EP3823945A1 - Verfahren zum hybriden zusammenbau von teilen aus keramik oder einem keramikmatrixverbundstoff mithilfe eines abgabematerials, das abgeschieden und dann ohne totalverschmelzung dieses abgabematerials erhitzt wird - Google Patents

Verfahren zum hybriden zusammenbau von teilen aus keramik oder einem keramikmatrixverbundstoff mithilfe eines abgabematerials, das abgeschieden und dann ohne totalverschmelzung dieses abgabematerials erhitzt wird

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Publication number
EP3823945A1
EP3823945A1 EP19753175.9A EP19753175A EP3823945A1 EP 3823945 A1 EP3823945 A1 EP 3823945A1 EP 19753175 A EP19753175 A EP 19753175A EP 3823945 A1 EP3823945 A1 EP 3823945A1
Authority
EP
European Patent Office
Prior art keywords
filler material
temperature
assembly
alloy
parts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19753175.9A
Other languages
English (en)
French (fr)
Inventor
Valérie CHAUMAT
Valérie MERVEILLEAU
Frédéric Sanchette
Marc Ferrato
Nadine LASCASSIES
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Universite de Technologie de Troyes
Mersten Boostec SA
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Original Assignee
Commissariat a lEnergie Atomique CEA
Universite de Technologie de Troyes
Mersten Boostec SA
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Commissariat a lEnergie Atomique CEA, Universite de Technologie de Troyes, Mersten Boostec SA, Commissariat a lEnergie Atomique et aux Energies Alternatives CEA filed Critical Commissariat a lEnergie Atomique CEA
Publication of EP3823945A1 publication Critical patent/EP3823945A1/de
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/006—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of metals or metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/008—Soldering within a furnace
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
    • B23K20/023—Thermo-compression bonding
    • B23K20/026—Thermo-compression bonding with diffusion of soldering material
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/005—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of glass or ceramic material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
    • B23K2103/52—Ceramics
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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    • C04B2235/963—Surface properties, e.g. surface roughness
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    • C04B2237/128—The active component for bonding being silicon
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    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium

Definitions

  • the present invention relates to a method of hybrid assembly of at least two parts made of ceramic-based materials or ceramic matrix composite by means of a heated filler material without total melting of this material. bring.
  • Brazing consists in positioning a filler material, also called brazing alloy or brazing, between the parts to be assembled or near and to melt it completely so that it fills the clearance between the parts and creates, at cooling, a joint between the parts. After cooling, the parts are thus assembled by a solder joint.
  • the filler material has a lower melting temperature than that of the materials to be assembled, so there is no melting of the parts to be assembled during the brazing process.
  • brazings comprising from 40 to 97 atomic% of silicon and from 60 to 3% of another metallic element.
  • these silicon-rich solders can also comprise from 15 to 19 atomic% of Pr (document FR-A-2 907 448-B1), from 30 to 44 atomic% Y (document FR-A- 2 936 176 ), or from 1 to 54% Nd (document FR-A-2 949 696), or be TiSi 2 (Elodie Jacques thesis, 2012, “Assembly of thin SiC / SiC composites: search for a composition of joint and an associated process ”).
  • the brazing alloys are systematically completely melted. To obtain parts with good mechanical strength and having a satisfactory seal on either side of the joint, the assembly process must satisfy several criteria:
  • the filler material can be non-reactive with the ceramic, that is to say that there is no reaction layer with formation of new compounds at the interface, but there is strong direct interactions between the filler material and the ceramic.
  • the material can also have limited and controlled reactivity (formation of compounds at the interface which do not damage the bond). It must not lead to an uncontrolled exacerbated reaction with embrittlement of the filler material / ceramic interface and possibly of the ceramic.
  • the filler material must cover the faces to be assembled well with the ceramic after the deposition and heat treatment steps.
  • the filler material must be placed correctly on the faces to be assembled after deposition and must not leave these areas during the heat treatment.
  • the filler material In the case of porous ceramics, such as composites, the filler material must not infiltrate the porous ceramic or very slightly so that the filler material remains positioned in the joint.
  • an object of the present invention to provide a method of assembling at least two pieces of ceramic-based material, making it possible to:
  • step c) bringing the filler material into contact with the two parts, d) heating the assembly obtained in step c), to an assembly temperature, and the assembly temperature being maintained for a period holding, e) Cooling of the assembly so as to form a joint between the two parts, and to assemble the two parts,
  • the assembly temperature being lower than the temperature at which the filler material is completely melted.
  • the assembly temperature is lower than the melting temperature of the filler material. By lower, we mean that it is strictly lower.
  • melting point is meant a temperature at which all of the filler material is in the liquid state. In the case of an alloy, it is the liquidus temperature. In the particular case of a eutectic alloy, it is the temperature of the eutectic. In the case of an alloy offset from the eutectic, that is to say a hyper eutectic or hypo eutectic alloy, it is the temperature of the liquidus. In the particular case of a defined compound with congruent fusion, this is the melting point.
