FR3115533A1 - Process for manufacturing a composite material part - Google Patents
Process for manufacturing a composite material part Download PDFInfo
- Publication number
- FR3115533A1 FR3115533A1 FR2010979A FR2010979A FR3115533A1 FR 3115533 A1 FR3115533 A1 FR 3115533A1 FR 2010979 A FR2010979 A FR 2010979A FR 2010979 A FR2010979 A FR 2010979A FR 3115533 A1 FR3115533 A1 FR 3115533A1
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- particles
- silicon
- carbon
- hot pressing
- metallic element
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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
- 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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Abstract
Procédé de fabrication d’une pièce en matériau composite La présente invention concerne la fabrication d’une pièce en matériau composite à matrice céramique durant lequel une ébauche déliantée est pressée à chaud (E5) pour former la matrice céramique par réaction chimique à l’état solide entre du carbone d’une composition pulvérulente et du silicium ou un élément métallique. Figure pour l’abrégé : Fig. 1.Process for manufacturing a composite material part The present invention relates to the manufacturing of a composite material part with a ceramic matrix during which a debinded blank is hot pressed (E5) to form the ceramic matrix by chemical reaction in the state solid between carbon of a powdery composition and silicon or a metallic element. Figure for abstract: Fig. 1.
Description
La présente invention se rapport à la fabrication des pièces en matériau composite, et plus particulièrement des pièces en matériau composite à matrice céramique (pièces en matériau CMC).The present invention relates to the manufacture of parts made of composite material, and more particularly parts made of composite material with a ceramic matrix (parts made of CMC material).
Les matériaux CMC, connus pour leurs bonnes propriétés mécaniques qui les rendent aptes à constituer des éléments de structures et pour conserver ces propriétés à températures élevées, constituent une alternative viable aux traditionnelles pièces métalliques. Leur masse réduite par rapport à leur équivalent métallique en font des pièces de choix pour répondre aux problématiques d’augmentation du rendement et de réduction des émissions polluantes des moteurs dans le domaine aéronautique.CMC materials, known for their good mechanical properties which make them suitable for constituting structural elements and for maintaining these properties at high temperatures, constitute a viable alternative to traditional metal parts. Their reduced mass compared to their metallic equivalent makes them the parts of choice to meet the problems of increasing efficiency and reducing polluting emissions from engines in the aeronautical field.
Les pièces en matériau CMC peuvent comprendre un renfort fibreux continu sous la forme d’un textile tissé, qui est densifié par une matrice céramique. Le renfort fibreux comprend ainsi des fibres longues continues, dont l’orientation peut être adaptée aux directions principales de sollicitation de la pièce lors de son utilisation. La préforme destinée à former le renfort fibreux est tissée à partir des fibres continues aux dimensions de la pièce à l’aide d’un métier à tisser adapté. L’étape de tissage est un processus long et coûteux, et qui n’est pas optimal pour réaliser des pièces de petite taille ou de géométrie complexe.CMC material parts can include a continuous fibrous reinforcement in the form of a woven textile, which is densified by a ceramic matrix. The fibrous reinforcement thus comprises long continuous fibers, the orientation of which can be adapted to the main directions of stress on the part during its use. The preform intended to form the fibrous reinforcement is woven from continuous fibers to the dimensions of the part using a suitable loom. The weaving step is a long and expensive process, and it is not optimal for making small parts or complex geometries.
En outre, il est connu d’obtenir la matrice de ces pièces en matériau CMC par la technique d’infiltration à l’état fondu. Selon cette technique, on peut introduire une composition fondue, par exemple à base de silicium, dans la porosité d’une structure fibreuse comprenant des particules de carbure de silicium afin de former une matrice céramique densifiant la structure fibreuse. Il est souhaitable dans cette technique que la composition fondue pénètre de manière homogène et complète au sein de la porosité de la structure fibreuse, afin que la pièce obtenue présente une porosité résiduelle minimale et donc des propriétés mécaniques optimisées. Toutefois, certaines des techniques d’infiltration à l’état fondu ne donnent pas des résultats entièrement satisfaisants dans la mesure où le degré d’avancée de la composition fondue dans la porosité peut être limité, conduisant à une pénétration inhomogène dans la structure fibreuse. Ce caractère inhomogène peut être d’autant plus prononcé dans le cadre des techniques d’infiltration à l’état fondu réactive (« Reactive Melt Infiltration ») où des particules de carbone sont présentes dans la structure fibreuse. Dans ce dernier cas, le produit de réaction entre la composition fondue et les particules de carbone peut en effet conduire à un bouchage local de la porosité de la préforme, rendant plus difficile l’avancée de la composition fondue.In addition, it is known to obtain the matrix of these parts in CMC material by the melt infiltration technique. According to this technique, a molten composition, for example based on silicon, can be introduced into the pores of a fibrous structure comprising particles of silicon carbide in order to form a ceramic matrix which densifies the fibrous structure. It is desirable in this technique for the molten composition to penetrate homogeneously and completely within the porosity of the fibrous structure, so that the part obtained has minimal residual porosity and therefore optimized mechanical properties. However, some of the melt infiltration techniques do not give entirely satisfactory results since the degree of advancement of the molten composition into the porosity can be limited, leading to inhomogeneous penetration into the fibrous structure. This inhomogeneous character can be all the more pronounced in the context of reactive melt infiltration techniques where carbon particles are present in the fibrous structure. In the latter case, the reaction product between the molten composition and the carbon particles can in fact lead to local clogging of the porosity of the preform, making it more difficult for the molten composition to advance.
