EP4377278A1 - Verfahren zur herstellung eines dicken teils aus cmc-verbundstoff - Google Patents
Verfahren zur herstellung eines dicken teils aus cmc-verbundstoffInfo
- Publication number
- EP4377278A1 EP4377278A1 EP22754475.6A EP22754475A EP4377278A1 EP 4377278 A1 EP4377278 A1 EP 4377278A1 EP 22754475 A EP22754475 A EP 22754475A EP 4377278 A1 EP4377278 A1 EP 4377278A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- preform
- organic binder
- silicon
- slip
- silicon carbide
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 45
- 239000011230 binding agent Substances 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000001764 infiltration Methods 0.000 claims abstract description 15
- 230000008595 infiltration Effects 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000000835 fiber Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000000197 pyrolysis Methods 0.000 claims description 17
- 238000007596 consolidation process Methods 0.000 claims description 13
- 230000016507 interphase Effects 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000002089 carbo-reduction Methods 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000002002 slurry Substances 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 18
- 239000010410 layer Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 238000005056 compaction Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001721 transfer moulding Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000000626 liquid-phase infiltration Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000009958 sewing Methods 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
- F01D25/00—Component parts, details, or accessories, not provided for in, or of interest apart from, other groups
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- F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
- F01D5/12—Blades
- F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
- F01D5/282—Selecting composite materials, e.g. blades with reinforcing filaments
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- F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
- F01D5/284—Selection of ceramic materials
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- F01D9/00—Stators
- F01D9/02—Nozzles; Nozzle boxes; Stator blades; Guide conduits, e.g. individual nozzles
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6027—Slip casting
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
- F05D2300/00—Materials; Properties thereof
- F05D2300/20—Oxide or non-oxide ceramics
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
- F05D2300/00—Materials; Properties thereof
- F05D2300/60—Properties or characteristics given to material by treatment or manufacturing
- F05D2300/603—Composites; e.g. fibre-reinforced
Definitions
- a field of application of the invention is the production of parts intended to be exposed in service to high temperatures, in particular in the aeronautical and space fields, in particular parts of hot parts of aeronautical turbomachines, it being noted that the invention can be applied in other fields, for example the field of industrial gas turbines.
- CMC materials instead of metallic materials for parts exposed in service to high temperatures has therefore been recommended, especially since CMC materials have a significantly lower density than the metallic materials for which they replace.
- a well-known process for manufacturing parts in CMC material includes the following steps:
- the invention proposes a process for manufacturing a part made of composite material with a ceramic matrix comprising:
- a slip comprising a powder of SiC particles in the consolidated fiber preform, the silicon carbide particles comprising silicon oxide carbide and silica on their surface,
- the densification comprising the infiltration of the preform with a composition based on molten silicon so as to form a part made of composite material with a ceramic matrix
- the slip further comprises at least one organic binder and in that the method comprises, before the infiltration of the preform with a composition based on molten silicon, a step of forming an amorphous carbon residue by pyrolysis of the organic binder and a step of carboreduction of the silicon oxide carbide and of the silica present on the surface of the silicon carbide particles by the carbon residue.
- the inventors have determined after study that the appearance of porosity in the core part is linked to the inability of silicon or its alloy to wet SiC particles which are poorly deoxidized, these particles having a thin layer of silica on the surface ( Si0 2 ) or SiOC.
- the contact angle of silicon on silica is greater than 90°.
- the carbon formed by the pyrolysis of the organic binder present in the slip allows the carboreduction of the SiC particles. Indeed, the carbon present reacts preferentially with the silica or the SiOC to form carbon monoxide (CO) and SiC, which makes it possible to deoxidize the SiC powder.
- CO carbon monoxide
- SiC silicon monoxide
- the wettability of the SiC particles by the silicon is thus considerably improved, which makes it possible to avoid the appearance of core porosity. This produces thick parts with good material health.
