FR3141167A1 - Process for manufacturing a part made of ceramic matrix composite material - Google Patents
Process for manufacturing a part made of ceramic matrix composite material Download PDFInfo
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- FR3141167A1 FR3141167A1 FR2210906A FR2210906A FR3141167A1 FR 3141167 A1 FR3141167 A1 FR 3141167A1 FR 2210906 A FR2210906 A FR 2210906A FR 2210906 A FR2210906 A FR 2210906A FR 3141167 A1 FR3141167 A1 FR 3141167A1
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- Prior art keywords
- layer
- protective layer
- fibrous structure
- silicon
- boron
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- 239000000463 material Substances 0.000 title claims abstract description 20
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims description 20
- 239000010410 layer Substances 0.000 claims abstract description 74
- 239000011159 matrix material Substances 0.000 claims abstract description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000280 densification Methods 0.000 claims abstract description 33
- 239000011241 protective layer Substances 0.000 claims abstract description 29
- 238000001764 infiltration Methods 0.000 claims abstract description 28
- 230000008595 infiltration Effects 0.000 claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- 238000000626 liquid-phase infiltration Methods 0.000 claims abstract description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 230000016507 interphase Effects 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052796 boron Inorganic materials 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 14
- 230000002787 reinforcement Effects 0.000 claims description 14
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 8
- 239000011229 interlayer Substances 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 7
- 238000009941 weaving Methods 0.000 claims description 6
- 229910052580 B4C Inorganic materials 0.000 claims description 5
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910002056 binary alloy Inorganic materials 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000002131 composite material Substances 0.000 description 9
- 238000000151 deposition Methods 0.000 description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 8
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 8
- 229920006184 cellulose methylcellulose Polymers 0.000 description 8
- 238000012710 chemistry, manufacturing and control Methods 0.000 description 8
- 238000007596 consolidation process Methods 0.000 description 8
- 230000008021 deposition Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 3
- 239000005055 methyl trichlorosilane Substances 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002296 pyrolytic carbon Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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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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- C04B35/00—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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- C04B35/565—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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- C04B35/626—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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
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Abstract
Procédé de fabrication d’une pièce en matériau composite à matrice céramique La présente invention concerne un procédé de fabrication d’une pièce en matériau composite à matrice céramique, comprenant : - l’infiltration (S60) d’une structure fibreuse pré-densifiée par une composition d’infiltration à l’état fondu comprenant du silicium afin de former une matrice céramique dans une porosité résiduelle de ladite structure fibreuse pré-densifiée, ladite structure fibreuse pré-densifiée comprenant une matrice de pré-densification comprenant une première couche de carbure de silicium et une deuxième couche protectrice recouvrant la première couche et apte à protéger celle-ci d’une attaque par le silicium de la composition d’infiltration, la deuxième couche protectrice étant formée par un système binaire B-C ou par un système ternaire Si-B-C, une poudre de carbure de silicium étant intercalée entre la première et la deuxième couches. Figure pour l’abrégé : Fig. 1.Method of manufacturing a part made of ceramic matrix composite material The present invention relates to a method of manufacturing a part of ceramic matrix composite material, comprising: - the infiltration (S60) of a pre-densified fibrous structure by a melt infiltration composition comprising silicon to form a ceramic matrix in a residual porosity of said pre-densified fibrous structure, said pre-densified fibrous structure comprising a pre-densification matrix comprising a first carbide layer of silicon and a second protective layer covering the first layer and capable of protecting the latter from attack by the silicon of the infiltration composition, the second protective layer being formed by a binary system B-C or by a ternary system Si- B-C, a silicon carbide powder being interposed between the first and second layers. Figure for abstract: Fig. 1.
Description
L’invention concerne la fabrication d’une pièce en matériau composite à matrice en céramique (« Ceramic Matrix Composite » ; « CMC ») durant laquelle la matrice céramique est formée par infiltration d’une composition à base de silicium fondu (« Melt-Infiltration » ; « MI »). L’invention propose la présence d’une couche protectrice permettant de protéger le carbure de silicium de pré-densification sous-jacent de l’attaque par le silicium fondu. La pièce en matériau composite ainsi obtenue peut trouver une application en tant que pièce de partie chaude de turbomachine, notamment de turbomachine aéronautique, telle qu’une pièce de turbine.The invention relates to the manufacture of a part made of ceramic matrix composite material (“Ceramic Matrix Composite”; “CMC”) during which the ceramic matrix is formed by infiltration of a composition based on molten silicon (“Melt- Infiltration”; “MI”). The invention proposes the presence of a protective layer making it possible to protect the underlying pre-densification silicon carbide from attack by molten silicon. The composite material part thus obtained can find application as a hot part of a turbomachine, in particular an aeronautical turbomachine, such as a turbine part.
