FR2664518A1 - Brazing composition for thermostructural composite materials and ceramic materials, and process for making it - Google Patents

Brazing composition for thermostructural composite materials and ceramic materials, and process for making it Download PDF

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Publication number
FR2664518A1
FR2664518A1 FR9008901A FR9008901A FR2664518A1 FR 2664518 A1 FR2664518 A1 FR 2664518A1 FR 9008901 A FR9008901 A FR 9008901A FR 9008901 A FR9008901 A FR 9008901A FR 2664518 A1 FR2664518 A1 FR 2664518A1
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Prior art keywords
brazing
resin
brazing composition
weight
materials
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FR9008901A
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French (fr)
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FR2664518B1 (en
Inventor
Ciais Jean-Pierre
Gramond Jean-Marie
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Societe Europeenne de Propulsion SEP SA
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Societe Europeenne de Propulsion SEP SA
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Priority to FR9008901A priority Critical patent/FR2664518B1/en
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Publication of FR2664518B1 publication Critical patent/FR2664518B1/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244Powders, particles or spheres; Preforms made therefrom
    • B23K35/025Pastes, creams, slurries
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/30Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3033Ni as the principal constituent

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Products (AREA)

Abstract

The brazing composition, which can be in the form of a powder with resin added in order to form a paste, comprises: 83 to 85% by weight of nickel, 14 to 17% by weight of titanium, 0 to 5% by weight of copper, and 0 to 5% by weight of silicon. th

Description

Composition de brasage pour matériaux céramiques et matériaux composites thermostructuraux et procédé pour sa mise en oeuvre.Brazing composition for ceramic materials and thermostructural composite materials and process for its implementation.

La présente invention concerne le brasage de matériaux céramiques et de matériaux composites thermostructuraux. The present invention relates to the brazing of ceramic materials and thermostructural composite materials.

Les matériaux composites thermostructuraux sont des matériaux composites qui présentent des propriétés mécaniques les rendant aptes à la réalisation d'éléments de structures, et qui conservent ces propriétés à des températures élevées. Des exemples typiques de matériaux composites thermostructuraux sont les carbone-carbone (C/C), constitués d'un renfort à base de fibres de carbone densifié par une matrice en carbone, et les composites à matrice céramique tCMC), constitués d'un renfort à base de fibres réfractaires (fibres en carbone ou fibre en céramique, par exemple) densifié par une matrice céramique. Un matériau céramique fréquemment utilisé pour la matrice et, le cas échéant, les fibres du renfort, est le carbure de silicium. Thermostructural composite materials are composite materials which have mechanical properties making them suitable for the production of structural elements, and which retain these properties at high temperatures. Typical examples of thermostructural composite materials are carbon-carbon (C / C), consisting of a reinforcement based on carbon fibers densified by a carbon matrix, and composites with a ceramic matrix tCMC), consisting of a reinforcement based on refractory fibers (carbon fibers or ceramic fibers, for example) densified by a ceramic matrix. A ceramic material frequently used for the matrix and, where appropriate, the fibers of the reinforcement, is silicon carbide.

La présente invention a notamment pour but de fournir une composition permettant une liaison par brasage entre des pièces en matériaux céramiques ou entre des pièces en matériaux composites thermostructuraux, ou encore entre une pièce en matériau céramique et une pièce en matériau composite thermostructural. The object of the present invention is in particular to provide a composition allowing a connection by brazing between parts made of ceramic materials or between parts made of thermostructural composite materials, or even between a part made of ceramic material and a part made of thermostructural composite material.

En particulier, la présente invention vise à fournir une composition de brasage qui autorise une température de service élevée pour la liaison brasée, ainsi que l'application de traitements particuliers à température élevée postérieurement au brasage. In particular, the present invention aims to provide a brazing composition which allows a high operating temperature for the brazed connection, as well as the application of specific treatments at high temperature after brazing.