- the use of an organic binder in the slip makes it possible to aggregate the SiC particles and to concentrate these particles in the fiber preform in a different way from that obtained with a slip without binder. Indeed, the compaction rates obtained are lower with slips using a binder. This makes it easier to evacuate the gases resulting from the deoxidation and, consequently, to prolong the deoxidation reaction (no thermodynamic equilibrium between products and reactants in this situation).
- the slip comprises between 1% and 20% by mass of organic binder.
- the organic binder is chosen from water-soluble organic binders and/or plasticizers and may for example be one of the following binders: polyvinyl alcohol (PVA), polyethylene glycol (PEG), glycerol, polymethylmethacrylate (PMMA), acrylic resin and polyvinyl butyral resin (PVB).
- PVA polyvinyl alcohol
- PEG polyethylene glycol
- PMMA polymethylmethacrylate
- PVB polyvinyl butyral resin
- the fibrous preform comprises between 0.001% and 0.25% by mass of amorphous carbon after the pyrolysis step of the organic binder.
- the pyrolysis step comprises a temperature rise at a rate of between 1° C./min and 3° C./min up to a temperature plateau of between 300° C. and 500° C., the temperature plateau being maintained over a period of between 1 h and 5 h.
- the latter further comprises, before the first densification step, the deposition on the fibers of the fiber preform of an interphase of pyrolytic carbon, boron nitride or nitride boron doped with silicon.
- the process for manufacturing a part made of SiC/SiC composite material of the invention can be applied in particular to the manufacture of a blade, a distributor, a turbine ring or a turbine combustion chamber. gas.
- Figure 1 is a flowchart indicating successive steps of an embodiment of a method according to the invention
- Figure 2 is a microscopic photograph of a thick piece of composite material obtained by implementing a process outside the invention
- Figure 3 is a microscopic photograph of a thick piece of composite material obtained by implementing an example of a process according to the invention.
- a fibrous preform comprising silicon carbide fibers is formed (step 10).
- This fibrous preform is intended to form the fibrous reinforcement of the part to be obtained.
- the fibers used can be silicon carbide (SiC) fibers supplied under the name “Nicalon”, “Hi-Nicalon” or “Hi-Nicalon-S” by the Japanese company Nippon Carbon or “Tyranno SA3” by the company UBE .
- the fibrous preform can be obtained by three-dimensional weaving between a plurality of layers of warp threads and a plurality of layers of weft threads.
- THE three-dimensional weave produced can be an "interlock" weave weave, that is to say a weave weave in which each layer of weft yarns binds several layers of warp yarns with all the yarns of the same weft column having the same movement in the plane of the armor.
- the fibrous preform can also be obtained by assembling a plurality of fibrous textures.
- the fibrous textures can be bonded together, for example by stitching or needling.
- the fibrous textures can in particular each be obtained from a layer or a stack of several layers of:
- UD unidirectional
- nD multidirectional
- a defragmenting interphase can be formed on the fibers of the preform (step 20).
- a surface treatment of the fibers prior to the formation of the interphase is preferably carried out to remove the size and a surface layer of oxide such as silica Si0 2 present on the fibers.
- the interphase can be formed by CVI.
- the interphase can be monolayer or multilayer.
- the interphase may have one or more layers of pyrolytic carbon (PyC), boron nitride (BN), or boron-doped carbon, denoted BC (the boron-doped carbon having an atomic boron content of between 5% and 20%, the remainder being carbon).
- the thickness of the interphase can be greater than or equal to 10 nm and for example be between 10 nm and 1000 nm. Of course, this does not depart from the scope of the invention when the interphase is formed on the fibers before formation of the preform.
- a consolidation phase comprising silicon carbide is then formed in the pores of the fiber preform in a manner known per se (step 30).
- the consolidation phase can be formed by chemical vapor infiltration.
- the consolidation phase may comprise only silicon carbide.
- the consolidation phase may include, in addition to silicon carbide, a self-healing material. It is possible to choose a self-healing material containing boron, for example an Si-BC ternary system or boron carbide B 4 C capable of forming, in the presence of oxygen, a glass of the borosilicate type having self-healing properties.
- the thickness of the consolidation phase deposit may be greater than or equal to 500 nm, for example between 1 ⁇ m and 30 ⁇ m.