Les matériaux composites à matrice céramique supportent des températures allant de 600°C à 1400°C. De par leur meilleure résistance aux hautes températures, les CMC nécessitent moins de refroidissement. Ce refroidissement étant traditionnellement issu d’un prélèvement dans le compresseur qui impacte le rendement de la turbomachine, les matériaux CMC permettent donc d’améliorer le rendement moteur ce qui réduit la consommation de carburant. Par ailleurs, leur utilisation contribue à optimiser les performances des turbomachines notamment par la baisse de la masse globale de la turbomachine qui contribue encore à une diminution de la consommation de carburant et donc à la réduction significative des émissions polluantes.Ceramic matrix composite materials withstand temperatures ranging from 600°C to 1400°C. Due to their better resistance to high temperatures, CMCs require less cooling. This cooling traditionally comes from a sample in the compressor which impacts the efficiency of the turbomachine, CMC materials therefore make it possible to improve engine efficiency which reduces fuel consumption. Furthermore, their use contributes to optimizing the performance of turbomachines, in particular by reducing the overall mass of the turbomachine, which further contributes to a reduction in fuel consumption and therefore to a significant reduction in polluting emissions.
Les pièces en CMC peuvent être densifiées par infiltration à l’état fondu. Dans cette technique, une composition de silicium fondu peut être introduite dans la porosité d’une structure fibreuse pré-densifiée par un dépôt de carbure de silicium et chargée par des particules de carbure de silicium. Cette méthode permet d’obtenir une matrice Si-SiC totalement dense de haut module et un composite à haute limite de linéarité. Les composites obtenus présentent de bonnes propriétés mécaniques mais les inventeurs ont observé une certaine variabilité dans l’allongement à rupture qui diminue la tolérance aux dommages du matériau. Il est souhaitable de proposer une solution pour répondre à cet inconvénient.CMC parts can be densified by melt infiltration. In this technique, a molten silicon composition can be introduced into the porosity of a fibrous structure pre-densified by a silicon carbide deposit and loaded with silicon carbide particles. This method makes it possible to obtain a completely dense high modulus Si-SiC matrix and a composite with a high linearity limit. The composites obtained have good mechanical properties but the inventors observed a certain variability in the elongation at break which reduces the damage tolerance of the material. It is desirable to propose a solution to address this drawback.
L’invention concerne un procédé de fabrication d’une pièce en matériau composite à matrice céramique, comprenant :
- l’infiltration d’une structure fibreuse pré-densifiée par une composition d’infiltration à l’état fondu comprenant du silicium afin de former une matrice céramique dans une porosité résiduelle de ladite structure fibreuse pré-densifiée, ladite structure fibreuse pré-densifiée comprenant une matrice de pré-densification comprenant une première couche de carbure de silicium et une deuxième couche protectrice recouvrant la première couche et apte à protéger celle-ci d’une attaque par le silicium de la composition d’infiltration, la deuxième couche protectrice étant formée par un système binaire B-C ou par un système ternaire Si-B-C, une poudre de carbure de silicium étant intercalée entre la première et la deuxième couches.The invention relates to a method of manufacturing a part made of ceramic matrix composite material, comprising:
- the infiltration of a pre-densified fibrous structure with a melt infiltration composition comprising silicon in order to form a ceramic matrix in a residual porosity of said pre-densified fibrous structure, said pre-densified fibrous structure comprising a pre-densification matrix comprising a first layer of silicon carbide and a second protective layer covering the first layer and capable of protecting the latter from attack by the silicon of the infiltration composition, the second protective layer being formed by a binary BC system or by a ternary Si-BC system, a silicon carbide powder being interposed between the first and second layers.
