (zh) * 2013-03-15 2015-12-23 通用电气公司 抗凹陷陶瓷基体复合物和环境阻隔涂层
CN106977219A (zh) * 2016-11-25 2017-07-25 北京航空航天大学 连续纤维增强陶瓷基复合材料火焰稳定器及其制备方法与应用
WO2018216816A1 (ja) * 2017-05-25 2018-11-29 イビデン株式会社 SiC/SiC複合材の製造方法
CN110330353A (zh) * 2019-08-15 2019-10-15 中南大学 一种SiCf/SiC复合材料火焰筒及其自动化制备方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114853480A (zh) * 2022-04-17 2022-08-05 西北工业大学 一种高温透波氮化物复合材料天线罩的低成本快速制备方法
CN114853480B (zh) * 2022-04-17 2023-08-18 西北工业大学 一种高温透波氮化物复合材料天线罩的低成本快速制备方法
CN116253584A (zh) * 2023-02-15 2023-06-13 中国航发北京航空材料研究院 一种用于陶瓷基复合材料的全氧化物热/环境障涂层及其制备方法
CN116253584B (zh) * 2023-02-15 2024-05-24 中国航发北京航空材料研究院 一种用于陶瓷基复合材料的全氧化物热/环境障涂层及其制备方法
CN117003572A (zh) * 2023-08-01 2023-11-07 上海大学 一种沉积PyC/SiC界面相的制备方法、陶瓷基复合材料
CN117003572B (zh) * 2023-08-01 2024-05-07 上海大学 一种沉积PyC/SiC界面相的制备方法、陶瓷基复合材料
CN117285362A (zh) * 2023-11-23 2023-12-26 中国航发北京航空材料研究院 SiC/SiC复合材料耐高温抗氧化界面层及制备方法
CN117285362B (zh) * 2023-11-23 2024-02-02 中国航发北京航空材料研究院 SiC/SiC复合材料耐高温抗氧化界面层及制备方法

Also Published As

Publication number Publication date
US20220055954A1 (en) 2022-02-24
CN110330353B (zh) 2020-03-13
US11591267B2 (en) 2023-02-28
CN110330353A (zh) 2019-10-15

Similar Documents

Publication Publication Date Title
WO2021027469A1 (zh) 一种SiCf/SiC复合材料火焰筒及其自动化制备方法
Wang et al. A review of third generation SiC fibers and SiCf/SiC composites
US10202854B2 (en) Abrasive tips for ceramic matrix composite blades and methods for making the same
RU2504030C2 (ru) Оболочка ядерного топлива с высокой удельной теплопроводностью и способ ее производства
Naslain Design, preparation and properties of non-oxide CMCs for application in engines and nuclear reactors: an overview
CN106977217B (zh) 一种高强高韧性碳化硅纤维增强碳化硅陶瓷基复合材料的制备方法
JP4740716B2 (ja) 層間強度を向上させるために非被覆繊維を組み込んだSiC/SiC複合材
Zhao et al. Construction of sandwich-structured C/C-SiC and C/C-SiC-ZrC composites with good mechanical and anti-ablation properties
CN105152671B (zh) SiCf/SiC复合材料的界面改性方法
US7510742B2 (en) Multilayered boron nitride/silicon nitride fiber coatings
CN106342033B (zh) 碳纤维增强超高温陶瓷基复合材料的制备方法
CN111217616B (zh) 一种近零膨胀特性的C/SiC结构材料的制备方法
JP2005240797A (ja) タービンエンジン部品用のSiC/SiCセラミック複合材の特性を改良するバイアス織物の使用
Luan et al. Wet oxidation behavior of SiC/(SiC‐SiBCN) x composites prepared by CVI combined with PIOP process
CN112374917B (zh) 一种高温陶瓷涂层及其制备方法
EP2931679B1 (en) Composite components with coated fiber reinforcements
US20100284810A1 (en) Process for inhibiting delamination in a bend of a continuous fiber-reinforced composite article
CN106977219B (zh) 连续纤维增强陶瓷基复合材料火焰稳定器及其制备方法与应用
Cao et al. Oxidation behavior of SiBC matrix modified C/SiC composites with different PyC interphase thicknesses
Feng et al. The ablation and mechanical behaviors of C/(SiC-ZrC) n multi-layer structure matrix composites by chemical vapor infiltration
Sayano et al. Development of a reaction-sintered silicon carbide matrix composite
CN117024164A (zh) 一种陶瓷改性碳碳复合材料鼻锥及其制备方法
Chen et al. Wet-oxygen corrosion resistance and mechanism of bi-layer Mullite/SiC coating for Cf/SiC composites
Zhang et al. Performance optimization of sol-derived C/Mullite composites by introducing a PyC-SiC double-layer interfacial coating
Luan et al. Effects of water vapor on corrosion behaviors of C/SiC in oxidizing atmosphere containing Na2SO4 vapor

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20853217

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20853217

Country of ref document: EP

Kind code of ref document: A1

122 Ep: pct application non-entry in european phase

Ref document number: 20853217

Country of ref document: EP

Kind code of ref document: A1

32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1) EPC (EPO FORM 1205A DATED 07/11/2022)

122 Ep: pct application non-entry in european phase

Ref document number: 20853217

Country of ref document: EP

Kind code of ref document: A1