US3789499A - Method of fabrication of a composite product made up of at least two components having different compositions - Google Patents

Method of fabrication of a composite product made up of at least two components having different compositions Download PDF

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Publication number
US3789499A
US3789499A US00277529A US3789499DA US3789499A US 3789499 A US3789499 A US 3789499A US 00277529 A US00277529 A US 00277529A US 3789499D A US3789499D A US 3789499DA US 3789499 A US3789499 A US 3789499A
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United States
Prior art keywords
components
contact surfaces
order
niobium
alumina
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Expired - Lifetime
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US00277529A
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English (en)
Inventor
M Pequignot
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/34—Oxidic
    • C04B2237/343—Alumina or aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/403—Refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C04B2237/765—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc at least one member being a tube
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/78—Side-way connecting, e.g. connecting two plates through their sides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering

Definitions

  • ABSTRACT At least two components having different compositions, such as niobium and alumina, and mating contact surfaces are. brought together in edgewise relation in order to be diffusion-bonded, the contact surface adopted for each component or the line of extension of said surface being such as to pass through an axis which is common to both components.
  • Each surface is polished to an optical finish and the components are assembled so that said surfaces are in mating relation with zero clearance.
  • a moderate holding pressure is applied to the components and these latter undergo a heat treatment at high temperature for a limited period of time and at low pressure in an inert atmosphere or in a vacuum.
  • FIG. 1 A first figure.
  • Thermionic conversion diodes are designed for hightemperature operation and are usually made up of two metallic sheaths between which is interposed an insulating spacer element.
  • the metal employed for the fabrication of the sheaths aforesaid is pure or alloyed niobium and the associated insulating spacer element is of alumina.
  • one of the problems involved in the construction of diodes of this type lies in the need for an intimate bond between two tubular components having different compositions, one component being formed of either pure or alloyed niobium and the other component being formed of alumina.
  • tubular components aforesaid are first engaged in interfitting relation and joined together in pairs at their respective lateral contact surfaces.
  • a method for bonding a ceramic element of alumina and an element of metal such as niobium without addition of any other material between the two elements to be bonded has also been proposed.
  • a niobium disc is applied against the extremity of a tube at a sufficient pressure to ensure that they are maintained in position.
  • the entire assembly is heated to 1,800 C and the disc is heated to 2,050 C for a few seconds in order to facilitate penetration of the disc at the surface of the alumina.
  • Diffusion bonding of two ceramic components formed of alumina, for example, by interposition of a metallic component has already been carried out with aluminum, titanium and vanadium but this type of bond has not been formed with niobium.
  • an alumina-niobium bond has been formed by placing the niobium in a mold, by pouring particles of alumina into said mold and then heating to a temperature within the range of 1,500 to 1,800 C between 150 and 250 kg/cm
  • Leak-tight joints have also been formed between ceramic and metal components within vacuum tubes or evacuated enclosures.
  • the surfaces to be placed in contact with each other are polished and coated with a thin layer of silver which is polished until an optical surface finish is obtained, diffusion being carried out in the hot state and under pressure.
  • the metals employed are silver, gold or platinum.
  • the present invention is directed to a method of obtaining a composite product of this type in the most economical manner.
  • the invention is also directed to the composite product which is thus obtained.
  • the method according to the invention which is generally intended for the fabrication of a composite prod uct made up of at least two components having different compositions and joined together by diffusion bonding along mating contact surfaces brought together in edgewise relation, is characterized in that the contact surface adopted for each component aforesaid or the line of extension of said surface intersects with an axis which is common to both components, said surface is polished to an optical finish, the components are assembled so that said surfaces are in mating relation with zero clearance, a moderate holding pressure is applied thereto and said components are subjected to a heat treatment at high temperature for a limited period of time and at low pressure in an inert atmosphere or in a vacuum.
  • the contact surface of the components to be joined together is a flat, conical or spherical surface.