Les inventeurs ont constaté que la variabilité du comportement à rupture était liée à une attaque non maîtrisée du carbure de silicium de la matrice de pré-densification par le silicium fondu dans la solution de l’art antérieur. Ce phénomène peut aller jusqu’à la dégradation du renfort fibreux et de l’interphase résultant en une diminution du caractère structural du composite. L’invention propose une fonctionnalisation de la matrice de pré-densification de sorte à y intégrer une couche protectrice telle que décrite plus haut qui permet de réduire l’attaque du carbure de silicium de la matrice de pré-densification. La couche protectrice, faisant partie intégrante de la matrice de pré-densification, est répartie de manière homogène dans la structure fibreuse pré-densifiée pour apporter une protection dans tout son volume et tout au long de l’infiltration. On obtient ainsi des matériaux composites avec un comportement à rupture bien plus performant. En outre, le dépôt de la deuxième couche protectrice après introduction de la poudre classiquement utilisée dans les techniques d’infiltration à l’état fondu permet d’avoir une protection efficace même pour une faible épaisseur du fait d’une augmentation de la surface spécifique liée à l’introduction préalable de la poudre. La deuxième couche a un comportement sacrificiel de sorte à protéger le carbure de silicium sous-jacent. Par ailleurs, les conditions imposées lors de la formation de la couche protectrice peuvent permettre de s’affranchir d’une étape subséquente de désoxydation de la poudre ou a minima de la simplifier grandement (réduction du temps et/ou de la température imposée) laquelle permet d’améliorer la mouillabilité par le silicium fondu.The inventors noted that the variability of the fracture behavior was linked to an uncontrolled attack on the silicon carbide of the pre-densification matrix by the molten silicon in the solution of the prior art. This phenomenon can go as far as the degradation of the fibrous reinforcement and the interphase resulting in a reduction in the structural character of the composite. The invention proposes a functionalization of the pre-densification matrix so as to integrate a protective layer as described above which makes it possible to reduce the attack of the silicon carbide of the pre-densification matrix. The protective layer, forming an integral part of the pre-densification matrix, is distributed homogeneously in the pre-densified fibrous structure to provide protection throughout its volume and throughout infiltration. We thus obtain composite materials with much more efficient breaking behavior. In addition, the deposition of the second protective layer after introduction of the powder conventionally used in melt infiltration techniques makes it possible to have effective protection even for a small thickness due to an increase in the specific surface area. linked to the prior introduction of the powder. The second layer has sacrificial behavior so as to protect the underlying silicon carbide. Furthermore, the conditions imposed during the formation of the protective layer can make it possible to dispense with a subsequent step of deoxidation of the powder or at least to greatly simplify it (reduction of the time and/or the temperature imposed) which makes it possible to improve wettability by molten silicon.
Dans un exemple de réalisation, la matrice de pré-densification comprend en outre une couche protectrice additionnelle de pyrocarbone recouvrant la deuxième couche.In an exemplary embodiment, the pre-densification matrix further comprises an additional protective layer of pyrocarbon covering the second layer.
Une telle caractéristique permet avantageusement de fournir une source de carbone supplémentaire permettant de réduire davantage encore le risque d’une attaque du carbure de silicium de la matrice de pré-densification.Such a characteristic advantageously makes it possible to provide an additional source of carbon making it possible to further reduce the risk of attack on the silicon carbide of the pre-densification matrix.
Dans un exemple de réalisation, la composition d’infiltration comprend du bore.In an exemplary embodiment, the infiltration composition comprises boron.
Une telle caractéristique permet avantageusement de protéger davantage encore le carbure de silicium sous-jacent.Such a characteristic advantageously makes it possible to further protect the underlying silicon carbide.
Dans un exemple de réalisation, la deuxième couche protectrice est en carbure de bore, avec éventuellement présence de carbone libre en excès, ou en carbone dopé au bore avec du bore en une proportion atomique comprise entre 5% et 20%.In an exemplary embodiment, the second protective layer is made of boron carbide, possibly with the presence of excess free carbon, or of carbon doped with boron with boron in an atomic proportion of between 5% and 20%.
Une telle couche protectrice présente l’avantage d’être relativement simple à former.Such a protective layer has the advantage of being relatively simple to form.
En variante, la deuxième couche protectrice est formée par un système ternaire Si-B-C ayant, en pourcentage atomique, une teneur en bore comprise entre 56% et 79%, une teneur en carbone comprise entre 17% et 39% et une teneur en silicium comprise entre 3% et 6%.Alternatively, the second protective layer is formed by a ternary Si-B-C system having, in atomic percentage, a boron content of between 56% and 79%, a carbon content of between 17% and 39% and a silicon content between 3% and 6%.
L’emploi d’un système ternaire Si-B-C est avantageux dans la mesure où il ne nécessite pas d’ajouter un précurseur carboné, rendant le système de traitement des effluents d’un four SiC-CVI compatible de la formation de ce système.The use of a ternary Si-B-C system is advantageous in that it does not require adding a carbon precursor, making the effluent treatment system from a SiC-CVI furnace compatible with the formation of this system.
Dans un exemple de réalisation, la structure fibreuse pré-densifiée comprend un renfort fibreux partiellement densifié par la matrice de pré-densification, et la deuxième couche protectrice, ou l’éventuelle couche protectrice additionnelle, forme la couche de la matrice de pré-densification la plus éloignée du renfort fibreux.In an exemplary embodiment, the pre-densified fibrous structure comprises a fibrous reinforcement partially densified by the pre-densification matrix, and the second protective layer, or the possible additional protective layer, forms the layer of the pre-densification matrix furthest from the fibrous reinforcement.
