EP3478645A1 - Verfahren zur herstellung eines keramikmatrixverbundteils - Google Patents

Verfahren zur herstellung eines keramikmatrixverbundteils

Info

Publication number
EP3478645A1
EP3478645A1 EP17742814.1A EP17742814A EP3478645A1 EP 3478645 A1 EP3478645 A1 EP 3478645A1 EP 17742814 A EP17742814 A EP 17742814A EP 3478645 A1 EP3478645 A1 EP 3478645A1
Authority
EP
European Patent Office
Prior art keywords
fibrous reinforcement
porosity
ceramic matrix
ceramic
particles
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.)
Ceased
Application number
EP17742814.1A
Other languages
English (en)
French (fr)
Inventor
Aurélia CLERAMBOURG
Marie LEFEBVRE
Sébastien Denneulin
Eric Philippe
Eric Bouillon
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 EP3478645A1 publication Critical patent/EP3478645A1/de
Ceased 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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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    • D10B2101/08—Ceramic
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2505/00—Industrial
    • D10B2505/02—Reinforcing materials; Prepregs

Definitions

  • the present invention relates to the general field of manufacturing processes of ceramic matrix composite material parts.
  • CMC ceramic matrix composite material
  • Pre-preg The so-called "Pre-preg” process is also known in which pre-impregnated carbon precursor resin threads are formed into webs which are then draped to obtain a fibrous preform.
  • the fiber preform is molded, baked, and finally infiltrated by a silicon alloy in the liquid state (infiltration technique in the molten state: "MI” for "Melt-Infiltration”).
  • MI infiltration technique in the molten state
  • the parts obtained by the MI technique may have a significant residual porosity, due in particular to the inhomogeneous penetration of the molten metal into the fibrous reinforcement.
  • the mechanical properties of the parts obtained by this method can therefore be improved.
  • the main object of the present invention is therefore to overcome such drawbacks by proposing a method for manufacturing a part made of composite material comprising a fibrous reinforcement and a ceramic matrix present in the porosity of the fibrous reinforcement, the process comprising at least the following steps:
  • step b) introducing into the porosity of the fibrous reinforcement after implementation of step b) of a powder comprising ceramic particles and / or carbon particles, and
  • step d) the infiltration of the fibrous reinforcement, after implementation of step c), with a melt infiltration composition comprising at least silicon so as to form a second ceramic matrix phase in the porosity of the fibrous reinforcement and thus obtain the piece of composite material.
  • a fibrous reinforcement weave interlock weave provides better penetration of the powder particles in the porosity of the latter during step c).
  • the interlock armor defines, after step b), porosity channels adapted to a better penetration of the particles in the thickness of the reinforcement. It follows that the melt infiltration composition will also penetrate more easily into the fibrous reinforcement, during step d), by wetting the ceramic and / or carbon particles already present in the porosity of the fibrous reinforcement. .
  • the porosity in the part obtained after implementation of step d) may be less than or equal to 5%, or even less than or equal to 3%.
  • the mechanical properties of the piece of CMC material obtained are improved and the residual porosity is reduced.
  • the use of three-dimensional weaving to achieve the fiber reinforcement makes it possible to obtain pieces of complex geometry.
  • particles of SiC, Si 3 N 4 , BN, SiB 6 , B 4 C, or a mixture of such particles may be introduced during step c).
  • SiC particles may be introduced during step c).
  • a mixture of SiC particles and carbon particles is introduced in step c).
  • the average particle size introduced during step c) may be less than or equal to 5 ⁇ m or even less than or equal to 1 ⁇ m.
  • average particle size is meant the size D 50 of the particles. particles.
  • the first ceramic matrix phase may comprise silicon carbide (SiC).
  • an interphase may be formed on the ceramic son before step b).
  • the fiber reinforcement may comprise silicon carbide wires having an oxygen content of less than or equal to 1% atomic percentage.
  • the invention relates to the method described above wherein the manufactured part is a turbomachine part.
  • the part can be a part of hot part of a gas turbine of an aeronautical engine or an industrial turbine.
  • the part may constitute at least a part of a distributor, a wall of a combustion chamber, a turbine ring sector or a turbomachine blade.
  • FIG. 1 is a flowchart representing the different steps of an exemplary method according to the invention
  • FIG. 2 is a schematic view showing an example of interlock weave weave
  • FIG. 3 is a photograph showing a section of a part obtained by a method according to the invention.
  • FIG. 4 is a photograph showing a section of a piece obtained by a method outside the invention. Detailed description of the invention
  • a first step E1 of the method may consist of forming the fibrous reinforcement of the piece by three-dimensional weaving to obtain a fibrous reinforcement having an interlock weave.
  • the fiber reinforcement may be formed of ceramic son, for example silicon carbide son.
  • the fibrous reinforcement obtained during step E1 constitutes a fibrous preform of the part to be manufactured.
  • Examples of usable silicon carbide threads may be "Nicalon", “Hi-Nicalon” or “Hi-Nicalon-S” yarns marketed by the Japanese company NGS.
  • the ceramic son of the fiber reinforcement may have an oxygen content less than or equal to 1% atomic percentage.
  • "Hi-Nicalon-S" wires have such a characteristic.
  • the fibrous reinforcement has an interlock weave.
  • Armor or interlock fabric means a 3D weave armor in which each layer of warp thread C binds several layers of weft threads T with all the threads of the same warp column having the same movement in the thread plane. armor.
  • a weft layer is formed of two adjacent half-weft layers t-offset with respect to each other in the warp direction. We therefore have here 18 half-layers of weft positioned in staggered rows.