Il existe donc un besoin pour un procédé de fabrication d’une pièce en matériau CMC permettant l’obtention d’une densification homogène et notamment adapté à la fabrication de pièces de petite taille et ayant éventuellement une géométrie complexe.There is therefore a need for a process for manufacturing a part in CMC material allowing obtaining a homogeneous densification and in particular suitable for the manufacture of small-sized parts and possibly having a complex geometry.
La présente invention concerne un procédé de fabrication d’une pièce en matériau composite à matrice céramique, comprenant au moins :
- le déliantage d’une ébauche de la pièce à obtenir comprenant un liant et une composition pulvérulente comprenant du carbone présente dans le liant, la composition pulvérulente comprenant :
(i) des premières particules de renfort, et
(ii) des deuxièmes particules, distinctes des premières particules, ayant une surface réactive comprenant du silicium ou un élément métallique, et
- le pressage à chaud de l’ébauche déliantée durant lequel il y a réaction thermochimique à l’état solide entre le carbone de la composition pulvérulente et le silicium ou l’élément métallique de la surface réactive des deuxièmes particules afin de former la matrice céramique.The present invention relates to a method for manufacturing a part made of composite material with a ceramic matrix, comprising at least:
- the debinding of a blank of the part to be obtained comprising a binder and a powder composition comprising carbon present in the binder, the powder composition comprising:
(i) first reinforcing particles, and
(ii) second particles, distinct from the first particles, having a reactive surface comprising silicon or a metallic element, and
- hot pressing of the debinded blank during which there is thermochemical reaction in the solid state between the carbon of the powdery composition and the silicon or the metallic element of the reactive surface of the second particles in order to form the ceramic matrix .
L’invention propose de réaliser une densification de la pièce par réaction chimique à l’état solide, sans fusion de la surface réactive des deuxièmes particules, alors que l’ébauche déliantée est comprimée durant le pressage à chaud. Durant le pressage à chaud, on impose une température inférieure à la température de fusion de la surface réactive mais suffisante pour activer la réaction chimique entre le silicium ou l’élément métallique de cette surface réactive et le carbone de la composition pulvérulente. On obtient ainsi une densification homogène de la pièce du fait d’une réduction de la porosité et de la suppression du phénomène de bouchage (« choking off ») qui peut être rencontré dans des techniques d’infiltration à l’état fondu réactive de l’art antérieur. On évite aussi le phénomène d’ascension du métal fondu. En outre, l’invention permet de conserver un nombre d’étapes réduit en s’affranchissant en particulier de la réalisation d’une étape de désoxydation des charges présentes, avant l’infiltration par une composition fondue, utile pour faciliter la montée capillaire de celle-ci. L’invention propose en outre la mise en œuvre d’un renfort particulaire, simplifiant la fabrication par rapport à un renfort fibreux tissé et permettant d’accéder plus facilement à des pièces de petite taille ou de géométrie complexe.The invention proposes to densify the part by chemical reaction in the solid state, without melting the reactive surface of the second particles, while the debinded blank is compressed during hot pressing. During hot pressing, a temperature lower than the melting point of the reactive surface is imposed but sufficient to activate the chemical reaction between the silicon or the metallic element of this reactive surface and the carbon of the pulverulent composition. A homogeneous densification of the part is thus obtained due to a reduction in the porosity and the elimination of the phenomenon of clogging ("choking off") which can be encountered in techniques of infiltration in the reactive molten state of the prior art. We also avoid the phenomenon of ascent of the molten metal. In addition, the invention makes it possible to keep a reduced number of steps by dispensing in particular with carrying out a step of deoxidizing the fillers present, before infiltration by a molten composition, useful for facilitating the capillary rise of this one. The invention also proposes the implementation of a particulate reinforcement, simplifying the manufacture compared to a woven fibrous reinforcement and allowing easier access to small parts or parts of complex geometry.
Le carbone de la composition pulvérulente réagissant avec le silicium ou l’élément métallique peut être apporté de diverses manières comme il va à présent être décrit.The carbon of the pulverulent composition reacting with the silicon or the metallic element can be provided in various ways as will now be described.