Dans un exemple de réalisation, une épaisseur de la deuxième couche est comprise entre 0,1 µm et 4 µm. Cette épaisseur est de préférence comprise entre 0,1 µm et 2 µm.In an exemplary embodiment, a thickness of the second layer is between 0.1 µm and 4 µm. This thickness is preferably between 0.1 µm and 2 µm.
Une telle caractéristique permet d’obtenir un bon compromis entre une protection efficace du carbure de silicium de pré-densification durant l’infiltration, sans pénaliser le temps de fabrication de la pièce par maîtrise de l’épaisseur de la couche protectrice.Such a characteristic makes it possible to obtain a good compromise between effective protection of the pre-densification silicon carbide during infiltration, without penalizing the manufacturing time of the part by controlling the thickness of the protective layer.
Dans un exemple de réalisation, la matrice de pré-densification comprend en outre un dépôt intercalaire situé entre la poudre de carbure de silicium et la deuxième couche protectrice, ledit dépôt intercalaire comprenant du carbure de silicium et/ou un matériau déviateur de fissures.In an exemplary embodiment, the pre-densification matrix further comprises an interlayer deposit located between the silicon carbide powder and the second protective layer, said interlayer deposit comprising silicon carbide and/or a crack deflecting material.
Une telle caractéristique participe à améliorer davantage encore la protection conférée.Such a characteristic helps to further improve the protection provided.
En particulier, le dépôt intercalaire peut comprendre une alternance de couches de carbure de silicium et de couches du matériau déviateur de fissures.In particular, the interlayer deposit may comprise alternating layers of silicon carbide and layers of crack deflecting material.
Une telle caractéristique permet d’améliorer davantage encore les performances à rupture du CMC. D’une manière générale, le fait d’introduire les leviers mécaniques (types déviateurs) après l’introduction de la poudre SiC, permet de tirer profit d’une surface spécifique plus importante et ainsi disposer d’une surface de déviateurs maximisée.Such a characteristic makes it possible to further improve the breaking performance of the CMC. Generally speaking, introducing mechanical levers (deviator types) after the introduction of the SiC powder allows you to take advantage of a larger specific surface area and thus have a maximized deviator surface area.
Dans un exemple de réalisation, la structure fibreuse pré-densifiée comprend en outre une interphase de nitrure de bore entre un renfort fibreux et la matrice de pré-densification.In an exemplary embodiment, the pre-densified fibrous structure further comprises a boron nitride interphase between a fibrous reinforcement and the pre-densification matrix.
La présence d’une interphase de nitrure de bore permet avantageusement de dévier les fissures qui peuvent apparaître dans la matrice de la pièce composite en fonctionnement de sorte à préserver le renfort fibreux, et d’apporter une résistance à l’oxydation.The presence of a boron nitride interphase advantageously makes it possible to deflect cracks which may appear in the matrix of the composite part in operation so as to preserve the fibrous reinforcement, and to provide resistance to oxidation.
Dans un exemple de réalisation, la structure fibreuse pré-densifiée comprend un renfort fibreux formé par tissage tridimensionnel ou à partir d’une pluralité de strates fibreuses bidimensionnelles.In an exemplary embodiment, the pre-densified fibrous structure comprises a fibrous reinforcement formed by three-dimensional weaving or from a plurality of two-dimensional fibrous layers.
Dans un exemple de réalisation, la pièce est une pièce de turbomachine.In an exemplary embodiment, the part is a turbomachine part.
La pièce peut être une pièce de turbine, par exemple une pièce de turbine de moteur d’aéronef. La pièce peut par exemple être une aube de turbomachine, un secteur d’anneau de turbine ou un distributeur.The part may be a turbine part, for example an aircraft engine turbine part. The part can for example be a turbomachine blade, a turbine ring sector or a distributor.