  • the bonding process in accordance with the invention does not simply consist in forming a bond by diffusion of the components into each other at the level of their contacting surface.
  • the aluminum which is formed penetrates into the metal to a depth which can attain I microns whilst the metal penetrates into the alumina to a depth which can attain 20 microns.
  • the heat treatment in accordance with the invention is advantageously applied only for a period of less than one hour; since the diffusion bonding operation should preferably be carried out in a pro- 1 tective atmosphere, this operation can be performed in accordance with the invention either in a vacuum or in an inert atmosphere at ordinary pressure or at a slight overpressure.
  • FIG. 1 is a partial axial sectional view of the composite product to be fabricated
  • FIG. 2 is a view in perspective showing said composite product prior to assembly
  • FIG. 3 is a view in sectional elevation which illustrates the bonding of said composite product
  • FIG. 4 is a view which is similar to FIG. 1 and relates to an alternative form of construction.
  • the invention is applied to the bonding of three tubular components placed successively in endto-end relation, namely a metallic component 10, an insulating component I1 and a metallic component 12.
  • the resultant composite product 13 finds an application especially in the construction of thermionic conversion diodes, in which case the metallic component 10 is made integral with a first metallic sheath (not shown) whilst the metallic component 12 is made integral with a second metallic sheath (not shown), said metallic sheath being separated from each other by the insulating distance-piece or spacer element 1 1.
  • the metallic components l0, 12 are frequently formed of pure or alloyed niobium and the spacer element 11 is formed of alumina.
  • the invention proposes to effect diffusion bonding of the components aforesaid along contact surfaces such that either the surfaces themselves or their lines of extension intersect with their axis 15.
  • said contact surfaces are plane surfaces 16 located at right angles to the axis 15.
  • said plane surfaces 16 are carefully machined as illustrated diagrammatically in FIG. 2 in such a manner as to give them a highly polished surface finish.
  • the thickness of this polished surface is at least of the order of one-tenth of a micron and preferably onehundredth of a micron.
  • the components 10, 11 and 12 are applied against each other in end-to-end relation at their contact surfaces 16, then placed within a sealed enclosure 20 which is equipped with heating means 21.
  • the components 10, 11 and 12 are held in position by subjecting these latter to a moderate pressure of the order of 1 bar as indicated diagrammatically by the arrow 22 of FIG. 3 and a plurality of units to be bonded can be placed on top of each other.
  • a vacuum is then created within the enclosure 20 and the components 10, 11 and 12 are brought by heating means 21 to a high temperature of the order of 1,500l ,800 C, for example, depending on the nature of the materials to be bonded.
  • This temperature is maintained for a period of less than 1 hour.
  • the components 10, 11 and 12 are then joined together by diffusion bonding and allowed to cool naturally either in a vacuum or in a neutral atmosphere this cooling process can last a few hours.
  • the contact surfaces 16 of the tubular components 10, 11 and 12 are spherical, the centers of said surfaces being preferably located on the axis of revolution of said components.
  • the arrangement adopted in this embodiment is such that the alumina component 11 is put in compression at the time of hightemperature service of the composite product which is thus formed; this putting in compression is conducive to long service life of the component since the compressive strength of alumina is higher than its tensile strength.
  • the invention does not apply solely to the construction of thermionic diodes but extends more generally to all devices which embody the principles of electron physics, e.g., electron tubes, particle accelerators, vacuum devices, semiconductor devices and the like.
  • a method of diffusion bonding components of alumina to niobium or niobium alloy components comprising the steps of polishing to an optical finish the contact surfaces of said components, assembling the components so that the contact surfaces are in mating relation with zero clearance, bonding said surfaces together by diffusion bonding by applying a moderate holding pressure of about one bar to the components while subjecting the components to a heat treatment at a temperature within the range of l,500to 1,800C. for a period of time on the order of one hour in an inert atmosphere or vacuum, and then naturally cooling the components.
  • optical polish applied to the contact surfaces is at least of the order of one-tenth of a micron and preferably of the order of one-hundredth of a micron.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Laminated Bodies (AREA)
US00277529A 1971-08-09 1972-08-03 Method of fabrication of a composite product made up of at least two components having different compositions Expired - Lifetime US3789499A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR7129035A FR2148888A5 (enrdf_load_stackoverflow) 1971-08-09 1971-08-09