Ainsi, dans un exemple de réalisation, les premières particules comprennent un noyau enrobé par un revêtement comprenant au moins une couche de surface en carbone, le carbone de cette couche de surface réagissant avec le silicium ou l’élément métallique durant le pressage à chaud.Thus, in an exemplary embodiment, the first particles comprise a core coated with a coating comprising at least one carbon surface layer, the carbon of this surface layer reacting with the silicon or the metallic element during the hot pressing.
En variante, les premières particules comprennent un noyau enrobé par un revêtement comprenant au moins une couche de surface en carbure de silicium et une couche intermédiaire en carbone située entre la couche de surface et le noyau, le carbone de la couche intermédiaire réagissant avec le silicium ou l’élément métallique durant le pressage à chaud. La couche de surface peut être sacrificielle afin de permettre au carbone sous-jacent de réagir avec le silicium ou l’élément métallique.Alternatively, the first particles comprise a core coated with a coating comprising at least one surface layer of silicon carbide and an intermediate layer of carbon located between the surface layer and the core, the carbon of the intermediate layer reacting with the silicon or metal part during hot pressing. The surface layer can be sacrificial to allow the underlying carbon to react with the silicon or metallic element.
Dans ce cas, la couche de surface en carbure de silicium ralentit la diffusion du silicium mais permet la réaction chimique avec le carbone de la couche intermédiaire.In this case, the surface layer of silicon carbide slows down the diffusion of the silicon but allows the chemical reaction with the carbon of the intermediate layer.
Les deux variantes qui viennent d’être décrites concernent un apport de carbone par les premières particules mais d’autres solutions sont envisageables lesquelles peuvent éventuellement être combinées entre elles ou à ce qui vient d’être décrit.The two variants which have just been described relate to a supply of carbon by the first particles but other solutions are possible which can possibly be combined with each other or with what has just been described.
Dans un exemple de réalisation, les deuxièmes particules comprennent en outre une région en carbone enrobée par la surface réactive, le carbone de cette région réagissant avec le silicium ou l’élément métallique durant le pressage à chaud.In an exemplary embodiment, the second particles further comprise a carbon region coated by the reactive surface, the carbon of this region reacting with the silicon or the metallic element during the hot pressing.
Dans un exemple de réalisation, la composition pulvérulente comprend en outre des troisièmes particules de carbone, distinctes des premières et deuxièmes particules, réagissant avec le silicium ou l’élément métallique durant le pressage à chaud.In an exemplary embodiment, the powder composition further comprises third carbon particles, distinct from the first and second particles, reacting with the silicon or the metallic element during the hot pressing.
Dans un exemple de réalisation, la surface réactive des deuxièmes particules est formée par du silicium ou un alliage de silicium.In an exemplary embodiment, the reactive surface of the second particles is formed by silicon or a silicon alloy.
Dans ce cas, le procédé permet de diminuer le taux de silicium libre dans la pièce finale par rapport à une infiltration de silicium fondu classique, améliorant ainsi la tenue en fluage à haute température.In this case, the process makes it possible to reduce the rate of free silicon in the final part compared to a conventional molten silicon infiltration, thus improving the creep resistance at high temperature.
En variante, la surface réactive des deuxièmes particules est formée par un métal de transition ou un alliage du métal de transition. Le métal de transition peut être le zirconium ou le titane.As a variant, the reactive surface of the second particles is formed by a transition metal or an alloy of the transition metal. The transition metal can be zirconium or titanium.
Dans un exemple de réalisation, les premières particules comprennent un noyau enrobé par une interphase.In an exemplary embodiment, the first particles comprise a core coated by an interphase.
Dans un exemple de réalisation, les premières particules sont des fibres courtes ayant une longueur moyenne comprise entre 50 µm et 5000 µm.In an exemplary embodiment, the first particles are short fibers having an average length of between 50 μm and 5000 μm.
Une dimension moyenne désigne la dimension donnée par la distribution granulométrique statistique à la moitié de la population, dite D50.An average dimension designates the dimension given by the statistical particle size distribution to half of the population, called D50.
En variante, les premières particules peuvent être sous la forme de grains plutôt que de fibres courtes. Les premières particules peuvent ainsi présenter une forme sphérique ou ellipsoïdale. Dans ce cas, la taille moyenne (D50) des premières particules peut être comprise entre 10 µm et 300 µm, par exemple entre 40 µm et 100 µm.Alternatively, the first particles may be in the form of grains rather than short fibers. The first particles can thus have a spherical or ellipsoidal shape. In this case, the average size (D50) of the first particles can be between 10 μm and 300 μm, for example between 40 μm and 100 μm.
Dans un exemple de réalisation, les premières particules comprennent du carbure du silicium, par exemple un noyau de carbure de silicium enrobé par un revêtement tel que décrit plus haut.In an exemplary embodiment, the first particles comprise silicon carbide, for example a core of silicon carbide coated with a coating as described above.