Un exemple de procédé de fabrication d’une pièce en matériau CMC selon l’invention va maintenant être décrit en lien avec l’ordinogramme de la
Une première étape S10 du procédé peut consister à former la structure fibreuse par mise en œuvre d’une ou plusieurs opérations textiles comme un tissage tridimensionnel. La structure fibreuse peut être formée de fils céramiques, par exemple de fils en carbure de silicium. La structure fibreuse peut constituer le renfort fibreux 10 de la pièce en matériau composite à obtenir. Des exemples de fils en carbure de silicium utilisables peuvent être des fils commercialisés sous la référence « Nicalon », « Hi-Nicalon », « Hi-Nicalon-S » ou Tyranno SA3 de la société UBE Industries. Les fils céramiques de la structure fibreuse peuvent présenter une teneur en oxygène inférieure ou égale à 1% en pourcentage atomique. Les fils « Hi-Nicalon-S », par exemple, présentent une telle caractéristique. Par « tissage tridimensionnel » ou « tissage 3D », il faut comprendre un mode de tissage par lequel certains au moins des fils de chaine lient des fils de trame sur plusieurs couches de trame. Une inversion des rôles entre chaine et trame est possible dans le présent texte et doit être considérée comme couverte aussi par les revendications. La structure fibreuse peut par exemple présenter une armure interlock. Par « armure ou tissu interlock », il faut comprendre une armure de tissage 3D dont chaque couche de fils de chaîne lie plusieurs couches de fils de trame avec tous les fils de la même colonne de chaîne ayant le même mouvement dans le plan de l’armure. Il est aussi possible de partir de textures fibreuses telles que des tissus bidimensionnels ou des nappes unidirectionnelles, et d’obtenir la structure fibreuse par drapage de telles textures fibreuses sur une forme. Ces textures peuvent éventuellement être liées entre elles par exemple par couture ou implantation de fils pour former la structure fibreuse.A first step S10 of the process may consist of forming the fibrous structure by implementing one or more textile operations such as three-dimensional weaving. The fibrous structure can be formed from ceramic wires, for example silicon carbide wires. The fibrous structure can constitute the fibrous reinforcement 10 of the composite material part to be obtained. Examples of usable silicon carbide wires may be wires marketed under the reference “Nicalon”, “Hi-Nicalon”, “Hi-Nicalon-S” or Tyranno SA3 from the company UBE Industries. The ceramic yarns of the fibrous structure may have an oxygen content less than or equal to 1% in atomic percentage. “Hi-Nicalon-S” threads, for example, have such a characteristic. By “three-dimensional weaving” or “3D weaving”, we must understand a mode of weaving by which at least some of the warp threads bind weft threads on several weft layers. A reversal of roles between warp and weft is possible in the present text and must be considered as also covered by the claims. The fibrous structure can for example have an interlock weave. By “weave or interlock fabric”, we must understand a 3D weave weave in which each layer of warp threads links several layers of weft threads with all the threads of the same warp column having the same movement in the plane of the armor. It is also possible to start from fibrous textures such as two-dimensional fabrics or unidirectional webs, and to obtain the fibrous structure by draping such fibrous textures on a form. These textures can possibly be linked together, for example by sewing or implantation of threads to form the fibrous structure.
Dans une étape S20, on peut former une interphase 20 de défragilisation par infiltration chimique en phase vapeur (« Chemical Vapor Infiltration ») sur les fils de la structure fibreuse. La structure fibreuse peut être positionnée dans un outillage de conformation permettant de la mettre à la forme de la pièce à obtenir durant le dépôt de l’interphase. L’épaisseur e20de l’interphase peut par exemple être comprise entre 10 nm et 1000 nm, et par exemple entre 200 nm et 500 nm. Après formation de l’interphase, la structure fibreuse reste poreuse, la porosité accessible initiale n’étant comblée que pour une partie minoritaire par l’interphase. L’interphase peut être monocouche ou multicouches. L’interphase peut comporter au moins une couche de carbone pyrolytique (PyC), de nitrure de bore (BN), de nitrure de bore dopé au silicium (BN(Si), avec du silicium en une proportion massique comprise entre 5% et 40%, le complément étant du nitrure de bore) ou de carbone dopé au bore (BC, avec du bore en une proportion atomique comprise entre 5% et 20%, le complément étant du carbone). L’interphase a ici une fonction de défragilisation du matériau composite qui favorise la déviation de fissures éventuelles parvenant à l’interphase après s’être propagées dans la matrice, empêchant ou retardant la rupture de fibres par de telles fissures. En variante, on notera qu’il est possible de former l’interphase sur les fils avant la formation de la structure fibreuse, c’est-à-dire avant mise en œuvre de l’étape S10.In a step S20, an interphase 20 of defragmentation can be formed by chemical vapor infiltration (“Chemical Vapor Infiltration”) on the threads of the fibrous structure. The fibrous structure can be positioned in conformation tooling allowing it to be shaped into the shape of the part to be obtained during the deposition of the interphase. The thickness e 20 of the interphase can for example be between 10 nm and 1000 nm, and for example between 200 nm and 500 nm. After formation of the interphase, the fibrous structure remains porous, the initial accessible porosity being filled for only a minority part by the interphase. The interphase can be single-layer or multi-layer. The interphase may comprise at least one layer of pyrolytic carbon (PyC), boron nitride (BN), boron nitride doped with silicon (BN(Si), with silicon in a mass proportion of between 5% and 40 %, the complement being boron nitride) or carbon doped with boron (BC, with boron in an atomic proportion of between 5% and 20%, the complement being carbon). The interphase here has a function of weakening the composite material which promotes the deflection of possible cracks reaching the interphase after having propagated in the matrix, preventing or delaying the rupture of fibers by such cracks. Alternatively, it will be noted that it is possible to form the interphase on the wires before the formation of the fibrous structure, that is to say before implementation of step S10.