  • ceramic defined broadly includes non-metallic inorganic solids.
  • ceramic a material obtained by sintering non-metallic inorganic powders (for example carbides, silicides, oxides, nitrides).
  • ceramic matrix composites also means a material formed from the association of a ceramic fiber (for example alumina fiber, silicon carbide fiber, carbon fiber) embedded in a ceramic matrix produced by liquid or gas route. .
  • the invention differs fundamentally from the prior art in that the filler material, during the hybrid assembly, is not completely melted. It is either partially melted (that is to say in a semi-solid state) or not melted (that is to say in the solid state).
  • a material which is not completely melted is a material which has a mixed liquid / solid phase (also called semi-solid state), particularly in majority in solid phase, even more particularly a mixed phase for which the mass percentage of liquid is less than 10%, preferably less than 5%.
  • a mixed liquid / solid phase also called semi-solid state
  • different compositions of filler material can be used, which makes it possible to use a wide choice of compositions depending on the intended application.
  • the hybrid assembly method according to the invention allows, firstly, to coat in a controlled and controlled manner the areas to be assembled with the filler material, then to assemble the coated parts, in particular avoiding the problems associated at wetting, at the formation of fillets, or at the leaks of the filler material outside the areas to be assembled.
  • the filler material is either solid or semi-solid. This coating can also be architectured.
  • Maintaining the filler material in its deposition zone is easier in solid or semi-solid phase than with total melting as implemented in brazing. The fact of not melting the filler material or only partially promotes the retention of the filler material in the joint.
  • the method according to the invention ensures good mechanical strength of the joints formed.
  • the strength of the joint, for the same given filler material is at least equal to, or even better than, that of a traditional brazing process (implementing the total melting of the filler material or of the solder).
  • the process according to the invention is a hybrid assembly process, not reactive or with limited and controlled reactivity, leading to the formation of a refractory or moderately refractory joint, depending on the nature of the filler material.
  • refractory is meant that the seal has good resistance to the effects induced by high temperatures (satisfactory mechanical properties at least up to 1000 ° C, even 1600 ° C).
  • moderately refractory is meant that the seal has good resistance to the effects induced by medium temperatures up to 600 ° C., or even 800 ° C.
  • Parts of large dimensions and / or complex shapes can thus be assembled.
  • the filler material is an alloy, and the assembly temperature is lower than the temperature of the solidus of the filler material.
  • the filler material is an alloy and the assembly temperature is between the solidus and liquidus temperatures of the filler material.
  • the ceramic-based materials are chosen from non-oxidized ceramics such as silicon carbide, silicon nitride, and aluminum nitride, oxide ceramics such as alumina, sapphire, mullite and zirconia, composites with non-oxide ceramic matrices (for example SiC / SiC composites with SiC matrix and SiC fibers, C / SiC composites, C / C composites) and composites with oxide ceramic matrices (for example matrix composites alumina and alumina fibers).
  • the method makes it possible to assemble ceramic, oxide or non-oxide, porous or non-porous, composite or non-composite parts, with or without a prior sealing coating for porous ceramics. In particular, this method prevents the filler material from migrating into the porosities of the porous parts to be assembled to the detriment of the formation of the joint.
  • step b) is carried out by depositing the filler material by the dry route on at least one of the two parts, and preferably on the two parts to be assembled.
  • the filler material is deposited by thermal spraying.
  • the thickness of the deposited filler material can range from 100 ⁇ m to 500 ⁇ m, preferably from 100 ⁇ m to 300 ⁇ m.
  • the process allows very thick joints to be produced while ensuring a good distribution of the phases of the filler material, which is not observed with the traditional brazing process.
  • thick joint is meant a joint whose thickness is greater than 100 ⁇ m.
  • the method comprises a step, between step b) and step c), in which the deposited filler material is rectified or polished.
  • the filler material is deposited by physical vapor deposition.
  • the thickness of the deposited filler material can range from lpm to 20pm.
  • the filler material is deposited by thermal chemical vapor deposition (CVD) or assisted by plasma.
  • step c pressure is applied when the filler material is brought into contact with the two parts.
  • step d) is carried out under vacuum, under neutral gas or under air.
  • the filler material comprises at least 40 atomic% of silicon.
  • the filler material can comprise at least 99 atomic% of silicon.
  • the filler material is solid or partially molten, which makes it possible to use almost pure silicon (at least 99 atomic% of silicon) or pure (100 atomic% of silicon).
  • the process is carried out in solid phase below the melting point of silicon.
  • the filler material can comprise from 40% to 97 atomic% of silicon and an additional element.
  • the additional element is metallic.