Par température élevée, on entend ici une température supérieure à 1 0000C. Or, les compositions de brasage connues, utilisées en particulier pour le brasage de céramique sur un métal, sont mises en oeuvre à des températures qui n'excèdent pas 600 à 7500C.By high temperature is meant here a temperature higher than 1 0000C. However, known brazing compositions, used in particular for brazing ceramic on a metal, are used at temperatures which do not exceed 600 to 7500C.

La présente invention a encore pour but de fournir une composition de brasage avec laquelle, dans le cas de composites thermostructuraux, le brasage peut être effectué sans dégradation des caractéristiques des fibres constitutives du renfort du matériau composite.  Another object of the present invention is to provide a brazing composition with which, in the case of thermostructural composites, brazing can be carried out without degrading the characteristics of the fibers constituting the reinforcement of the composite material.

Conformément à l'invention, une composition de brasage pour matériaux céramiques ou matériaux composites thermostructuraux comprend : 83 à 85 % en poids de nickel, 14 à 17 % en poids de titane, 0 à 5 % en poids de cuivre, et 0 à 5 % en poids de silicium. According to the invention, a brazing composition for ceramic materials or thermostructural composite materials comprises: 83 to 85% by weight of nickel, 14 to 17% by weight of titanium, 0 to 5% by weight of copper, and 0 to 5 % by weight of silicon.

La composition de brasage peut se présenter sous forme de fil, de feuillard ou de pâte. The brazing composition can be in the form of wire, strip or paste.

En particulier, la composition de brasage peut être sous forme d'une poudre additionnée d'une résine pour constituer une pâte, éventuellement diluée par un solvant de la résine. In particular, the brazing composition may be in the form of a powder added with a resin to form a paste, optionally diluted with a solvent for the resin.

La résine peut être une résine fugitive, c'est-à-dire une résine ne laissant pas de résidu solide après carbonisation. La carbonisation de la résine a lieu à une température inférieure à celle à laquelle le brasage est effectué. The resin may be a fugitive resin, that is to say a resin which does not leave a solid residue after carbonization. The carbonization of the resin takes place at a temperature lower than that at which the soldering is carried out.

La résine peut aussi être choisie parmi des résines laissant, après carbonisation, des résidus réfractaires constituant des éléments additionnels ajoutés à la brasure. Ces éléments additionnels peuvent être constitués de carbone ou de céramique. The resin can also be chosen from resins leaving, after carbonization, refractory residues constituting additional elements added to the solder. These additional elements can consist of carbon or ceramic.

Des exemples de telles résines sont les polycarbosilanes donnant un résidu en carbure de silicium et les polytitanocarbosilanes.Examples of such resins are polycarbosilanes giving a residue in silicon carbide and polytitanocarbosilanes.

L'invention vise aussi à fournir un procédé de mise en oeuvre de la composition de brasage définie plus haut. The invention also aims to provide a method of using the brazing composition defined above.

Conformément à l'invention, le brasage est effectué sous -2 2 -4 une pression inférieure à 1,5.10 N/m (environ 10 Torr), à une température comprise entre 1 3000C et 1 4000C pendant au moins 15 min. In accordance with the invention, brazing is carried out at -2 2 -4 at a pressure of less than 1.5 × 10 N / m (approximately 10 Torr), at a temperature between 1300C and 14000C for at least 15 min.

Dans le cas où la composition de brasage est sous forme d'une poudre additionnée de résine, Le procédé de brasage comprend en outre un palier à une température suffisante pour carboniser la résine, généralement à environ 9000C, avant le brasage proprement dit. In the case where the brazing composition is in the form of a powder added with resin, the brazing method further comprises a bearing at a temperature sufficient to carbonize the resin, generally at around 9000C, before the actual brazing.

Un exemple de mise en oeuvre d'une composition de brasage conforme à l'invention sera maintenant décrit, à titre indicatif mais non limitatif, en référence à la figure unique annexée.  An example of implementation of a brazing composition in accordance with the invention will now be described, by way of indication but not limitation, with reference to the single appended figure.