Il est ensuite réalisé une étape S30 de formation d’un dépôt de carbure de silicium. Cette étape S30 peut être séparée en deux phases. Lors de la première phase, la structure fibreuse est toujours dans l’outillage de conformation et une couche 301 de consolidation de carbure de silicium est déposée sur l’interphase 20 et le renfort fibreux 10. La couche 301 de consolidation peut être déposée au contact de l’interphase 20. Cette couche a une épaisseur suffisante pour lier suffisamment les fibres de sorte que la structure conserve sa forme sans assistance de l’outillage de maintien. Cette couche apporte une protection à l’interphase vis-à-vis de l’oxydation et peut être formée par infiltration chimique en phase vapeur de manière connue en soi, par exemple à partir d’une phase gazeuse comprenant du méthyltrichlorosilane (MTS) et de l’hydrogène (H2). L’épaisseur e301de la couche 301 de consolidation peut être supérieure ou égale à 0,1 µm, par exemple comprise entre 0,1 µm et 5 µm. Lors de la deuxième phase, la structure fibreuse consolidée et mise à la forme de la pièce à obtenir peut être retirée de l’outillage et la formation de la matrice de pré-densification peut être initiée en déposant une première couche 302 de celle-ci en carbure de silicium. La première couche 302 peut être déposée au contact de la couche 301 de consolidation. L’épaisseur e302de la première couche 302 peut être supérieure à l’épaisseur e301de la couche 301 de consolidation. Cette première couche 302 de carbure de silicium apporte une large contribution de performance mécanique au matériau composite et apporte une protection vis-à-vis du silicium fondu mis en œuvre lors de l’infiltration ultérieure. L’épaisseur e302de la première couche 302 peut être supérieure ou égale à 1 µm, par exemple comprise entre 1 µm et 20 µm. Comme pour la couche de consolidation, la première couche de la matrice de pré-densification peut être formée par infiltration chimique en phase vapeur de manière connue en soi. D’une manière générale, la matrice de pré-densification peut être formée par infiltration chimique en phase vapeur.A step S30 of forming a silicon carbide deposit is then carried out. This step S30 can be separated into two phases. During the first phase, the fibrous structure is still in the conformation tooling and a consolidation layer 301 of silicon carbide is deposited on the interphase 20 and the fibrous reinforcement 10. The consolidation layer 301 can be deposited in contact of the interphase 20. This layer has sufficient thickness to sufficiently bind the fibers so that the structure retains its shape without assistance from the holding tooling. This layer provides protection to the interphase against oxidation and can be formed by chemical vapor infiltration in a manner known per se, for example from a gas phase comprising methyltrichlorosilane (MTS) and hydrogen (H 2 ). The thickness e 301 of the consolidation layer 301 may be greater than or equal to 0.1 µm, for example between 0.1 µm and 5 µm. During the second phase, the fibrous structure consolidated and shaped into the part to be obtained can be removed from the tooling and the formation of the pre-densification matrix can be initiated by depositing a first layer 302 thereof. made of silicon carbide. The first layer 302 can be deposited in contact with the consolidation layer 301. The thickness e 302 of the first layer 302 may be greater than the thickness e 301 of the consolidation layer 301. This first layer 302 of silicon carbide provides a large contribution of mechanical performance to the composite material and provides protection against the molten silicon used during subsequent infiltration. The thickness e 302 of the first layer 302 may be greater than or equal to 1 µm, for example between 1 µm and 20 µm. As for the consolidation layer, the first layer of the pre-densification matrix can be formed by chemical vapor infiltration in a manner known per se. Generally speaking, the pre-densification matrix can be formed by chemical vapor infiltration.
Le procédé se poursuit par introduction d’une poudre 50 dans une porosité résiduelle de la structure pré-densifiée (étape S40). Cette poudre 50 peut être introduite dans la structure fibreuse par voie barbotine (« slurry-cast ») de manière connue en soi. La poudre comprend au moins une poudre de carbure de silicium et éventuellement une poudre de carbone et/ou une poudre de carbure de bore.The process continues by introducing a powder 50 into a residual porosity of the pre-densified structure (step S40). This powder 50 can be introduced into the fibrous structure by slurry-cast method in a manner known per se. The powder comprises at least one silicon carbide powder and optionally a carbon powder and/or a boron carbide powder.