  • the additional element is chosen from the following elements Ag, Ge, Cr, Co, Ce, Cu, Hf, Ti, V, Zr, Nd, Pr, Ru, Rh, Re, Y, I r, Ni, Pt , Pd, Mo, and W.
  • Many compositions of filler material can be used.
  • a composition will be chosen with a limited number of elements (preferably two, possibly three), if possible without expensive elements to facilitate its preparation and implementation, and / or reduce the preparation costs.
  • the filler material (30) is an alloy of silicon and cobalt which comprises from 58% to 97 atomic% in silicon and from 42% to 3 atomic% in cobalt.
  • the assembly temperature is a temperature between 1100 ° C and 1350 ° C, in particular the assembly temperature is chosen either so that the alloy remains at the solid state, so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and zirconium which comprises 60% to 97 atomic% of silicon and 40% to 3 atomic% of zirconium.
  • the assembly temperature is a temperature between 1100 ° C and 1600 ° C, preferably 1200 to 1550 ° C, in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and chromium which comprises 50% to 97 atomic% of silicon and 50% to 3 atomic% of chromium.
  • the assembly temperature is a temperature between 1100 ° C and 1420 ° C, preferably between 1200 ° C and 1420 ° C, in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and cerium which comprises 53% to 97 atomic% of silicon and 47% to 3 atomic% of cerium.
  • the assembly temperature is a temperature between 1100 ° C and 1550 ° C, in particular the assembly temperature is chosen either so that the alloy remains at the solid state, so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and hafnium which comprises 66% to 97 atomic% of silicon and 44% to 3 atomic% of hafnium.
  • the assembly temperature is a temperature between 1100 ° C and 1500 ° C, preferably between 1200 ° C and 1500 ° C, in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and titanium which comprises 60% to 97 atomic% of silicon and 40% to 3 atomic% of titanium.
  • the assembly temperature is a temperature between 1100 ° C and 1450 ° C, preferably between 1200 ° C and 1420 ° C, in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and vanadium which comprises 55% to 97 atomic% of silicon and 45% to 3 atomic% of vanadium.
  • the assembly temperature is a temperature between 1100 ° C and 1600 ° C, preferably between 1200 ° C and 1550 ° C, in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and neodymium which comprises 56% to 97 atomic% of silicon and 44% to 3 atomic% of neodymium.
  • the assembly temperature is a temperature between 1100 ° C. and 1600 ° C., in particular the assembly temperature is chosen either so that the alloy remains at the solid state, so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and praseodymium which comprises 58% to 97 atomic% of silicon and 42% to 3 atomic% of praseodymium.
  • the assembly temperature is a temperature between 1100 ° C. and 1600 ° C., in particular the assembly temperature is chosen either so that the alloy remains at the solid state, so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and rhenium which comprises 40% to 97 atomic% of silicon and 60% to 3 atomic% of rhenium.
  • the assembly temperature is a temperature between 1100 ° C and 1600 ° C, preferably between 1200 ° C and 1600 ° C in particular the assembly temperature is chosen either so that the alloy remains in the solid state, or so that the alloy is in a semi-solid state.
  • the filler material comprises an alloy of silicon and ytrium which comprises 40% to 97 atomic% of silicon and 60% to 3 atomic% of ytrium.
  • the assembly temperature is a temperature between 1100 ° C. and 1600 ° C., in particular the assembly temperature is chosen either so that the alloy remains at the solid state, so that the alloy is in a semi-solid state.
  • the filler material is a silver-based alloy, such as AgZr, or silver-copper based, such as AgCuTi. This material will preferably be deposited so as to favor the presence of Ti or Zr close to the ceramic.
  • FIG. 1 is a diagrammatic representation, in section and in profile, of two parts to be assembled and of a filler material, in a “sandwich” configuration, according to a particular embodiment of the invention
  • FIG. 2 represents a photograph obtained under an optical microscope of the surface of a solder deposited by thermal spraying on a part to be assembled, according to a particular embodiment of the invention
  • FIG. 3 represents the microstructure of a joint obtained from a CoSi solder deposited by thermal spraying on a part to be assembled, according to a particular embodiment of the method of the invention
  • FIGS. 4A and 4B represent the microstructure of a joint obtained after partial melting of a CoSi solder used to assemble SiC parts, according to a particular embodiment of the method of the invention, at different magnifications,
  • FIG. 5 represents a photographic photograph of two SiC plates on which a CoSi alloy has been deposited by thermal projection, according to a particular embodiment of the invention
  • FIG. 6 shows a photographic snapshot of 4-point bent SiC machined test pieces, the solder joint being obtained from a CoSi alloy, according to a particular embodiment of the invention
  • FIG. 7 shows a photographic snapshot of two parts of a model, called bursting model, the parts being intended to be assembled according to a particular embodiment of the present invention in order to conduct a test, called bursting test ;
  • FIG. 8 shows a photographic snapshot of the parts of Figure 7 assembled according to a particular embodiment of the present invention.