En plus des premières, deuxièmes et éventuellement troisièmes particules, la composition pulvérulente peut comprendre une charge inerte de carbure de silicium. Dans le cas d’une surface réactive comprenant du silicium, cela permet d’obtenir une matrice céramique SiC-Si après le pressage à chaud.In addition to the first, second and optionally third particles, the pulverulent composition can comprise an inert filler of silicon carbide. In the case of a reactive surface comprising silicon, this makes it possible to obtain a SiC-Si ceramic matrix after hot pressing.
Dans un exemple de réalisation, une température imposée lors du pressage à chaud est comprise entre 1150°C et 1300°C, par exemple comprise entre 1200°C et 1300°C, par exemple comprise entre 1200°C et 1250°C.In an exemplary embodiment, a temperature imposed during the hot pressing is between 1150°C and 1300°C, for example between 1200°C and 1300°C, for example between 1200°C and 1250°C.
Une telle caractéristique permet une activation rapide de la réaction chimique à l’état solide durant le pressage à chaud.Such a feature allows rapid activation of the solid state chemical reaction during hot pressing.
Dans un exemple de réalisation, une pression imposée lors du pressage à chaud est supérieure ou égale à 50 MPa, par exemple comprise entre 50 MPa et 75 MPa.In an exemplary embodiment, a pressure imposed during the hot pressing is greater than or equal to 50 MPa, for example between 50 MPa and 75 MPa.
Une telle caractéristique participe à améliorer davantage encore l’homogénéité de la densification de la pièce.Such a characteristic helps to further improve the homogeneity of the densification of the part.
Dans un exemple de réalisation, la teneur volumique en composition pulvérulente dans l’ébauche est comprise entre 45% et 85% et la teneur volumique en liant dans l’ébauche est comprise entre 15% et 55%, et la composition pulvérulente comprend :
- les premières particules dans en une teneur volumique dans la composition pulvérulente comprise entre 10% et 50%, par exemple comprise entre 15% et 35%,
- les deuxièmes particules, seules ou en combinaison avec une charge inerte éventuellement présente, en une teneur volumique dans la composition pulvérulente comprise entre 50% et 90%, par exemple entre 65% et 85%, et
- éventuellement des troisièmes particules de carbone, distinctes des premières et deuxièmes particules, en une teneur volumique dans la composition pulvérulente comprise entre 1% et 10%.In an exemplary embodiment, the volume content of powder composition in the blank is between 45% and 85% and the volume content of binder in the blank is between 15% and 55%, and the powder composition comprises:
- the first particles in a content by volume in the pulverulent composition of between 10% and 50%, for example between 15% and 35%,
- the second particles, alone or in combination with an inert filler optionally present, in a content by volume in the pulverulent composition of between 50% and 90%, for example between 65% and 85%, and
- optionally third carbon particles, distinct from the first and second particles, in a content by volume in the pulverulent composition of between 1% and 10%.
Sauf mention contraire, ces teneurs sont prises avant le début du pressage à chaud.Unless otherwise stated, these contents are taken before the start of hot pressing.
Le procédé peut tout d’abord comprendre une étape d’obtention des premières particules et deuxièmes particules (étape E1 à la
La
Le revêtement 14 peut être multicouches et comporter une interphase 16, comme illustré. L’interphase 16 peut être au contact du noyau 12. L’épaisseur e1de l’interphase 16 peut par exemple être comprise entre 10 nm et 1000 nm, et par exemple entre 10 nm et 500 nm. L’interphase 16 peut être monocouche ou multicouches. Dans l’exemple illustré, l’interphase 16 est monocouche. L’interphase 16 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), de nitrure de silicium (Si3N4) 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 16 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 du renfort par de telles fissures.Coating 14 may be multi-layered and include an interphase 16, as shown. The interphase 16 can be in contact with the core 12. The thickness e 1 of the interphase 16 can for example be between 10 nm and 1000 nm, and for example between 10 nm and 500 nm. The interphase 16 can be monolayer or multilayer. In the example illustrated, the interphase 16 is monolayer. The interphase 16 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 balance being boron nitride), silicon nitride (Si 3 N 4 ) or boron-doped carbon (BC, with boron in an atomic proportion between 5% and 20%, the balance being carbon). The interphase 16 here has a function of weakening the composite material which promotes the deflection of any cracks reaching the interphase after having propagated in the matrix, preventing or delaying the rupture of the reinforcement by such cracks.