La formation de la matrice de pré-densification peut être poursuivie par formation du dépôt protecteur 40 sur la première couche 302 et sur la poudre 50 (étape S50). La poudre 50 est intercalée entre la première 302 et la deuxième couche 40. Dans l’exemple illustré aux figures 2 et 3, la deuxième couche protectrice 40 est au contact à la fois de la poudre 50 et de la première couche 302 mais on ne sort pas du cadre de l’invention si ce n’est pas le cas, comme cela sera détaillé dans la suite. Comme indiqué plus haut, ce dépôt 40 permet de protéger le carbure de silicium sous-jacent de l’attaque par le silicium fondu. Différentes structures sont envisageables pour ce dépôt comme il va à présent être décrit.The formation of the pre-densification matrix can be continued by formation of the protective deposit 40 on the first layer 302 and on the powder 50 (step S50). The powder 50 is interposed between the first 302 and the second layer 40. In the example illustrated in Figures 2 and 3, the second protective layer 40 is in contact with both the powder 50 and the first layer 302 but we do not does not fall outside the scope of the invention if this is not the case, as will be detailed below. As indicated above, this deposit 40 makes it possible to protect the underlying silicon carbide from attack by molten silicon. Different structures are possible for this deposit as will now be described.
Dans l’exemple de la
D’autres variantes de matrice de pré-densification sont possibles comme illustré aux figures 4 et 5. Il a ainsi été envisagé de remplacer les deux dépôts 301 et 302 précédemment décrits par une unique étape de dépôt de la couche 301 de consolidation qui a été rallongée et forme la première couche de la matrice de pré-densification. Cela permet de supprimer une étape en réacteur CVI. La poudre 50 est intercalée entre la couche 301 et la deuxième couche 40 qui peut également être plus épaisse que celle des exemples des figures 2 et 3. A titre d’exemple dans ce cas, l’épaisseur e301de la couche 301 peut être comprise entre 1 µm et 10 µm, et l’épaisseur de la couche 40 peut être comprise entre 1 µm et 10 µm. Other variants of pre-densification matrix are possible as illustrated in Figures 4 and 5. It was thus envisaged to replace the two deposits 301 and 302 previously described by a single step of depositing the consolidation layer 301 which was elongated and forms the first layer of the pre-densification matrix. This makes it possible to eliminate a step in the CVI reactor. The powder 50 is interposed between the layer 301 and the second layer 40 which can also be thicker than that of the examples in Figures 2 and 3. As an example in this case, the thickness e 301 of the layer 301 can be between 1 µm and 10 µm, and the thickness of layer 40 can be between 1 µm and 10 µm.
Selon une variante, on peut déposer par CVI un dépôt intercalaire 60 comprenant du carbure de silicium et/ou un matériau déviateur de fissures entre la poudre 50 et la couche 40. Ce dépôt peut être sous la forme d’une couche de carbure de silicium ou d’un empilement de couches de matériaux différents. Ce dernier cas est illustré à la
Quel que soit le mode de réalisation considéré, le taux volumique de porosité résiduelle de la structure fibreuse pré-densifiée peut être inférieur ou égal à 25%, par exemple compris entre 15% et 25%.Whatever the embodiment considered, the residual porosity volume rate of the pre-densified fibrous structure can be less than or equal to 25%, for example between 15% and 25%.
Une fois la matrice de pré-densification formée, on réalise l’étape S60 durant laquelle on infiltre la porosité résiduelle avec une composition d’infiltration à l’état fondu comprenant au moins du silicium de manière à former une matrice céramique dans la porosité de la structure fibreuse. La formation de cette matrice céramique peut permettre de finaliser la densification de la pièce. Cette étape d’infiltration correspond à une étape d’infiltration à l’état fondu. La composition d’infiltration peut être constituée de silicium pur fondu ou en variante être sous la forme d’un alliage fondu de silicium et d’un ou plusieurs autres constituants. La composition d’infiltration peut comprendre majoritairement en masse du silicium, c’est-à-dire présenter une teneur massique en silicium supérieure ou égale à 50%. La composition d’infiltration peut par exemple présenter une teneur massique en silicium supérieure ou égale à 75%. Le(s) constituant(s) présent(s) au sein de l’alliage de silicium peuvent être choisi(s) parmi B, Al, Mo, Ti, Ge et leurs mélanges. Lorsque la composition pulvérulente comprend des particules de carbone, une réaction chimique peut se produire entre la composition d’infiltration et ces particules de carbone lors de l’infiltration aboutissant à la formation de carbure de silicium.Once the pre-densification matrix is formed, step S60 is carried out during which the residual porosity is infiltrated with a melt infiltration composition comprising at least silicon so as to form a ceramic matrix in the porosity of the fibrous structure. The formation of this ceramic matrix can make it possible to finalize the densification of the part. This infiltration step corresponds to a melt infiltration step. The infiltration composition may consist of pure molten silicon or alternatively be in the form of a molten alloy of silicon and one or more other constituents. The infiltration composition may comprise a majority of silicon by 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 within the silicon alloy can be chosen from B, Al, Mo, Ti, Ge and their mixtures. When the powder composition comprises carbon particles, a chemical reaction can occur between the infiltration composition and these carbon particles during infiltration resulting in the formation of silicon carbide.
