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  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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  • C04B35/628—Coating the powders or the macroscopic reinforcing agents
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  • C04B35/71—Ceramic products containing macroscopic reinforcing agents
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  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical 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
  • C23C16/26—Deposition of carbon only
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  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical 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
  • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
  • C23C16/34—Nitrides
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  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical 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 method of coating
  • C23C16/54—Apparatus specially adapted for continuous coating
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  • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
  • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
  • C04B2111/00982—Uses not provided for elsewhere in C04B2111/00 as construction elements for space vehicles or aeroplanes
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  • C04B2235/52—Constituents or additives characterised by their shapes
  • C04B2235/5208—Fibers
  • C04B2235/5216—Inorganic
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• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
  • D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
  • D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
  • D06B5/00—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating
  • D06B5/02—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating through moving materials of indefinite length
  • D06B5/06—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating through moving materials of indefinite length through yarns, threads or filaments

Definitions

• the present invention relates to ceramic matrix composite (CMC) parts and methods for making such parts.
• CMC ceramic matrix composite
• One field of application of the invention lies in the production of parts which are intended to be exposed to high operating temperatures, specifically in the fields of aviation and space, and in particular parts for the parts.
• hot air turbine engines it being understood that the invention can be applied to other fields, for example to the field of industrial gas turbines.
• CMC materials exhibit good thermostructural properties, that is, good mechanical properties which make them suitable for the constitution of structural parts, together with the ability to retain these properties at elevated temperatures.
• CMC materials include a fibrous reinforcement made of cables of ceramic or carbonaceous materials present in a ceramic matrix.
• the use of CMC materials instead of metallic materials for parts that are exposed to high service temperatures is desirable, especially since these materials exhibit a density that is considerably less than the density of the metallic materials they replace. .
• a CMC part by means of a technique in which plies of fibers coated with an interphase are impregnated with a resin mixture and then superimposed in the desired orientation so that a preform of the part to be obtained is obtained. get.
• the resin is pyrolyzed and then densification of the preform is performed by infiltration with molten silicon or a molten silicon alloy to form a ceramic matrix.
• the inventors have observed that the product thus obtained may not be entirely satisfactory because matrix layers between each ply can lead to a weakness in temperature creep, due to the presence of free silicon.
• the incorporated matrix phases characterized by low creep resistance, in the form of free silicon in the matrix obtained by melt infiltration, can lead to overloading of the fibers exceeding their creep resistance. and therefore to a reduction in the breaking time.
• the present invention provides a method of manufacturing a part in CMC, the method comprising at least:
• a consolidated fiber preform by treatment of the fiber preform by chemical vapor infiltration to form a consolidation phase on the interphase, the consolidation phase comprising silicon carbide and having a Young's modulus greater than or equal at 350 GPa.
• the Young's modulus of the consolidation phase is measured at 20 ° C.
• the interphase formed offers in particular a better transfer of charge from fiber to fiber and also avoids the risk of a vitreous bond (“glass linkage”) and of a rupture of bundles of adjacent fibers during an oxidative exposure. .
• the solution proposed by the present invention therefore provides a part made of CMC having better mechanical properties at high temperatures.
• the consolidation phase has a Young's modulus greater than or equal to 375 GPa, for example greater than or equal to 400 GPa.
• This feature further improves the creep resistance of the CMC part.
• the residual volume porosity of the consolidated fiber preform is in the range of 25% to 45%, for example in the range of 30% to 35%.
• the method further comprises densifying the consolidated fiber preform by forming a silicon carbide matrix phase over the consolidation phase by infiltration with a molten composition comprising silicon, carbon particles and / or ceramic being present in the porosity of the consolidated preform before infiltration.
• This characteristic advantageously results in a ceramic matrix having a low porosity, which thus reduces the stress concentrations under mechanical load and improves the resistance of the matrix to cracking.
• the interphase is formed from at least one layer of the following materials: boron nitride, silicon doped boron nitride, pyrolytic carbon or boron doped carbon.
• the interphase may be covered with a protective layer of at least one of the following materials: silicon nitride or silicon carbide.
• the cables comprise silicon carbide fibers having an oxygen content which is less than or equal to 1% atomic percentage.
• the present invention also provides a part in CMC comprising at least:
• a 3D woven fiber reinforcement comprising a plurality of cables, the cables having a plurality of fibers which are individually coated with an interphase;
• This part in CMC can be obtained by implementing the method described above.