Le revêtement 14 peut en outre comprendre des couches supplémentaires recouvrant l’interphase 16. Le revêtement 14 peut ainsi comprendre une couche 18 en carbure de silicium recouvrant l’interphase 16. La couche 18 en carbure de silicium peut être au contact de l’interphase 16. La couche 18 peut avoir pour fonction de protéger l’interphase lors de la formation de la matrice. L’épaisseur e2de la couche 18 peut être supérieure ou égale à 0,5 µm, par exemple supérieure ou égale à 1 µm, par exemple comprise entre 0,5 µm et 5 µm, par exemple comprise entre 1 µm et 3 µm. Le revêtement 14 peut en outre comprendre une couche de surface 20 en carbone recouvrant la couche 18 en carbure de silicium. La couche de surface 20 peut être au contact de la couche 18. L’épaisseur e3de la couche de surface 20 peut être supérieure ou égale à 100 nm, par exemple comprise entre 100 nm et 2 µm. L’épaisseur e3de la couche de surface 20 peut être inférieure ou égale à 2 µm. Dans l’exemple de la
La
Le revêtement 14 ou 140 peut être formé directement sur le noyau 12 ou, en variante, sur fibre longue avant découpe et broyage. Le revêtement 14 ou 140 peut être formé par dépôt chimique en phase vapeur par défilement de fibre longue dans une enceinte, ou par exemple par dépôt chimique en phase vapeur en lit fluidisé s’il est recherché de revêtir directement le noyau 12.The coating 14 or 140 can be formed directly on the core 12 or, alternatively, on long fiber before cutting and grinding. The coating 14 or 140 can be formed by chemical vapor deposition by scrolling a long fiber in an enclosure, or for example by chemical vapor deposition in a fluidized bed if it is desired to coat the core 12 directly.
On vient de décrire des structures possibles pour les premières particules 10 et 100 en lien avec les figures 2 et 3. L’invention n’est pas limitée à de telles structures et d’autres variantes non illustrées sont possibles. On peut en particulier mettre en œuvre des premières particules ayant la structure selon la
La
Dans l’exemple de la
Les premières 10, 100 et deuxièmes particules 200 peuvent être mélangées dans un liant afin d’obtenir la composition destinée à former l’ébauche (étape E2). Le liant peut être un liant polymérique. Le liant peut par exemple comprendre une résine thermoplastique ou thermodurcissable. Dans un exemple de réalisation, le liant peut comprendre au moins un polymère thermoplastique. Par exemple, le liant peut comprendre au moins un composé choisi parmi les suivants : alcool polyvinylique (PVA), polyéthylène glycol (PEG), polypropylène (PP), polyoxyméthylène (POM), polytéréphtalate d’éthylène (PET). Dans un exemple de réalisation, le liant peut comprendre au moins un polymère thermodurcissable. Par exemple, le liant peut comprendre au moins un composé choisi parmi les suivants : résines époxydes, résines phénoliques, résines pré-céramiques. Le liant peut comprendre de l’acide stéarique.The first 10, 100 and second 200 particles can be mixed in a binder in order to obtain the composition intended to form the blank (step E2). The binder can be a polymeric binder. The binder can for example comprise a thermoplastic or thermosetting resin. In an exemplary embodiment, the binder can comprise at least one thermoplastic polymer. For example, the binder may comprise at least one compound chosen from the following: polyvinyl alcohol (PVA), polyethylene glycol (PEG), polypropylene (PP), polyoxymethylene (POM), polyethylene terephthalate (PET). In an exemplary embodiment, the binder can comprise at least one thermosetting polymer. For example, the binder can comprise at least one compound chosen from the following: epoxy resins, phenolic resins, pre-ceramic resins. The binder may include stearic acid.
On peut adjoindre au mélange des troisièmes particules de carbone, distinctes des premières 10, 100 et deuxièmes 200 particules, qui peuvent réagir avec le silicium ou l’élément métallique durant le pressage à chaud afin de participer à la formation de la matrice céramique. On peut aussi adjoindre une charge inerte de carbure de silicium, distincte des premières 10, 100 et deuxièmes 200 particules.Third carbon particles can be added to the mixture, distinct from the first 10, 100 and second 200 particles, which can react with the silicon or the metallic element during the hot pressing in order to participate in the formation of the ceramic matrix. It is also possible to add an inert filler of silicon carbide, distinct from the first 10, 100 and second 200 particles.
Avant déliantage, le mélange obtenu ou l’ébauche peut comprendre la composition pulvérulente en une teneur volumique comprise entre 45% et 85% et le liant en une teneur volumique comprise entre 15% et 55%. La composition pulvérulente peut comprendre:
- les premières particules 10, 100 en une teneur volumique dans la composition pulvérulente comprise entre 10% et 50%, par exemple comprise entre 15% et 35%,
- les deuxièmes particules 200, seules ou en combinaison avec la charge inerte de carbure de silicium éventuellement présente, en une teneur volumique dans la composition pulvérulente comprise entre 50% et 90%, par exemple entre 65% et 85%, et
- éventuellement les troisièmes particules de carbone en une teneur volumique dans la composition pulvérulente comprise entre 1% et 10%.Before debinding, the mixture obtained or the blank may comprise the pulverulent composition in a content by volume of between 45% and 85% and the binder in a content by volume of between 15% and 55%. The powder composition may include:
- the first particles 10, 100 in a content by volume in the pulverulent composition of between 10% and 50%, for example between 15% and 35%,
- the second particles 200, alone or in combination with the inert filler of silicon carbide possibly present, in a content by volume in the pulverulent composition of between 50% and 90%, for example between 65% and 85%, and
- optionally the third carbon particles in a volume content in the powder composition of between 1% and 10%.