  • the hybrid assembly method according to the invention comprises the following successive steps:
  • the assembly temperature being lower than the temperature at which the filler material is completely melted.
  • the method can include a surface step b1) executed between steps b) and c).
  • step b1) is in particular intended to make on the surface of the layer formed by the filler material 30 compatible with the contacting (assembly) of step c). More particularly, step b1) can be intended to reduce the roughness of the surface of the layer formed by the filler material 30.
  • the method makes it possible to assemble at least two parts 10, 20. It can make it possible to assemble more parts, for example, three or four parts. We can, for example, assemble a larger number of parts of up to 100.
  • the parts 10, 20 supplied in step a) can be of any shape.
  • the faces to be assembled can be flat or have reliefs.
  • parts 10, 20 will be chosen whose faces 11, 21 to be assembled are flat to facilitate assembly (FIG. 1).
  • the parts to be assembled are preferably of monolithic structure. These are rigid parts.
  • the pieces have, for example, large dimensions and / or are of complex shapes.
  • the parts 10, 20 to be assembled can be porous.
  • the parts 10, 20 to be assembled are made of a ceramic-based material. They can be of the same material or of different materials.
  • ceramic-based material any material whose ceramic content is greater than 80% by weight and preferably greater than 90% by weight.
  • Ceramics is, for example, chosen from:
  • non-oxidized ceramics such as silicon carbide, silicon nitride SÎ3N 4 and aluminum nitride AIN,
  • - oxide ceramics for example alumina (AI2O3), silica, aluminosilicate, such as mullite (defined compound of formula 3AI2O3, 2SÎ0 2 which can be obtained by heating silica in the presence of alumina) and cordierite, zirconia ZrO2,
  • oxide ceramic matrices oxide matrix / oxide fiber for example
  • non-oxide matrix / non-oxide fiber for example, SiC / SiC, C / SiC, C / C composite
  • silicon carbide is meant, for example, sintered silicon carbide with or without pressure.
  • C / SiC an SiC matrix with C fibers or a C matrix and SiC fibers.
  • a coating of the surface of the oxide ceramics with a layer of carbon will advantageously be used to improve wetting, as described in document FR-A-2831533.
  • a carbon layer may also be used.
  • the method according to the present invention uses a filler material which can in particular be a solder or brazing alloy.
  • the filler material 30 is rich in silicon. It comprises at least 40 atomic% of silicon. It comprises, for example, from 40% to 100% atomic silicon.
  • the filler material 30 comprises at least 99 atomic% of silicon.
  • the filler material 30 can be made of silicon. By constituted, it is meant that it can contain impurities linked to its preparation process and / or to its handling. The impurities represent less than 1% by mass of the composition. In this embodiment, a hybrid assembly without fusion of the filler material 30 is carried out.
  • the filler material 30 rich in silicon is a brazing alloy.
  • the alloy can be a eutectic composition or a compound with congruent fusion in the case of brazing without fusion of the solder 30.
  • the brazing alloy can also be a composition offset from the eutectic (hypo eutectic or hyper eutectic).
  • eutectic hypo eutectic or hyper eutectic
  • Such an alloy has a liquidus and a solidus, that is to say that the alloy has a semi-solid domain (a liquid part in equilibrium with a solid part) between the temperature of the liquidus TL and the temperature of the solidus Ts . In the process of the invention, such an alloy may not be melted or be partially melted during step d).
  • the alloy comprises from 40% to 97 atomic% of silicon and one or more other elements chosen from the following elements: Ag, Cr, Co, Ce, Cu, Hf, Ge, Ti, V, Zr, Nd, Pr, Ru, Rh, Re, Y, Ir, Ni, Pt, Pd, Mo, and W.
  • the process makes it possible to use numerous alloys, and even alloys containing one or more elements chosen from Ti, V, Co and Or.
  • the alloy is a binary alloy.
  • the second element preferably represents from 3% to 60% atomic of the solder 30.
  • a silicon alloy comprising, in atomic percentage, 60 to 80% Si and 40 to 20% Co.
  • the filler material 30 is, for example, chosen from the alloys presented in table 1. This table indicates in particular temperature ranges d assembly allowing partial fusion of the filler material as a function of the atomic percentage of Si in said filler material.
  • the filler material 30 is, for example, chosen from the alloys listed in table 2. This table indicates mme ranges of assembly temperatures allowing without fusion of the filler material as a function of the atomic percentage of Si in said filler material.
  • the filler material 30 is an alloy based on silver or silver-copper.
  • it is the AgCuTi alloy.
  • It is an Ag-Cu matrix and an active element Ti at low concentration, for example with 1 to 10% by mass of Ti. This alloy is less refractory than alloys based on silicon.
  • the filler material or solder 30 may be in the form of a powder whose composition is that of the solder 30 or a mixture of powders whose overall composition corresponds to that of the solder 30.