Après l’étape S60, on obtient une pièce en matériau CMC. Une telle pièce en matériau CMC peut être une pièce statique ou rotative de turbomachine. Des exemples de pièces de turbomachine ont été mentionnés plus haut. Une telle pièce peut en outre être revêtue d’un revêtement de barrière environnementale ou thermique avant son utilisation.After step S60, we obtain a part made of CMC material. Such a part made of CMC material can be a static or rotating part of a turbomachine. Examples of turbomachine parts have been mentioned above. Such a part may additionally be coated with an environmental or thermal barrier coating before use.
L’expression « compris(e) entre … et … » doit se comprendre comme incluant les bornes.The expression “between… and…” must be understood as including the limits.
Claims (12)
- l’infiltration (S60) d’une structure fibreuse pré-densifiée par une composition d’infiltration à l’état fondu comprenant du silicium afin de former une matrice céramique dans une porosité résiduelle de ladite structure fibreuse pré-densifiée, ladite structure fibreuse pré-densifiée comprenant une matrice de pré-densification comprenant une première couche (301 ; 302) de carbure de silicium et une deuxième couche (40) protectrice recouvrant la première couche et apte à protéger celle-ci d’une attaque par le silicium de la composition d’infiltration, la deuxième couche protectrice étant formée par un système binaire B-C ou par un système ternaire Si-B-C, une poudre (50) de carbure de silicium étant intercalée entre la première et la deuxième couches.Process for manufacturing a part made of ceramic matrix composite material, comprising:
- infiltration (S60) of a pre-densified fibrous structure with a melt infiltration composition comprising silicon in order to form a ceramic matrix in a residual porosity of said pre-densified fibrous structure, said fibrous structure pre-densified comprising a pre-densification matrix comprising a first layer (301; 302) of silicon carbide and a second protective layer (40) covering the first layer and capable of protecting the latter from attack by silicon the infiltration composition, the second protective layer being formed by a binary BC system or by a ternary Si-BC system, a silicon carbide powder (50) being interposed between the first and second layers.
Method according to any one of claims 1 to 11, in which the part is a turbomachine part.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR2210906A FR3141167A1 (en) | 2022-10-21 | 2022-10-21 | Process for manufacturing a part made of ceramic matrix composite material |
| PCT/FR2023/051584 WO2024084153A1 (en) | 2022-10-21 | 2023-10-11 | Method for manufacturing a part made of ceramic matrix composite material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR2210906A FR3141167A1 (en) | 2022-10-21 | 2022-10-21 | Process for manufacturing a part made of ceramic matrix composite material |
| FR2210906 | 2022-10-21 |
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| FR3141167A1 true FR3141167A1 (en) | 2024-04-26 |
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| WO (1) | WO2024084153A1 (en) |
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| FR2668477A1 (en) | 1990-10-26 | 1992-04-30 | Europ Propulsion | REFRACTORY COMPOSITE MATERIAL PROTECTED AGAINST CORROSION, AND METHOD FOR THE PRODUCTION THEREOF. |
| WO1996030317A1 (en) | 1995-03-28 | 1996-10-03 | Societe Europeenne De Propulsion | Composite material protected from oxidation by a self-healing matrix, and method for making same |
| FR2950622A1 (en) * | 2009-09-28 | 2011-04-01 | Snecma Propulsion Solide | PIECE OF COMPOSITE MATERIAL WITH CERAMIC MATRIX AND METHOD FOR MANUFACTURING THE SAME |
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| WO2016001026A1 (en) * | 2014-07-03 | 2016-01-07 | Herakles | Part coated with a surface coating and associated methods |
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2022
- 2022-10-21 FR FR2210906A patent/FR3141167A1/en active Pending
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| FR2668477A1 (en) | 1990-10-26 | 1992-04-30 | Europ Propulsion | REFRACTORY COMPOSITE MATERIAL PROTECTED AGAINST CORROSION, AND METHOD FOR THE PRODUCTION THEREOF. |
| WO1996030317A1 (en) | 1995-03-28 | 1996-10-03 | Societe Europeenne De Propulsion | Composite material protected from oxidation by a self-healing matrix, and method for making same |
| FR2950622A1 (en) * | 2009-09-28 | 2011-04-01 | Snecma Propulsion Solide | PIECE OF COMPOSITE MATERIAL WITH CERAMIC MATRIX AND METHOD FOR MANUFACTURING THE SAME |
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| WO2016001026A1 (en) * | 2014-07-03 | 2016-01-07 | Herakles | Part coated with a surface coating and associated methods |
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