EP4377278A1 - Verfahren zur herstellung eines dicken teils aus cmc-verbundstoff - Google Patents

Verfahren zur herstellung eines dicken teils aus cmc-verbundstoff

Info

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
Application number
EP22754475.6A
Other languages
English (en)
French (fr)
Inventor
Emilie Chantal Gisèle MENDEZ
Alexandre Marchais
Nicolas Eberling-Fux
Mélissa BAZERQUE
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Safran Ceramics SA
Original Assignee
Safran Ceramics SA
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 Safran Ceramics SA filed Critical Safran Ceramics SA
Publication of EP4377278A1 publication Critical patent/EP4377278A1/de
Pending legal-status Critical Current

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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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    • C04B35/515—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
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    • 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)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Composite Materials (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Ceramic Products (AREA)
EP22754475.6A 2021-07-26 2022-07-15 Verfahren zur herstellung eines dicken teils aus cmc-verbundstoff Pending EP4377278A1 (de)

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

Publications (1)

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EP4377278A1 true EP4377278A1 (de) 2024-06-05

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EP (1) EP4377278A1 (de)
CN (1) CN117836255A (de)
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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CN117836255A (zh) 2024-04-05
FR3125528A1 (fr) 2023-01-27

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