Sur cette figure, la référence 1 désigne une pièce cylindrique en matériau composite SiC/SiC (renfort à base de fibres en carbure de silicium et matrice en carbure de silicium) destinée à être brasée dans un trou d'un substrat 2 de même nature. In this figure, the reference 1 designates a cylindrical part made of SiC / SiC composite material (reinforcement based on silicon carbide fibers and matrix in silicon carbide) intended to be brazed in a hole in a substrate 2 of the same kind.

Le brasage est réalisé au moyen d'une pâte 3 déposée entre les pièces 1 et 2 en couche uniforme d'épaisseur égale à environ 0,1 mm (plues une réserve dans l'angle 5). La pâte 3 est constituée d'un mélange de poudres de nickel et de titane de granulométrie inférieure à 0,1 mm additionne d'une résine, la préparation de la pâte étant effectuée sous vide. Dans le mélange de poudres métalliques, le nickel représente 83 % en poids et Le titane 17 % en poids. La résine est ajoutée au mélange de poudres métalliques en quantité représentant environ 20 % en masse de celui-ci. La résine est constituée par exemple de 50 % en masse de polytitanocarbosilane et 50 % en masse de xyLène.  The brazing is carried out by means of a paste 3 deposited between the parts 1 and 2 in a uniform layer of thickness equal to approximately 0.1 mm (greater a reserve in the angle 5). The paste 3 consists of a mixture of nickel and titanium powders with a particle size of less than 0.1 mm, added with a resin, the preparation of the paste being carried out under vacuum. In the mixture of metallic powders, nickel represents 83% by weight and titanium 17% by weight. The resin is added to the mixture of metal powders in an amount representing approximately 20% by mass thereof. The resin consists for example of 50% by mass of polytitanocarbosilane and 50% by mass of xyLene.

Le brasage est effectué dans un four sous vide (pression de 5.10 5 Torr soit environ 7,5.10 N/m2), la pièce 1 étant maintenue en place par une masselotte 4 en molybdène. Le brasage comprend une première phase de montée lente en température jusqu'à 3000C suivie d'un maintien à cette température pendant 1 h, une deuxième phase de montée lente jusqu'à 700 0C suivie d'un maintien à cette température pendant 1 h, une troisième phase de montée rapide en température jusqu'à 1 4000C suivie d'un maintien à cette température pendant 15 min, une première phase de refroidissement lent jusqu a 300 0C (refroidissement naturel du four), et une deuxième phase de refroidissement rapide sous balayage d'azote jusqu'à la température ambiante. Brazing is carried out in a vacuum oven (pressure of 5.10 5 Torr or about 7.5.10 N / m2), the part 1 being held in place by a molybdenum counterweight 4. Brazing comprises a first phase of slow rise in temperature to 3000C followed by a maintenance at this temperature for 1 h, a second phase of slow rise to 700 0C followed by a maintenance at this temperature for 1 h, a third phase of rapid temperature rise to 1 4000C followed by maintaining at this temperature for 15 min, a first phase of slow cooling to 300 0C (natural cooling of the oven), and a second phase of rapid cooling under nitrogen sweep to room temperature.

Le brasage proprement dit avec fusion du mélange de poudres métalliques a lieu lorsque la température dépasse environ 1 3000C.  The actual brazing with melting of the mixture of metal powders takes place when the temperature exceeds about 1300C.