• the consolidation phase has a Young's modulus greater than or equal to 375 GPa, for example greater than or equal to 400 GPa.
• this feature further improves the creep resistance of the CMC part.
• the volume fraction of the consolidation phase is in the range from 5% to 30%, for example in the range from 10% to 30%.
• This characteristic advantageously optimizes the resistance to creep at high temperatures.
• the part further comprises a silicon carbide matrix phase located on the consolidation phase, said silicon carbide matrix phase having a residual volume porosity less than or equal to 8
• this characteristic advantageously reduces stress concentrations under mechanical load and improves the resistance of the die to cracking.
• the interphase is formed from at least one layer of the following materials: boron nitride, silicon doped boron nitride, pyrolytic carbon, and boron doped carbon.
• the cables comprise silicon carbide fibers having an oxygen content which is less than or equal to 1% atomic percentage.
• the part can be a turbine engine part.
• the part can be a turbine ring or a turbine ring sector, a movable blade, a fixed blade, a combustion chamber wall, or a distributor.
• FIG. 1 is a flowchart of an example of a method according to the invention.
• FIG. 2 generally illustrates a device for forming
• the process begins by coating the cables with interphase by means of the implementation of vapor deposition (step S10 in Fig. 1).
• the cables can comprise ceramic fibers, for example nitride or carbide fibers, for example silicon carbide fibers.
• the cables can comprise carbon fibers.
• the cables comprise silicon carbide fibers having an oxygen content which is less than or equal to 1% atomic percentage. Examples of such cables are marketed under the name “Hi-Nicalon-S” by the company NGS, under the name “Tyranno SA3” by the supplier UBE, or under the name “Sylramic i-BN” by the supplier COI Ceramics.
• a cable comprises a plurality of fibers, for example at least one hundred fibers, typically 500 fibers.
• the interphase is used to slow down the breaking of cable fibers by cracks that initially start in the matrix.
• the defragilization interphase may comprise a material of lamellar structure which, for a crack reaching the interphase, is capable of dissipating the cracking energy by localized uncoupling at the atomic scale so that the crack be deviated in the interphase.
• Interphase is a coating that can consist of a single layer or multiple layers.
• the interphase may contain one or more layers of: boron nitride BN, boron nitride doped with silicon BN (Si) (having a mass content of silicon in the range of 5% to 40%, the remainder being nitride boron), PyC pyrolytic carbon or boron doped carbon (having an atomic boron content in the range of 5% to 20%, the remainder being carbon) or boron carbide.
• the thickness of the interphase may be greater than or equal to 10 nanometers (nm), and for example may be in the range from 10 nm to 1000 nm.
• it may be preferable to carry out a surface treatment on the fibers of the cables before the formation of the interphase in order to remove the size and a surface layer of oxide such as silica S1O2 present. on the fibers.
• the device 1 comprises a treatment chamber 4 in which a plurality of cables 2 intended to be coated are transported by being driven by a conveying system 6, comprising here first 6a and second 6b sets of pulleys. Each set 6a or 6b comprises one or more pulleys.
• the conveying system 6 is configured to transport the cables 2 through the processing chamber 4 along a Y conveying axis. In the example shown, the Y conveying axis is parallel to the longitudinal axis X of the device 1.
• the cables 2 are put under tension between the pulleys 6a and 6b and are put under tension between the input and output ends 5a and 5b.
• the fibers of the cables 2 move apart, which leads to a more homogeneous filling of the cables 2 and to an individual coating of the fibers.
• the cables 2 can be transported continuously through the processing chamber 4 during coating with the interphase. In this case, the cables 2 do not stop as they are transported through processing chamber 4.
• the cables 2 which are to be coated with the interphase may not be linked together (in particular the cables 2 are not woven, knitted, or braided together).
• the cables 2 may not have been subjected to a textile operation and may not form a fibrous structure during coating with the interphase.
• the interphase is obtained by injecting a gas phase 10 into the processing chamber through an inlet port 7 to form the interphase on the cables 2.
• the interphase can be formed by chemical vapor deposition (CVD ).
• the interphase can be formed in contact with the fibers of the cables.
• the unreacted gas phase, together with reaction by-products, are pumped out through an outlet 8 (arrow 11).
• the device 1 also comprises a heating system configured to heat the treatment chamber 4 in order to carry out vapor deposition.
• the heating system can heat the treatment chamber 4 by inductive or radiant heating.
• the gas phase 10 can comprise one or more gaseous hydrocarbons, for example selected from methane, ethane, propane and butane.