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US (1) US3789499A (enrdf_load_stackoverflow)
FR (1) FR2148888A5 (enrdf_load_stackoverflow)
GB (1) GB1365403A (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4661181A (en) * 1984-05-25 1987-04-28 Thomson-Csf Method of assembly of at least two components of ceramic material each having at least one flat surface
US4662958A (en) * 1983-03-18 1987-05-05 The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland Method of making a ceramic evacuatable enclosure
US5573173A (en) * 1992-11-02 1996-11-12 U.S. Philips Corporation Vacuum tube comprising a ceramic element and a method of interconnecting a ceramic element and a conductive element

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015046091A1 (ja) * 2013-09-27 2015-04-02 独立行政法人産業技術総合研究所 ステンレス鋼部材の接合方法およびステンレス鋼

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2564738A (en) * 1947-02-25 1951-08-21 Foerderung Forschung Gmbh Method of forming a vacuum-tight bond between ceramics and metals
GB761045A (en) * 1952-08-29 1956-11-07 Lodge Plugs Ltd Improvements in or relating to the bonding of ceramics with copper
US3324543A (en) * 1965-03-26 1967-06-13 Charles I Mcvey Pressure bonded ceramic-to-metal gradient seals
US3389215A (en) * 1966-03-04 1968-06-18 Gen Motors Corp High temperature alumina-to-niobium article
US3468647A (en) * 1967-10-04 1969-09-23 Hughes Aircraft Co Ceramic-metal seal
US3517432A (en) * 1968-05-02 1970-06-30 Atomic Energy Commission Diffusion bonding of ceramics
US3531853A (en) * 1966-11-30 1970-10-06 Philips Corp Method of making a ceramic-to-metal seal
US3736658A (en) * 1970-10-12 1973-06-05 Atomic Energy Commission Thermionic gas-pressure-bonded sheathed insulators and method of producing same

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2564738A (en) * 1947-02-25 1951-08-21 Foerderung Forschung Gmbh Method of forming a vacuum-tight bond between ceramics and metals
GB761045A (en) * 1952-08-29 1956-11-07 Lodge Plugs Ltd Improvements in or relating to the bonding of ceramics with copper
US3324543A (en) * 1965-03-26 1967-06-13 Charles I Mcvey Pressure bonded ceramic-to-metal gradient seals
US3389215A (en) * 1966-03-04 1968-06-18 Gen Motors Corp High temperature alumina-to-niobium article
US3531853A (en) * 1966-11-30 1970-10-06 Philips Corp Method of making a ceramic-to-metal seal
US3468647A (en) * 1967-10-04 1969-09-23 Hughes Aircraft Co Ceramic-metal seal
US3517432A (en) * 1968-05-02 1970-06-30 Atomic Energy Commission Diffusion bonding of ceramics
US3736658A (en) * 1970-10-12 1973-06-05 Atomic Energy Commission Thermionic gas-pressure-bonded sheathed insulators and method of producing same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Garrett et al., Broad Applications of Diffusion Bonding, NASA CR 409, March 1966, pp.xii xiii, 32 39, Technical Library. *
Morris Berg et al., Ceramic to Aluminum Seal, RCA Technical Notes No. 124, Mar. 12, 1958. *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4662958A (en) * 1983-03-18 1987-05-05 The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland Method of making a ceramic evacuatable enclosure
US4661181A (en) * 1984-05-25 1987-04-28 Thomson-Csf Method of assembly of at least two components of ceramic material each having at least one flat surface
US5573173A (en) * 1992-11-02 1996-11-12 U.S. Philips Corporation Vacuum tube comprising a ceramic element and a method of interconnecting a ceramic element and a conductive element

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GB1365403A (en) 1974-09-04
FR2148888A5 (enrdf_load_stackoverflow) 1973-03-23

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