Claims (6)

REVENDICATIONS 1. Composition de brasage pour matériaux céramiques et matériaux composites thermostructuraux, caractérisée en ce qu'elle comprend 83 à 85 % en poids de nickel, 14 à 17 % en poids de titane, 0 à 5 % en poids de cuivre, et 0 à 5 % en poids de silicium.1. Brazing composition for ceramic materials and thermostructural composite materials, characterized in that it comprises 83 to 85% by weight of nickel, 14 to 17% by weight of titanium, 0 to 5% by weight of copper, and 0 to 5% by weight of silicon. 2. Composition de brasage selon la revendication 1, caractérisée en ce qu'elle est sous forme d'une poudre additionnée de résine pour constituer une pâte.2. Brazing composition according to claim 1, characterized in that it is in the form of a powder added with resin to form a paste. 3. Composition de brasage selon la revendication 2, caractérisée en ce que la résine est une résine fugitive. 3. Brazing composition according to claim 2, characterized in that the resin is a fugitive resin. 4. Composition de brasage selon la revendication 2, caractérisée en ce que la résine est une résine laissant un résidu réfractaire après carbonisation.4. Brazing composition according to claim 2, characterized in that the resin is a resin leaving a refractory residue after carbonization. 5. Procédé de brasage de matériaux céramiques ou de matériaux composites thermostructuraux au moyen d'une composition de brasage selon L'une quelconque des revendications 1 à 4, caractérisé en ce que Le brasage est effectué sous une pression inférieure à 1,5.10 2 N/m2, à une température comprise entre 1 300 et 1 4000C et pendant au moins 15 min5. A method of brazing ceramic materials or thermostructural composite materials using a brazing composition according to any one of claims 1 to 4, characterized in that the brazing is carried out under a pressure of less than 1.5.10 2 N / m2, at a temperature between 1 300 and 1 4000C and for at least 15 min 6. Procédé de brasage selon la revendication 5, utilisant une composition de brasage selon L'une quelconque des revendications 3 et 4, caractérisé en ce qu'il comprend une étape de carbonisation de la résine avant le brasage proprement dit. 6. A brazing method according to claim 5, using a brazing composition according to any one of claims 3 and 4, characterized in that it comprises a step of carbonization of the resin before the actual brazing.
FR9008901A 1990-07-12 1990-07-12 BRAZING COMPOSITION FOR CERAMIC MATERIALS AND THERMOSTRUCTURAL COMPOSITE MATERIALS AND METHOD FOR ITS IMPLEMENTATION. Expired - Fee Related FR2664518B1 (en)

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FR9008901A FR2664518B1 (en) 1990-07-12 1990-07-12 BRAZING COMPOSITION FOR CERAMIC MATERIALS AND THERMOSTRUCTURAL COMPOSITE MATERIALS AND METHOD FOR ITS IMPLEMENTATION.

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FR9008901A FR2664518B1 (en) 1990-07-12 1990-07-12 BRAZING COMPOSITION FOR CERAMIC MATERIALS AND THERMOSTRUCTURAL COMPOSITE MATERIALS AND METHOD FOR ITS IMPLEMENTATION.

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FR2664518B1 FR2664518B1 (en) 1995-02-17

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2979573A1 (en) * 2011-09-07 2013-03-08 Snecma PROCESS FOR MANUFACTURING TURBINE DISPENSER SECTOR OR COMPRESSOR RECTIFIER OF COMPOSITE MATERIAL FOR TURBOMACHINE AND TURBINE OR COMPRESSOR INCORPORATING A DISPENSER OR RECTIFIER FORMED OF SUCH SECTORS
WO2013034837A1 (en) 2011-09-07 2013-03-14 Snecma Assembly consisting of a turbine nozzle or a compressor stator vane made of cmc for a turbine engine and an abradable support ring, and turbine or compressor including such an assembly
WO2013060977A2 (en) 2011-10-25 2013-05-02 Herakles Method for manufacturing a turbine nozzle guide vanes sector or a compressor guide vanes sector in composite material for a turbomachine and turbine or compressor incorporating turbine nozzle guide vanes or compressor guide vanes formed of such sectors
US9033673B2 (en) 2010-06-28 2015-05-19 Herakles Turbomachine blade or vane having complementary asymmetrical geometry
US9045992B2 (en) 2010-06-28 2015-06-02 Herakles Turbomachine blades or vanes having complementary even/odd geometry
US9062562B2 (en) 2008-11-28 2015-06-23 Herakles Composite material turbomachine engine blade or vane, compressor stator segment or turbine nozzle segment incorporating such vanes and method for manufacturing same
US9506355B2 (en) 2009-12-14 2016-11-29 Snecma Turbine engine blade or vane made of composite material, turbine nozzle or compressor stator incorporating such vanes and method of fabricating same