• the gas phase 10 can contain a gaseous precursor of a ceramic material, such as a combination of boron trichloride BCI 3 and ammonia NH 3 .
• a multilayer interphase can be achieved by placing a plurality of such units in series, each comprising a device for injecting a gas phase and a device for removing the residual gas phase.
• the process continues by performing a three-dimensional weaving of the coated cables to form a fiber preform of the part to be obtained (step S20 in Fig. 1).
• the fiber preform serves to form the fiber reinforcement of the part to be obtained.
• the fiber preform is obtained by three-dimensional weaving between a plurality of layers of warp cables and a plurality of layers of warp cables. frame.
• the fiber preform can be made in one piece by three-dimensional weaving. Three-dimensional weaving can be achieved with weaving
• interlock that is to say a weaving in which each layer of weft cables binds a plurality of layers of warp cables, with all the cables of a same weft column having the same movement in the plane of armor.
• the roles of the warps and wefts can be reversed, and this reversal is to be considered also to be covered by the claims.
• the use of other types of 3D weaving are of course not within the scope of the invention.
• Various suitable weaving techniques are described in WO 2006/136755.
• a sizing composition comprising a linear polysiloxane
• An example of such a sizing composition is disclosed in document US 2017/073854.
• Another solution to avoid any risk of damage to the interphase is to form the preform using a loom having elements which come into contact with the cables which are made of molybdenum. This type of loom is disclosed in document FR 3045679.
• a consolidation phase comprising silicon carbide is formed by CVI in the pores of the fiber preform and on the interphase (step S30 in Fig. 1).
• the consolidation phase can be formed in contact with the interphase.
• the consolidation phase obtained by CVI does not contain free silicon and has a high Young's modulus, greater than or equal to 350 GPa.
• the Young's modulus of the consolidation phase can for example be located in the range going from 350 GPa to 450 GPa, for example in the range going from 350 GPa to 420 GPa.
• this consolidation phase gives the part the desired creep resistance at high temperatures.
• the consolidation phase comprises silicon carbide, optionally doped with a self-healing material such as boron B or boron carbide B 4 C.
• the thickness of the consolidation phase may be greater than or equal to 500 nm, for example lying in the range going from 1 micrometer (pm) to 30 pm.
• the thickness of the consolidation phase is sufficient to consolidate the fiber preform, that is to say to bind together the cables of the blank enough to allow the preform to be handled while retaining its shape without the assistance of a holding tool.
• the residual volume porosity of the consolidated fiber preform may be less than or equal to 45%, for example may be located in the range from 30% to 35%.
• the volume fraction of the consolidation phase in the consolidated fiber preform (or in the CMC part) can be greater than or equal to 5%. In one example, this volume fraction of the consolidation phase is in the range from 10% to 30%.
• an additional densification step can be performed to complete the densification of the preform (step S40).
• the ceramic matrix phase formed during the additional densification step S40 is formed on the consolidation phase and may be in contact with the consolidation phase.
• this additional densification step is performed
• the consolidated prefome can be impregnated with a slip containing the powder suspended in a liquid medium, for example water.
• the powder can be retained in the preform by filtration, optionally with the assistance of suction or pressure. It is preferable to use a powder consisting of particles having an average size (D50) of 5 ⁇ m or less, or even 2 ⁇ m or less.
• D50 average size
• the powder is present in the pores of the consolidated fiber preform.
• the powder can include particles of silicon carbide.
• particles of another material for example such as carbon, boron carbide, silicon boride, silicon nitride, may be present in the pores of the fiber preform.
• the consolidated fiber preform comprising the particles is infiltrated with a molten composition comprising silicon.
• This composition can correspond to molten silicon alone or to a silicon alloy in the molten state which also contains one or more other elements such as titanium, molybdenum, boron, iron or niobium.
• the proportion by weight of silicon in the molten composition may be greater than or equal to 50%, for example greater than or equal to 75%, for example greater than or equal to 90%.
• the additional densification step can be carried out in a known manner by CVI or by a technique of polymer infiltration and pyrolysis (“Polymer Infiltration and Pyrolysis”; “PIP”).
• the CVI technique used to form the consolidation phase can be continued so as to completely densify the fiber preform.
• the entire ceramic matrix of the CMC part can be obtained by CVI.
• the expression "within the range from ... to " should be understood as including the limits.

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• 2020
  • 2020-03-30 EP EP20713333.1A patent/EP3947319A1/de active Pending
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