  • This powder form is, for example, used to carry out thermal spray deposition.
  • the filler material can also be in solid form (for example to then be used during PVD deposition), either a solid material whose composition is that of the filler material, or several pure solid materials which are involved in the composition of the filler material.
  • the filler material 30 is deposited at least on one of the parts 10, 20 to be assembled. For example, in FIG. 1, it is deposited only on the face 21 of one of the parts 20 to be assembled.
  • the filler material 30 partially or completely covers the face or faces 11, 21 to be assembled.
  • the filler material 30 completely covers the face 11, 21 to be assembled.
  • the filler material forms a coating consisting of an alloy or of a pure element or of a multilayer or of a gradient or architectural material.
  • the faces 11, 21 of the parts 10, 20 to be assembled are degreased in an organic solvent, for example of the alcohol, ketone, ester, ether type, or a mixture of these. , etc.
  • the filler material 30 is deposited by a dry deposition technique.
  • the vapor can be any physical vapor deposition (PVD) process.
  • the vapor can be obtained by magnetron sputtering (conventional or HiPIMS), by thermal evaporation, by electron beam, or by evaporation by cathode arc.
  • Magnetron sputtering is a technique of depositing thin layers at low pressure and low temperature in the presence of a cold plasma, from one or more targets.
  • the filler material 30 can be obtained either from a single target (solid disc) whose composition is identical to that of the desired filler material 30, or from several pure targets, each target corresponding to a constituent of the filler material 30, either from pure targets and allied (or composite) targets involved in the composition of the filler material.
  • the target (s) are sprayed and the process parameters are defined so as to obtain the targeted composition or a controlled architecture (either by spraying the composition target with that of the filler material 30, or by co-spraying the pure targets, or by co-spraying pure targets and alloyed or composite targets).
  • the thickness of the deposits obtained can vary between a few nanometers (for example 5 nm) to a few tens of micrometers (for example 20 pm).
  • the thickness of the filler material 30 deposited on the parts 10, 20 to be assembled ranges from 1 pm to 20 pm, for example of the order of 10 pm.
  • the deposit obtained is adherent and slightly rough, and may in particular have a roughness of less than 1 ⁇ m, and more particularly between 0.2 ⁇ m and 0.3 ⁇ m. It is therefore not necessary to rectify or polish the layer formed by the filler material.
  • the filler material 30 is deposited by a thermal chemical vapor deposition (CVD) process or by plasma assisted chemical vapor deposition (PECVD).
  • CVD thermal chemical vapor deposition
  • PECVD plasma assisted chemical vapor deposition
  • the filler material 30 is deposited by a spraying process.
  • it is a thermal projection, for example a plasma thermal projection in an enclosure under low pressure.
  • the filler material 30, in the form of powder is projected by means of a carrier gas onto the substrate to be coated.
  • Thermal spraying can be carried out under an inert atmosphere or in air.
  • thermal spray deposition under an inert atmosphere to avoid oxidizing the elements of the filler material (in the case where the filler materials are liable to oxidize).
  • a person skilled in the art may also choose to carry out the deposition by thermal spraying in air, for example, for Si-based solders.
  • This embodiment makes it possible to cover the parts 10, 20 to be assembled with a layer of filler material 30 having a thickness ranging from 100 ⁇ m to 300 ⁇ m.
  • the layer obtained has a lamellar structure.
  • the deposition step is preferably followed by a step in which the roughness of the deposited filler material is reduced.
  • the thermal projection leads to a deposit of high roughness (typically greater than 20 pm, even greater than 40 pm, FIG. 2). Dips and bumps with maximum deviations of a few tens of micrometers are observed.
  • This step can be carried out by rectifying or polishing the deposited solder composition.
  • the rectification can be carried out by machining with a diamond wheel.
  • the roughness Ra is reduced to a value ranging from 0.1 to 1 miti.
  • the roughness can be measured with an interferometer or with a roughness meter.
  • the parts 10, 20 can be assembled without modifying the roughness of the deposited filler material 30.
  • step c the faces 11, 21 of the parts 10, 20 to be assembled are brought into contact.
  • the filler material or the solder 30 is preferably in direct contact with the parts to be assembled. There are no intermediate elements between the filler material and the parts 10, 20 to be assembled.
  • the filler material 30 is interposed between the faces 11, 21 of the parts 10, 20 to be assembled (so-called “sandwich” configuration).
  • Tools can be used to maintain good contact between the surfaces.
  • pressure is applied to the parts 10, 20 to be assembled.
  • This pressure is slight in the case of an embodiment with partial fusion and more important in an embodiment without fusion.
  • the pressure can be exerted, for example, by tightening a tool or by expanding a tool or with a hot axial compression machine or by hot isostatic compression.
  • a pressure of 2 to 30 MPa and preferably 5 to 30 MPa can be applied.