La composition pulvérulente comprenant les premières, deuxièmes, et éventuellement la charge inerte et/ou les troisièmes particules, peut être dispersée de manière homogène dans le liant.The pulverulent composition comprising the first, second, and optionally the inert filler and/or the third particles, can be dispersed homogeneously in the binder.
Selon un exemple, on peut utiliser un mélange comprenant une composition pulvérulente qui comprend :According to one example, it is possible to use a mixture comprising a powder composition which comprises:
- des premières particules à raison de 15% en teneur volumique dans la composition pulvérulente, sous la forme de fibres courtes de carbure de silicium ayant une longueur moyenne de 250 µm et un diamètre moyen compris entre 8 µm et 12 µm, revêtues par une interphase BN de 0,5 µm et d’une couche de carbure de silicium d’épaisseur comprise entre 1 µm et 2 µm,- first particles at a rate of 15% by volume content in the pulverulent composition, in the form of short fibers of silicon carbide having an average length of 250 μm and an average diameter of between 8 μm and 12 μm, coated with an interphase BN of 0.5 µm and a layer of silicon carbide with a thickness of between 1 µm and 2 µm,
- des deuxièmes particules formées de silicium ou d’un alliage de silicium, ou ayant une surface réactive de silicium ou d’un alliage de silicium enrobant une région de composition différente, les deuxièmes particules étant présentes à raison de 10% en teneur volumique dans la composition pulvérulente, et- second particles formed of silicon or of a silicon alloy, or having a reactive surface of silicon or of a silicon alloy coating a region of different composition, the second particles being present at a rate of 10% by volume content in the powder composition, and
- une charge inerte de carbure de silicium ayant une taille moyenne comprise entre 1 µm et 50 µm et présente à raison de 75% en teneur volumique dans la composition pulvérulente.- an inert filler of silicon carbide having an average size of between 1 μm and 50 μm and present at a rate of 75% by volume content in the pulverulent composition.
On procède ensuite à la formation de l’ébauche à partir du mélange obtenu par introduction dans un moule (étape E3) et à une élimination du liant, par dissolution chimique ou traitement thermique ou thermochimique (étape E4) afin d’obtenir une ébauche déliantée. Les techniques de formation du mélange, de l’ébauche et de déliantage sont connues en soi et ne nécessitent pas d’être davantage détaillées ici.The blank is then formed from the mixture obtained by introduction into a mold (step E3) and removal of the binder, by chemical dissolution or heat or thermochemical treatment (step E4) in order to obtain a debinded blank . The techniques for forming the mixture, the blank and the debinding are known per se and do not need to be further detailed here.
Le procédé se poursuit par une étape de pressage à chaud (étape E5) durant lequel l’ébauche déliantée est comprimée sous température afin de réduire la porosité obtenue à l’issue du déliantage. On réalise durant le pressage à chaud une densification de l’ébauche déliantée durant laquelle la porosité va progressivement se réduire et l’ébauche se contracter pour atteindre les dimensions de la pièce finale. Durant le pressage à chaud, on impose une température inférieure à la température de fusion de la surface réactive mais suffisante pour activer la réaction chimique à l’état solide entre du carbone présent dans la composition pulvérulente et le silicium ou l’élément métallique de la surface réactive des deuxièmes particules, de sorte à former la matrice céramique. Comme indiqué plus haut, le carbone réactif peut être apporté par les premières particules 10,100 et/ou par les deuxièmes particules 200 et/ou par les troisièmes particules. On notera que dans l’hypothèse où un résidu carboné de pyrolyse du liant demeure après le déliantage, ce résidu peut apporter du carbone réactif supplémentaire réagissant avec le silicium ou l’élément métallique pour participer à la formation de la matrice céramique. Les deuxièmes particules peuvent être dispersées de manière homogène dans l’ébauche déliantée subissant le pressage à chaud. Lors du pressage à chaud, la réaction thermochimique aboutissant à la matrice céramique peut avoir lieu simultanément dans l’ensemble de l’ébauche déliantée. On peut réaliser un frittage sous contrainte durant le pressage à chaud, par exemple un frittage flash (également connu sous l’acronyme « SPS », de l’anglais « Spark Plasma Sintering »).The process continues with a hot pressing step (step E5) during which the debinded blank is compressed under temperature in order to reduce the porosity obtained at the end of the debinding. During hot pressing, the debinded blank is densified during which the porosity will gradually reduce and the blank will contract to reach the dimensions of the final part. During hot pressing, a temperature lower than the melting point of the reactive surface is imposed but sufficient to activate the chemical reaction in the solid state between the carbon present in the pulverulent composition and the silicon or the metallic element of the reactive surface of the second particles, so as to form the ceramic matrix. As indicated above, the reactive carbon can be provided by the first particles 10,100 and/or by the second particles 200 and/or by the third particles. It should be noted that in the event that a carbonaceous residue from pyrolysis of the binder remains after debinding, this residue can provide additional reactive carbon reacting with the silicon or the metallic element to participate in the formation of the ceramic matrix. The second particles can be homogeneously dispersed in the debinded parison undergoing the hot pressing. During hot pressing, the thermochemical reaction resulting in the ceramic matrix can take place simultaneously throughout the debinded blank. Sintering under stress can be carried out during hot pressing, for example flash sintering (also known by the acronym "SPS", from the English "Spark Plasma Sintering").