  • Each warp C binds 3 half-layers of weft t.
  • a reversal of roles between warp and weft is possible in the present text and should be considered as also covered by the claims.
  • a step E2 of surface treatment of the ceramic son, prior to the formation of an interphase, is preferably carried out in particular to eliminate the size that may be present on the fibers.
  • a defibrillation interphase can be formed by CVI on the ceramic son of the fibrous reinforcement.
  • the thickness of the interphase may for example be between 10 nm and 1000 nm, and for example between 10 nm and 100 nm.
  • the interphase can be monolayer or multilayer.
  • the interphase may comprise at least one layer of pyrolytic carbon (PyC), boron nitride (BN), silicon doped boron nitride (BN (Si), with silicon in a mass proportion of between 5% and 40%). %, the balance being boron nitride) or boron doped carbon (BC, with boron in an atomic proportion of between 5% and 20%, the balance being carbon).
  • the interphase here has a function of defragilating the composite material which favors the deflection of possible cracks reaching the interphase after having propagated in the matrix, preventing or delaying the breaking of fibers by such cracks.
  • a step E4 of forming a first ceramic matrix phase in the porosity of the fibrous reinforcement is then carried out on the interphase which may have been previously formed or directly on the fibers of the fibrous reinforcement.
  • This matrix phase can be formed by CVI.
  • the first ceramic matrix phase may for example comprise SiC.
  • the residual porosity rate of the fibrous reinforcement following this step E4 and before introduction of the powder may be greater than or equal to 30%, for example between 30% and 35%. In general, the residual porosity rate of the fibrous reinforcement after implementation of step E4 (step b)) is sufficient to allow the introduction of a powder into the porosity of the fibrous reinforcement and the formation of a second matrix phase.
  • step E5 the introduction of a powder comprising particles of ceramic material and / or carbon particles into the residual porosity of the fibrous reinforcement (step c)).
  • the fiber reinforcement can be impregnated with a composition, for example in the form of a slip, introduced into the porosity of the fibrous reinforcement by methods known per se, for example by injection.
  • Said composition may comprise the powder in suspension in a liquid medium.
  • the ceramic particles may be particles of SiC, Si 3 N 4 , BN, SiB 6 , B 4 C, or a mixture of such particles.
  • the size (D 50 ) of the particles of the powder may be less than or equal to 5 Mm, or even less than or equal to 1 Mm.
  • step E6 the fibrous reinforcement in which the powder introduced in step E5 is introduced is infiltrated with a melt infiltration composition (step d)) comprising at least silicon so as to form a second ceramic matrix phase in the porosity of the fibrous reinforcement and to finalize the densification to obtain the part.
  • a melt infiltration composition (step d)) comprising at least silicon so as to form a second ceramic matrix phase in the porosity of the fibrous reinforcement and to finalize the densification to obtain the part.
  • This infiltration step corresponds to a step of infiltration in the molten state (MI process).
  • the infiltration composition may consist of pure molten silicon or alternatively may be in the form of a molten silicon alloy and one or more other components.
  • the infiltration composition may comprise predominantly silicon mass, that is to say have a silicon mass content greater than or equal to 50%.
  • the infiltration composition may, for example, have a silicon mass content greater than or equal to 75%.
  • the constituent (s) present (s) within the silicon alloy may be selected from B, Al, Mo, Ti, and mixtures thereof.
  • the particles of the powder introduced in step E5 are particles of C, B 4 C, or a mixture of these particles, a chemical reaction may occur between the infiltration composition and the powder particles during infiltration resulting in the formation of silicon carbide.
  • step E6 the piece of material CMC is obtained.
  • a piece of CMC material may be a static or rotary turbine engine part. Examples of turbomachine parts have been mentioned above.
  • Such a piece may further be coated with an environmental / thermal barrier coating.
  • FIG. 3 shows a photograph of a sectional cut of CMC material obtained by an exemplary method according to the invention.
  • the fibrous reinforcement has an interlock weave and has been pre-densified by CVI (step E4) to obtain a first phase of SiC matrix.
  • the fibrous reinforcement had a residual porosity in volume of between 30% and 35%.
  • an SiC powder (sold by Marion Technologies under the reference SiC MT59) having an average size (D 50 ) of particles of 0.8 ⁇ m was introduced inside the porosity of the fibrous reinforcement. pre-densified.
  • the infiltration was carried out using pure silicon (marketed by HC Starck under the reference Silicium Grade AX-20).
  • the photograph of FIG. 3 shows the matrix M and the wires F in the piece of CMC material thus obtained.
  • the overall porosity measured in the room is less than 1%.
  • FIG. 4 is a photograph showing a sectional view of the CMC material part obtained in this test. Black pores are visible in the photograph of FIG. 4. An overall porosity greater than 15% has been measured in the part, and it can be seen in FIG. 4 that this porosity is also present between the F yarns. Thus, it can be seen that it is more difficult to fill the porosity in the fibrous reinforcement when the latter has a weave that is not interlocked. The mechanical properties are therefore less for this part than with that obtained in the previous test using a fibrous reinforcement with interlock weave.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Woven Fabrics (AREA)
EP17742814.1A 2016-06-29 2017-06-28 Verfahren zur herstellung eines keramikmatrixverbundteils Ceased EP3478645A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1656093A FR3053328B1 (fr) 2016-06-29 2016-06-29 Procede de fabrication d'une piece en materiau composite a matrice ceramique
PCT/FR2017/051733 WO2018002525A1 (fr) 2016-06-29 2017-06-28 Procede de fabrication d'une piece en materiau composite a matrice ceramique