- the outer layer of the consolidation phase (furthest from the fibers) is advantageously made of silicon carbide in order to form a reaction barrier between the underlying fibers and the molten silicon composition introduced subsequently.
- the thickness of the consolidation phase is sufficient to consolidate the fibrous preform, that is to say to bind together the fibers of the preform sufficiently so that the preform can be manipulated while retaining its shape without the assistance of holding tool.
- the preform remains porous, the initial porosity being for example filled only for a minority part by the interphase and the consolidation phase.
- the next step consists of injecting a slurry comprising a powder of silicon carbide particles into the fiber preform (“Slurry Cast” or “Slurry Transfer Molding”) (step 40).
- the slip also comprises at least one organic binder.
- the organic binder used here is capable of producing carbonaceous residues by pyrolysis.
- the main function of the organic binder is not to form a coating of carbon on the surface of the SiC particles but to allow the carboreduction of the SiC particles and, consequently, the deoxidation of these particles as explained below.
- the organic binder is a binder having a carbonization rate of less than 5%.
- the organic binder is thus capable of forming between 1% and 5% by mass of amorphous carbon (coke content) after pyrolysis.
- the organic binder can be chosen from water-soluble organic binders and/or plasticizers and can be, for example, one of the following binders: polyvinyl alcohol (PVA), polyethylene glycol (PEG), glycerol, polymethylmethacrylate (PMMA), acrylic resin and polyvinyl butyral resin ( PVB).
- PVA polyvinyl alcohol
- PEG polyethylene glycol
- PMMA polymethylmethacrylate
- acrylic resin polyvinyl butyral resin
- PVB polyvinyl butyral resin
- the slip comprises between 1% and 20% by mass of organic binder relative to the mass of SiC present in the slip and more preferably between 1% and 10% by mass.
- the slip comprises a SiC powder filler content of between 30% and 50% by volume and more preferably a content of 45% by volume.
- the viscosity of the slip is less than 500 mPa.s (cPs) and is therefore very fluid and easy to inject.
- an organic binder in the slip already provides a first effect before heat treatment. Indeed, the binder makes it possible to maintain a state of flocculation of the SiC particles and will play the role of steric hindrance, which will concentrate (stack) the particles in the fibrous preform in a different way from that obtained with a slip. without binder. The compaction rates obtained are then lower with a filled slip using a binder. This makes it possible to have larger porosity channels and to more easily evacuate the gases resulting from the deoxidation and, consequently, to prolong the deoxidation reaction (no thermodynamic equilibrium between products and reactants in this situation).
- the rate of compaction of a fibrous preform impregnated with a slip filled with SiC particles and without organic binder is between 55% and 65%, whereas the degree of compaction of a fibrous preform impregnated with a slip filled with SiC particles and comprising an organic binder is between 45% and 50%.
- the average size of the porosity channels present in the fiber preform after injection/filtration of a slip of SiC particles and without organic binder is less than 100 nm while the average size of the porosity channels present in the fiber preform after injection/filtration of a slip of SiC particles and comprising an organic binder is between 100 nm and 300 nm.
- a pyrolysis heat treatment of the organic binder is carried out in order to form a carbon residue in the preform (step 50).
- the pyrolysis step is carried out at a temperature between 300°C and 500°C. More specifically, depending on the quantity of organic binder present in the slurry, the pyrolysis step includes a temperature rise at a rate of between 1°C/min and 3°C/min up to a temperature plateau of between between 300° C. and 500° C., the staggered temperature plateau maintained over a period of between 1 h and 5 h.
- This pyrolysis step (rise in temperature and plateau) can be carried out before the final densification step by infiltration of the preform with a composition based on molten silicon, that is to say during a separate heat treatment, or during the temperature rise ramp preparatory to the infiltration of the preform with a composition based on molten silicon whose melting temperature is much higher than that of the pyrolysis of the organic binder.
- the pyrolysis step is carried out before the infiltration of the preform with a composition based on molten silicon.