Au moins une dimension de l’ébauche déliantée peut être réduite d’au moins 10%, par exemple d’au moins 15%, durant le pressage à chaud. Au moins une dimension de l’ébauche déliantée peut être réduite d’une valeur comprise entre 15% et 25% durant le pressage à chaud. La compaction de l’ébauche déliantée est maintenue durant le pressage à chaud.At least one dimension of the debinded parison can be reduced by at least 10%, for example by at least 15%, during hot pressing. At least one dimension of the debinded blank can be reduced by a value between 15% and 25% during hot pressing. The compaction of the debinded blank is maintained during hot pressing.
La température imposée durant le pressage à chaud peut être comprise entre 1150°C et 1300°C et la pression imposée durant le pressage à chaud supérieure ou égale à 50 MPa, par exemple comprise entre 50 MPa et 75 MPa. La durée du pressage à chaud peut être supérieure ou égale à 1 minute, par exemple à 2 minutes.The temperature imposed during the hot pressing may be between 1150° C. and 1300° C. and the pressure imposed during the hot pressing greater than or equal to 50 MPa, for example between 50 MPa and 75 MPa. The duration of the hot pressing may be greater than or equal to 1 minute, for example 2 minutes.
On peut ensuite réaliser, si cela est souhaité, un usinage pour obtenir la forme définitive pour la pièce.It is then possible to carry out, if desired, machining to obtain the final shape for the part.
La pièce peut présenter une teneur volumique en renfort comprise entre 10% et 50%, par exemple comprise entre 20% et 40%, et une teneur volumique en matrice comprise entre 50% et 90%, par exemple entre 50% et 70%. Lorsque la surface réactive des deuxièmes particules comprend du silicium, le taux volumique de silicium libre dans la pièce peut être inférieur ou égal à 15%, par exemple inférieur ou égal à 5%.The part may have a reinforcement content by volume of between 10% and 50%, for example between 20% and 40%, and a matrix content by volume of between 50% and 90%, for example between 50% and 70%. When the reactive surface of the second particles comprises silicon, the volume content of free silicon in the part can be less than or equal to 15%, for example less than or equal to 5%.
Si cela est souhaité, on peut procéder à une finalisation de la densification après le pressage à chaud en introduisant une faible quantité de métal à l’état fondu par mise en œuvre d’une technique classique d’infiltration à l’état fondu.If desired, densification can be finalized after hot pressing by introducing a small amount of molten metal using a conventional molten infiltration technique.
La pièce obtenue peut être une pièce de turbomachine, par exemple une pièce de turbomachine aéronautique. La pièce peut être une pièce de turbine à gaz d’un moteur aéronautique ou d’une turbine industrielle. En particulier, la pièce peut constituer une partie au moins d’un distributeur, une paroi d’une chambre de combustion, un secteur d’anneau de turbine ou une aube de turbomachine.The part obtained can be a turbomachine part, for example an aeronautical turbomachine part. The part can be a gas turbine part of an aero engine or an industrial turbine. In particular, the part can constitute at least part of a distributor, a wall of a combustion chamber, a sector of a turbine ring or a turbine engine blade.
L’expression « comprise entre … et … » doit se comprendre comme incluant les bornes.The expression “between … and …” must be understood as including the limits.
Claims (12)
- le déliantage (E4) d’une ébauche de la pièce à obtenir comprenant un liant et une composition pulvérulente comprenant du carbone présente dans le liant, la composition pulvérulente comprenant :
(i) des premières particules (10 ; 100) de renfort, et
(ii) des deuxièmes particules (200), distinctes des premières particules, ayant une surface réactive (204) comprenant du silicium ou un élément métallique, et
- le pressage à chaud (E5) de l’ébauche déliantée durant lequel il y a réaction thermochimique à l’état solide entre le carbone de la composition pulvérulente et le silicium ou l’élément métallique de la surface réactive des deuxièmes particules afin de former la matrice céramique.Method for manufacturing a part made of composite material with a ceramic matrix, comprising at least:
- the debinding (E4) of a blank of the part to be obtained comprising a binder and a powder composition comprising carbon present in the binder, the powder composition comprising:
(i) first particles (10; 100) of reinforcement, and
(ii) second particles (200), distinct from the first particles, having a reactive surface (204) comprising silicon or a metallic element, and
- hot pressing (E5) of the debinded blank during which there is thermochemical reaction in the solid state between the carbon of the powdery composition and the silicon or the metallic element of the reactive surface of the second particles in order to form the ceramic matrix.