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1086609A (en) * 1952-11-05 1955-02-15 Ericsson Telefon Ab L M Brazing process
US2844867A (en) * 1955-06-24 1958-07-29 Martin Co Dip brazing
US2847302A (en) * 1953-03-04 1958-08-12 Roger A Long Alloys for bonding titanium base metals to metals
FR1400348A (en) * 1964-07-09 1965-05-21 Thomson Houston Comp Francaise Improvements to alloys for the production of watertight seals
US3428450A (en) * 1965-05-12 1969-02-18 Mallory & Co Inc P R Alloys for brazing silicon nitride material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1086609A (en) * 1952-11-05 1955-02-15 Ericsson Telefon Ab L M Brazing process
US2847302A (en) * 1953-03-04 1958-08-12 Roger A Long Alloys for bonding titanium base metals to metals
US2844867A (en) * 1955-06-24 1958-07-29 Martin Co Dip brazing
FR1400348A (en) * 1964-07-09 1965-05-21 Thomson Houston Comp Francaise Improvements to alloys for the production of watertight seals
US3428450A (en) * 1965-05-12 1969-02-18 Mallory & Co Inc P R Alloys for brazing silicon nitride material

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9062562B2 (en) 2008-11-28 2015-06-23 Herakles Composite material turbomachine engine blade or vane, compressor stator segment or turbine nozzle segment incorporating such vanes and method for manufacturing same
US9506355B2 (en) 2009-12-14 2016-11-29 Snecma Turbine engine blade or vane made of composite material, turbine nozzle or compressor stator incorporating such vanes and method of fabricating same
US9033673B2 (en) 2010-06-28 2015-05-19 Herakles Turbomachine blade or vane having complementary asymmetrical geometry
US9045992B2 (en) 2010-06-28 2015-06-02 Herakles Turbomachine blades or vanes having complementary even/odd geometry
FR2979573A1 (en) * 2011-09-07 2013-03-08 Snecma PROCESS FOR MANUFACTURING TURBINE DISPENSER SECTOR OR COMPRESSOR RECTIFIER OF COMPOSITE MATERIAL FOR TURBOMACHINE AND TURBINE OR COMPRESSOR INCORPORATING A DISPENSER OR RECTIFIER FORMED OF SUCH SECTORS
WO2013034857A2 (en) 2011-09-07 2013-03-14 Snecma Method for manufacturing a sector of a turbine nozzle or compressor stator vane made of a composite material for a turbine engine, and turbine or compressor including a nozzle or stator vane consisting of said sectors
WO2013034837A1 (en) 2011-09-07 2013-03-14 Snecma Assembly consisting of a turbine nozzle or a compressor stator vane made of cmc for a turbine engine and an abradable support ring, and turbine or compressor including such an assembly
WO2013034857A3 (en) * 2011-09-07 2013-10-24 Snecma Method for manufacturing a sector of a turbine nozzle or compressor stator vane made of a composite material for a turbine engine, and turbine or compressor including a nozzle or stator vane consisting of said sectors
WO2013060977A2 (en) 2011-10-25 2013-05-02 Herakles Method for manufacturing a turbine nozzle guide vanes sector or a compressor guide vanes sector in composite material for a turbomachine and turbine or compressor incorporating turbine nozzle guide vanes or compressor guide vanes formed of such sectors
US9784113B2 (en) 2011-10-25 2017-10-10 Herakles Method of fabricating a turbine or compressor guide vane sector made of composite material for a turbine engine, and a turbine or a compressor incorporating such guide vane sectors

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