  • it will advantageously be limited to a pressure of 20 MPa or even 10 MPa so as not to damage the parts 10, 20.
  • step d) the filler material 30 and the parts 10, 20 to be assembled are subjected to a heat treatment.
  • the heat treatment is carried out at a temperature corresponding to the assembly temperature, also called the maximum bearing temperature, to carry out the assembly, properly speaking, so as to form a joint and a single assembled object.
  • the assembly temperature is maintained for a determined period, called hold time, so as to achieve a plateau at the assembly temperature.
  • the assembly temperature, as well as the holding time can be determined by phases of assembly test and characterization of the joint formed by the filler material.
  • the characterization of the joint can in particular be carried out via a mechanical test making it possible to evaluate the connections between the filler material and the surface of the parts to be assembled. The result of these tests then makes it possible to determine the most suitable assembly temperature / holding time couple depending on the characteristics of the seal required.
  • the assembly temperature is chosen so as to partially melt the filler material or the solder 30, which makes it possible to form the joint and strong part / joint interfaces.
  • the bearing temperature is lower than the melting temperature of the filler material 30.
  • the filler material 30 is an alloy having a liquidus and a solidus.
  • the bearing temperature is higher than the temperature of the solidus Ts and lower than that of the liquidus TL of the alloy.
  • a domain between the liquidus and the solidus that is not too narrow, that is to say with a difference of at least 50 ° C. between the liquidus and the solidus, will be chosen to carry out the assembly with partial fusion.
  • the temperature is at least 10 to 30 ° C lower than the liquidus temperature of the filler material 30.
  • an assembly temperature which is at least 10 to 20 ° C lower will be chosen, or from 20 to 30 ° C, at the liquidus temperature of the filler material 30.
  • the bearing temperature is chosen so as not to melt the alloy.
  • a temperature below the melting temperature or the solidus temperature of the filler material 30 so as not to melt the alloy.
  • the temperature is 20 to 200 ° C lower than the melting temperature or the solidus temperature of the filler material 30 so as not to melt the alloy.
  • a bearing temperature of 30 to 150 ° C., and even more preferably from 50 to 100 ° C. will be chosen at the melting temperature or at the temperature of the solidus of the filler material 30.
  • the material intake or solder 30 does not necessarily have a liquidus and a distinct solidus, that is to say that the filler material 30 can be a eutectic composition (total fusion as soon as the temperature of the eutectic is reached) or a compound defined with congruence fusion therefore without semi-solid domain .
  • This embodiment is not limited to filler materials with a liquidus - solidus domain extended by at least 50 ° C.
  • the heat treatment is carried out under vacuum and / or under neutral gas.
  • neutral gas is meant an inert gas, such as argon. It can also be carried out in air for certain filler materials.
  • the vacuum is a secondary vacuum, that is to say that the pressure is from 10 3 to 10 4 Pa.
  • the first stage is carried out in the solid domain, for example at a temperature of 100 ° C. to 200 ° C. below the assembly stage for a period of time, for example, from 0.5 to 1 hour.
  • step e the assembly is cooled to room temperature (20-25 ° C).
  • the joint obtained at the end of the process has a very homogeneous microstructure, which reduces the dispersion in the mechanical behavior of the junction and improves the reliability of the junction.
  • the mechanical behavior with a two-phase alloy is better than with pure silicon.
  • the assembly can operate at very high temperatures. It can withstand operating temperatures up to 1600 ° C.
  • the applications of the method according to the invention are multiple.
  • Example 1 Assembly of sintered SiC / brazing 30 CoSi deposited by thermal spraying under vacuum / sintered SiC obtained after partial melting of the filler material 30.
  • two pieces 10, 20 of SiC, of dimensions 15 mm ⁇ 15 mm ⁇ 5 mm, are assembled with a solder 30 comprising a lOCo-90Si alloy (atomic%).
  • the alloy was produced by mixing Si and CoSi 2 powders and shaped by an agglomeration-drying process.
  • the filler material 30 was deposited by thermal spraying under vacuum (120 mbar) by blown arc plasma on the faces 11, 21 to be assembled from each part. A dense and adherent deposit, with a thickness of 150 ⁇ m, is thus obtained. It has a fine, two-phase lamellar structure, formed of Si lamellae and CoSi 2 lamellae ( Figure 3).
  • the coated faces 11, 21 are polished and then cleaned with acetone and then with ethanol.
  • the faces 11, 21 thus prepared are brought into contact and held by a tool.
  • the tooling makes it possible to avoid any offset between the parts 10, 20 during the subsequent operations.
  • the whole is placed in an oven, under secondary vacuum, then heated to 1200 ° C, for 2 hours, then heated to 1300 ° C, for 5 minutes.
  • the filler material 30 is partially melted at such a temperature.