- les premières particules dans en une teneur volumique dans la composition pulvérulente comprise entre 10% et 50%, par exemple comprise entre 15% et 35%,
- les deuxièmes particules, seules ou en combinaison avec une charge inerte éventuellement présente, en une teneur volumique dans la composition pulvérulente comprise entre 50% et 90%, par exemple entre 65% et 85%, et
- éventuellement des troisièmes particules de carbone, distinctes des premières et deuxièmes particules, en une teneur volumique dans la composition pulvérulente comprise entre 1% et 10%.Process according to any one of Claims 1 to 11, in which the volume content of powder composition in the parison is between 45% and 85% and the volume content of binder in the parison is between 15% and 55% , and the powder composition comprises:
- the first particles in a content by volume in the pulverulent composition of between 10% and 50%, for example between 15% and 35%,
- the second particles, alone or in combination with an inert filler optionally present, in a content by volume in the pulverulent composition of between 50% and 90%, for example between 65% and 85%, and
- optionally third carbon particles, distinct from the first and second particles, in a content by volume in the pulverulent composition of between 1% and 10%.
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FR2010979A FR3115533B1 (en) | 2020-10-27 | 2020-10-27 | Process for manufacturing a composite material part |
PCT/FR2021/051865 WO2022090655A1 (en) | 2020-10-27 | 2021-10-22 | Method for manufacturing a part made from a ceramic matrix composite material |
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WO2024084155A1 (en) * | 2022-10-21 | 2024-04-25 | Safran Ceramics | Infiltration of a fibrous structure comprising a liquid silicon reactive layer |
WO2024084161A1 (en) * | 2022-10-21 | 2024-04-25 | Safran Ceramics | Process for manufacturing part made of a composite material having a ceramic matrix |
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FR3130274A1 (en) * | 2021-12-13 | 2023-06-16 | Safran Ceramics | Process for manufacturing a composite material part with reduced residual porosity |
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US5043118A (en) * | 1989-12-18 | 1991-08-27 | Hoechst Celanese Corp. | Whisker-reinforced ceramic matrix composite by injection molding |
US6024909A (en) * | 1993-08-12 | 2000-02-15 | Agency Of Industrial Science & Technology | Coated ceramic particles, a ceramic-base sinter and a process for producing the same |
US20070158150A1 (en) * | 2005-11-05 | 2007-07-12 | Audi Ag | Brake disk with intermediate layer |
WO2019122758A1 (en) * | 2017-12-22 | 2019-06-27 | Safran Ceramics | Method for manufacturing a ceramic matrix composite part |
US20200071236A1 (en) * | 2017-05-15 | 2020-03-05 | Kyoto University | Silicon carbide ceramic |
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- 2020-10-27 FR FR2010979A patent/FR3115533B1/en active Active
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US5043118A (en) * | 1989-12-18 | 1991-08-27 | Hoechst Celanese Corp. | Whisker-reinforced ceramic matrix composite by injection molding |
US6024909A (en) * | 1993-08-12 | 2000-02-15 | Agency Of Industrial Science & Technology | Coated ceramic particles, a ceramic-base sinter and a process for producing the same |
US20070158150A1 (en) * | 2005-11-05 | 2007-07-12 | Audi Ag | Brake disk with intermediate layer |
US20200071236A1 (en) * | 2017-05-15 | 2020-03-05 | Kyoto University | Silicon carbide ceramic |
WO2019122758A1 (en) * | 2017-12-22 | 2019-06-27 | Safran Ceramics | Method for manufacturing a ceramic matrix composite part |
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WO2024084155A1 (en) * | 2022-10-21 | 2024-04-25 | Safran Ceramics | Infiltration of a fibrous structure comprising a liquid silicon reactive layer |
WO2024084161A1 (en) * | 2022-10-21 | 2024-04-25 | Safran Ceramics | Process for manufacturing part made of a composite material having a ceramic matrix |
FR3141169A1 (en) * | 2022-10-21 | 2024-04-26 | Safran Ceramics | Process for manufacturing a part made of ceramic matrix composite material |
FR3141165A1 (en) * | 2022-10-21 | 2024-04-26 | Safran Ceramics | Infiltration of a fibrous structure comprising a layer reactive to liquid silicon. |
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