Publications (1)

Publication Number Publication Date
EP3478645A1 true EP3478645A1 (de) 2019-05-08

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US (1) US20200181029A1 (de)
EP (1) EP3478645A1 (de)
CN (1) CN109415269A (de)
FR (1) FR3053328B1 (de)
WO (1) WO2018002525A1 (de)

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Publication number Priority date Publication date Assignee Title
WO2020201202A1 (fr) * 2019-04-05 2020-10-08 Safran Ceramics Procede de fabrication d'une piece en cmc
FR3101629B1 (fr) * 2019-10-07 2022-06-17 Safran Ceram Procédé de fabrication d'une pièce en CMC
FR3098514B1 (fr) * 2019-07-10 2023-10-27 Safran Ceram Structure poreuse en céramique pour pièce en matériau CMC et procédé pour l’obtenir
FR3129615A1 (fr) * 2021-11-26 2023-06-02 Safran Ceramics Noyau pour la réalisation de distributeur en Composite à Matrice Céramique

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Publication number Priority date Publication date Assignee Title
US20060163773A1 (en) * 2005-01-24 2006-07-27 General Electric Company Method for performing silicon melt infiltration of ceramic matrix composites
FR2955609B1 (fr) * 2010-01-26 2012-04-27 Snecma Aube composite a canaux internes
CN101913894A (zh) * 2010-07-08 2010-12-15 西北工业大学 一种碳化硅陶瓷基复合材料的双重自愈合改性方法
FR2983193B1 (fr) * 2011-11-30 2014-05-09 Snecma Propulsion Solide Procede de fabrication de piece en materiau cmc
US9650303B2 (en) * 2013-03-15 2017-05-16 Rolls-Royce Corporation Silicon carbide ceramic matrix composites
FR3023212B1 (fr) * 2014-07-03 2019-10-11 Safran Ceramics Procede de fabrication d'une piece revetue par un revetement de surface comportant un alliage

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WO2018002525A1 (fr) 2018-01-04
FR3053328B1 (fr) 2022-01-21
US20200181029A1 (en) 2020-06-11
FR3053328A1 (fr) 2018-01-05
CN109415269A (zh) 2019-03-01

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