EP1343600B1 - Herstellungsverfahren für dünne bänder aus metall/keramik-kompositmaterial - Google Patents

Herstellungsverfahren für dünne bänder aus metall/keramik-kompositmaterial Download PDF

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Publication number
EP1343600B1
EP1343600B1 EP01999450A EP01999450A EP1343600B1 EP 1343600 B1 EP1343600 B1 EP 1343600B1 EP 01999450 A EP01999450 A EP 01999450A EP 01999450 A EP01999450 A EP 01999450A EP 1343600 B1 EP1343600 B1 EP 1343600B1
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EP
European Patent Office
Prior art keywords
suspension
ceramic
metal
film
binder
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.)
Expired - Lifetime
Application number
EP01999450A
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English (en)
French (fr)
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EP1343600A1 (de
Inventor
Jean-François SILVAIN
Thierry Chartier
Pierre-Marie Geffroy
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Centre National de la Recherche Scientifique CNRS
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Centre National de la Recherche Scientifique CNRS
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    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the invention relates to a method for manufacturing thin metal / ceramic composite films, in which the ceramic reinforcements are homogeneously distributed in the metal matrix.
  • the invention finds applications in all fields using metal / ceramic composite substrates or films and, in particular, in the field of the manufacture of electronic components intended, for example, in the field of automotive or automotive aeronautics.
  • the metal films are made by a rolling process.
  • this rolling method does not make it possible to obtain a homogeneous distribution of the ceramic reinforcements in the metal matrix; it is therefore not suitable for the manufacture of metal / ceramic composite films.
  • the residual stresses, caused by rolling lead to cracking of the film.
  • the purpose of the invention is precisely to remedy the thin film manufacturing processes described above. To this end, it proposes a method for manufacturing thin metal / ceramic composite films using a strip casting method.
  • the band casting technique is used to orient and control the distribution of ceramic reinforcements.
  • the process described according to the invention makes it possible to manufacture metal / ceramic composite films with an orientation of the ceramic particles in the plane of the film, in particular for highly anisotropic particles, such as fibers and platelets. This improves some properties of the composite in the plane of the film, such as decreasing the thermal coefficient of expansion and increasing the thermal conductivity.
  • the suspension has a viscosity of between 0.5 and 3 Pa.s.
  • the dispersant is a phosphoric ester, a polyacrylate, a sulfonate, a perfluorate or a carbon chain acid of 2 to 30 carbon atoms.
  • the metal powder may be a powder of copper, aluminum, silver, gold, nickel, titanium, chromium, zinc or an alloy of two or more of these materials .
  • the ceramic reinforcement may be a powder and / or a short fiber (that is to say a fiber whose length varies between 1 and 500 ⁇ m) of graphite, carbides, nitrides or oxides.
  • the densification of the film consists of sintering the film in an oven.
  • the densification of the film consists of hot rolling and annealing of the film.
  • the invention relates to a method for manufacturing thin metal / ceramic composite films.
  • This process consists in preparing a suspension, also called “slip”, comprising a substantially homogeneous mixture of ceramic reinforcements and metal particles.
  • metal particles and ceramic reinforcements are chosen, respectively, in the form of one or more metal powder (s) and one or more ceramic reinforcement (s). These powders and short fibers are mixed with an organic solvent, a dispersant, a binder and a plasticizer.
  • This step of preparation of the suspension S consists, first of all, in a grinding jar, or attrition, metal and ceramic powders with the solvent and the dispersant.
  • This grinding step is carried out by means of an attritor mill (represented by reference 1 in FIG. 1) or by a jar crusher.
  • the assembly thus obtained is then mixed with binders and plasticizers, using a mixer, referenced 2.
  • the metal powder (s) intended to form the metal matrix of the suspension may be, for example, a powder of copper, aluminum or silver. gold, nickel, titanium, chromium, zinc or an alloy of two or more of these metals.
  • the ceramic reinforcement (s) intended to form the ceramic reinforcements of this suspension may be, for example, a powder or a short graphite fiber, or a powder or a short fiber based on carbides, such as silicon carbide, nitrides, such as aluminum nitride, or oxides, such as silica or zirconium tungstate.