  • the assembly obtained was cut, coated and polished to be observed by scanning electron microscopy ( Figures 4A and 4B).
  • the images obtained are represented in FIGS. 4A and 4B.
  • the joint is well filled with the filler material 30.
  • the microstructure is very homogeneous with a good distribution of the CoSi 2 phases (in white in FIGS. 4A and 4B) and Si (in gray).
  • the brazing joint is more homogeneous than a brazing joint which would be obtained after total melting and solidification. Such a joint would have a heterogeneous structure with primary Si and eutectic crystals.
  • Example 2 Assembly of sintered SiC / brazing 30 CoSi deposited by thermal spraying under vacuum / sintered SiC obtained after partial melting of the filler material 30, manufacture of 4-point bending test pieces and 4-point bending test.
  • 4-point bending test pieces are obtained by assembling two SiC plates (dimensions 120 mm x 26 mm x 7 mm) with a solder 30 identical to that of Example 1.
  • the filler material 30 was deposited by thermal spraying under vacuum by arc plasma blown on the faces 11, 21 to be assembled from each plate (FIG. 5).
  • the coated faces 11, 21 are rectified, then positioned one against the other in a holding and tightening tool. This assembly is placed in a secondary vacuum oven then heated to 1200 ° C for 2 hours, then heated to 1330 ° C for 15 minutes.
  • test pieces were characterized at 20 ° C and five test pieces were characterized at 1000 ° C. At 20 ° C, they have rupture stresses between 41 and 63 MPa (average: 56 MPa). At 1000 ° C, the breaking stresses are between 138 and 230 MPa (average: 180 MPa).
  • Example 3 Assembly of sintered SiC / brazing 30 CoSi deposited by thermal spraying in air / sintered SiC obtained after partial melting of the filler material 30, manufacture of 4-point bending test pieces and 4-point bending test.
  • 4-point bending test pieces are obtained by assembling two SiC plates (dimensions 120 mm x 26 mm x 7 mm) with a solder 30 identical to that of Example 1.
  • the filler material 30 was deposited by thermal spraying in air by arc plasma blown on the faces 11, 21 to be assembled from each plate.
  • the coated faces 11, 21 are rectified, then positioned one against the other in a holding and tightening tool.
  • This assembly is placed in a secondary vacuum oven then heated to 1200 ° C for 2 hours, then heated to 1330 ° C for 15 minutes.
  • Example 4 Assembly of sintered SiC / brazing 30 CoSi deposited by vacuum PVD / sintered SiC obtained after partial melting of the filler material 30, manufacture of 4-point bending test pieces and 4-point bending test.
  • 4-point bending test pieces are obtained by assembling two SiC plates (dimensions 120 mm x 26 mm x 7 mm) with a solder 30 comprising an lOCo-90Si alloy (atomic%).
  • the SiCo alloy was deposited on the faces to be assembled by magnetron sputtering by co-sputtering of Si and Co targets. A dense and adherent deposit, with a thickness of 15 to 20 ⁇ m, is thus obtained.
  • the coated faces 11, 21 are positioned one against the other in a holding and tightening tool. This assembly is placed in a secondary vacuum oven then heated to 1200 ° C for 2 hours, then heated to 1330 ° C for 15 minutes.
  • the two plates are integral and 4-point bending test pieces (50 x 4 x 3 mm 3 ) are machined in this set (11 test pieces). They have a joint thickness of the order of 35 ⁇ m. These test pieces were characterized at 20 ° C and have rupture stresses between 54 and 116 MPa, average at 92 MPa (on 6 test pieces). At 1000 ° C, the breaking stresses are between 131 and 168 MPa (average: 147 MPa on 5 test pieces).
  • Example 5 Assembly of sintered SiC / brazing ZrSi 30 deposited by vacuum PVD / sintered SiC obtained without fusion of the filler material 30, manufacture of 4-point bending test pieces and 4-point bending test.
  • 4-point bending test pieces are obtained by assembling two SiC plates (dimensions 120 mm x 26 mm x 7 mm) with a solder 30 comprising an alloy 10Zr -90Si (atomic%).
  • the SiZr alloy was deposited on the faces to be assembled by magnetron sputtering by co-sputtering of Si and Zr targets. A dense and adherent deposit, with a thickness of 20 to 25 ⁇ m, is thus obtained.
  • the coated faces 11, 21 are positioned one against the other in a holding and tightening tool. This assembly is placed in a secondary vacuum oven then heated to 1200 ° C for 2 hours, then heated to 1330 ° C for 10 hours.
  • the two plates are integral and 4-point bending test pieces (50 x 4 x 3 mm 3 ) are machined in this set (10 test pieces). They have a joint thickness of the order of 45 ⁇ m.
  • test pieces were characterized at 20 ° C and have rupture stresses between 47 and 77 MPa, average at 57 MPa on 10 test pieces.