- a preform which comprises between 0.001% and 0.25% by mass of amorphous carbon.
- This carbonaceous residue promotes the carboreduction of the SiC particles.
- the carbon present reacts preferentially with silica or silicon oxide carbide (SiOC) present on the surface of the SiC particles to form carbon monoxide (CO) and SiC, which makes it possible to deoxidize the powder. of SiC.
- SiOC silicon oxide carbide
- the fibrous preform is then infiltrated with the molten composition comprising mainly molten silicon by mass (step 60).
- This composition can correspond to molten silicon alone or to a silicon alloy with the molten state which also contains one or more other elements such as titanium, molybdenum, boron, iron or niobium.
- the mass content of silicon in the molten composition may be greater than or equal to 90%.
- the molten silicon or its alloy easily wets the silicon carbide present in the preform, which greatly facilitates its penetration into the pores of the preform by capillarity.
- a part made of composite material with a ceramic matrix is thus obtained which has a very low level of porosity even in the case of thick parts typically greater than 5 mm.
- Figures 2 and 3 are microscopic photographs showing the morphology of a thick zone of CMC composite material parts obtained by implementing the following steps:
- the slip does not contain any organic binder
- the slip used to manufacture the part in FIG. 3 contains an organic binder in accordance with the invention as described above. It can be seen that the part in figure 2 has a significant residual porosity whereas the part in figure 3 is perfectly densified, the space present between the fibers being entirely filled by the matrix.
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
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Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR2108108A FR3125528A1 (fr) | 2021-07-26 | 2021-07-26 | Procédé de fabrication d’une pièce épaisse en matériau composite CMC |
PCT/FR2022/051418 WO2023007073A1 (fr) | 2021-07-26 | 2022-07-15 | Procede de fabrication d'une piece epaisse en materiau composite cmc |
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EP4377278A1 true EP4377278A1 (de) | 2024-06-05 |
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EP22754475.6A Pending EP4377278A1 (de) | 2021-07-26 | 2022-07-15 | Verfahren zur herstellung eines dicken teils aus cmc-verbundstoff |
Country Status (4)
Country | Link |
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EP (1) | EP4377278A1 (de) |
CN (1) | CN117836255A (de) |
FR (1) | FR3125528A1 (de) |
WO (1) | WO2023007073A1 (de) |
Family Cites Families (7)
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US6503572B1 (en) * | 1999-07-23 | 2003-01-07 | M Cubed Technologies, Inc. | Silicon carbide composites and methods for making same |
US20040191411A1 (en) * | 2003-03-31 | 2004-09-30 | Hornor John A. | Method for making silicon carbide composites by melt infiltration |
FR2887601B1 (fr) | 2005-06-24 | 2007-10-05 | Snecma Moteurs Sa | Piece mecanique et procede de fabrication d'une telle piece |
US20130287941A1 (en) * | 2012-04-27 | 2013-10-31 | General Electric Company | Method of producing a melt-infiltrated ceramic matrix composite article |
US10017424B2 (en) * | 2014-12-04 | 2018-07-10 | Rolls-Royce Corporation | Ceramic matrix composites and methods of making the same |
FR3047988B1 (fr) | 2016-02-18 | 2018-03-16 | Centre National De La Recherche Scientifique | Procede de fabrication d'une piece en materiau composite a matrice ceramique |
FR3071247B1 (fr) * | 2017-09-21 | 2019-09-20 | Safran Ceramics | Procede de fabrication d'une piece en cmc |
-
2021
- 2021-07-26 FR FR2108108A patent/FR3125528A1/fr active Pending
-
2022
- 2022-07-15 WO PCT/FR2022/051418 patent/WO2023007073A1/fr active Application Filing
- 2022-07-15 CN CN202280051965.6A patent/CN117836255A/zh active Pending
- 2022-07-15 EP EP22754475.6A patent/EP4377278A1/de active Pending
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Publication number | Publication date |
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WO2023007073A1 (fr) | 2023-02-02 |
CN117836255A (zh) | 2024-04-05 |
FR3125528A1 (fr) | 2023-01-27 |
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