  • Example 6 Assembly of a bursting maguette: Sintered SiC / ZrSi brazing deposited by thermal spraying under vacuum / Sintered SiC obtained without fusion of the filler material. Burst test.
  • two SiC plates of dimensions 115 mm x 80 mm x 10.5 mm with a machining in the center, including a plate with a hole, (see FIG. 7), are assembled with a solder comprising an alloy lOZr— 90Si ( % atomic) (the solder appears in gray, the SiC not coated in black).
  • the alloy was produced by mixing Si and ZrSi 2 powders and shaped by an agglomeration-drying process.
  • the filler material 30 was deposited by thermal spraying under vacuum (120 mbar) by blown arc plasma on the faces to be assembled of the model, masks cover the internal machined area so as not to be coated. A dense and adherent deposit, with a thickness of 280 ⁇ m, is thus obtained on each.
  • the coated faces are rectified to reach a thickness of 100 ⁇ m of deposit.
  • the parts are then cleaned with acetone and then with ethanol.
  • the faces thus prepared are brought into contact and maintained by a clamping tool.
  • the whole is placed in an oven, under secondary vacuum, then heated to 1200 ° C, for 2 hours, then heated to 1350 ° C, for 10 hours.
  • the filler material 30 is not melted at such a temperature.
  • the assembly obtained was installed on a test bench to increase the water pressure.

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  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Laminated Bodies (AREA)
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EP19753175.9A 2018-07-20 2019-07-18 Verfahren zum hybriden zusammenbau von teilen aus keramik oder einem keramikmatrixverbundstoff mithilfe eines abgabematerials, das abgeschieden und dann ohne totalverschmelzung dieses abgabematerials erhitzt wird Pending EP3823945A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1856772A FR3084077B1 (fr) 2018-07-20 2018-07-20 Procede d'assemblage hybride de pieces en ceramique ou en composite a matrice ceramique a l'aide d'un materiau d'apport depose puis chauffe sans fusion totale de ce materiau d'apport
PCT/FR2019/051810 WO2020016535A1 (fr) 2018-07-20 2019-07-18 Procede d'assemblage hybride de pieces en ceramique ou en composite a matrice ceramique a l'aide d'un materiau d'apport depose puis chauffe sans fusion totale de ce materiau d'apport

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EP3823945A1 true EP3823945A1 (de) 2021-05-26

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CN112338346B (zh) * 2020-10-29 2022-11-04 河海大学常州校区 一种采用瞬间液相扩散焊连接蓝宝石的方法
CN113979771B (zh) * 2021-10-19 2022-10-11 中国航发沈阳黎明航空发动机有限责任公司 一种含导热层的夹芯结构陶瓷基复合材料及制备方法

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Publication number Priority date Publication date Assignee Title
DE3003186C2 (de) * 1980-01-30 1983-01-27 Dornier System Gmbh, 7990 Friedrichshafen Anwendung des Diffusionsschweißens zur Verbindung von Bauteilen aus Siliciumverbundwerkstoffen
DE69313972T2 (de) * 1992-10-30 1998-03-26 Corning Inc Mikrolaminierte Verbundstoffe und Verfahren zu deren Herstellung
FR2728561B1 (fr) * 1994-12-21 1997-01-24 Commissariat Energie Atomique Composition et procede de brasage d'une ceramique comprenant de l'alumine
FR2748471B1 (fr) * 1996-05-07 1998-06-12 Commissariat Energie Atomique Assemblage par brasage de materiaux ceramiques contenant du carbure de silicium
FR2749787B1 (fr) * 1996-06-12 1998-07-24 Commissariat Energie Atomique Procede d'assemblage a l'aide d'un joint epais de pieces en materiaux a base de sic par brasage refractaire et joint refractaire et epais ainsi obtenu
FR2831533B1 (fr) 2001-10-29 2004-07-30 Commissariat Energie Atomique Procede de metallisation et/ou brasage selectif par une composition de metallisation de pieces en ceramique oxyde non mouillable par ladite composition
FR2907448B1 (fr) 2007-09-25 2010-12-10 Snecma Composition de brasure et procede d'assemblage par brasage utilisant cette composition
FR2936176B1 (fr) 2008-09-22 2011-06-03 Commissariat Energie Atomique Procede d'assemblage moyennement refractaire de pieces en materiaux a base de sic par brasage non reactif, compositions de brasure, et joint et assemblage obtenus par ce procede
FR2949696B1 (fr) 2009-09-08 2012-01-13 Commissariat Energie Atomique Procede d'assemblage de pieces en materiaux a base de sic par brasage non-reactif, compositions de brasure, et joint et assemblage obtenus par ce procede.
FR2984781B1 (fr) * 2011-12-22 2014-01-24 Commissariat Energie Atomique Procede d'assemblage par brasage d'un substrat comprenant du pyrocarbone avec des pieces comprenant du pyrocarbone.

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