  • the ceramic reinforcements may be in the form of fibers or platelets or substantially spherical grains, with a diameter of between about 0.1 microns and 100 microns.
  • the fibers are generally short fibers with a diameter of 10 nm to 10 ⁇ m, and a length of 100 nm to 10 mm.
  • These ceramic reinforcements may be coated with a layer of metallic material, such as cobalt, nickel, silver or gold.
  • the thickness of the metal coating is at least 0.01 ⁇ m. This coating can be achieved by immersing the ceramic reinforcements in an electrolytic bath. This coating has the advantage of improving the densification of the material during the densification step of the film, and in particular when this densification consists of sintering because it makes it possible to increase the metal / ceramic interface.
  • the suspension used according to the invention is a suspension or organic system.
  • the solvent used to make this suspension S is an organic solvent, generally chosen from ketones, alcohols and mixtures thereof.
  • the dispersant used to produce this suspension serves to ensure the homogeneity and stability of the suspension by developing repulsion between ceramic reinforcements and metal particles.
  • the dispersant ensures good stability and good dispersion of the particles together.
  • the dispersant makes it possible, after drying, to obtain a homogeneous and compact strip.
  • This dispersant is chosen from surfactants, macromolecules, such as fish oil, phosphoric esters, polyacrylates, sulphonates, perfluorates and carbon chain acids having from 2 to 30 carbon atoms, for example oxalic acid and stearic acid.
  • the binder used to make this suspension has the role of ensuring the cohesion of the strip (or film), after evaporation of the solvent.
  • This binder is generally a non-water-soluble compound chosen from polyalcohols, vinyl compounds, such as polyvinyl butyral and acrylic compounds and mixtures thereof.
  • the plasticizer used in this suspension has the role of ensuring a great flexibility, a great fluidity, to the band; this flexibility is necessary during the casting strip of the suspension and, later, during the handling of the band.
  • This plasticizer may be, for example, a polyethylene glycol or dibutyl phthalate.
  • the suspension also contains a plasticizer which makes it possible to obtain a strip, or thin film, in flexible raw material and sufficiently strong to be handled.
  • the report binder / plasticizer makes it possible to adjust the mechanical cohesion of the strip and its flexibility. These strips can therefore be stacked and thermocompressed so as to produce stacks of bands of different compositions. This solution is not possible with the methods of the prior art.
  • FIG. 2 shows schematically the second step of the method of the invention, that is to say the strip casting step of the suspension.
  • the suspension S made during the first step is cast on a casting bench 3 so as to form a band B, also called thin film.
  • the strip casting consists of casting the suspension S on a support which may be, for example, a steel strip 8 or a polymer wire, referenced 5 in FIG. 2.
  • this suspension In order to allow easy casting of the suspension, this suspension must have a viscosity of the order of 0.5 to 3 Pa.s.
  • the casting of the suspension is obtained by the relative movement between a shoe 6 of the casting bench and the support 5.
  • the shoe 6 comprises knives 7, whose height is adjustable.
  • the thickness of the film can be modified by changing the height between these knives 7 and the support 5. It is thus possible, thanks to this band casting, a very regular film thickness.
  • thermal debinding consists in slowly heating the strip of material in a controlled atmosphere, in an oven or dryer 4 in order to remove the organic compounds contained mainly binder and plasticizer.
  • the heating rate in the dryer is of the order of 0.2 to 2 ° C / min between 100 ° C and 500 ° C.
  • Figures 3A and 3B show two different embodiments of the third step of the method of the invention, that is to say the densification step of the film.
  • This densification step consists of evaporating the solvent and drying the thin film obtained after debinding.
  • This step of densification of the film has the role of evaporating the solvent. It can be carried out, for example, in two different ways: the film can be densified by sintering in a passage furnace or in a batch oven, or by hot rolling, using a rolling mill and an annealing furnace.
  • the first variant shows that the film B, obtained after debinding, is cut into plates P1 to Pn. These plates are introduced into an oven, referenced 9, under a controlled atmosphere.
  • This oven can be a furnace or a batch oven. Densification by sintering is carried out under a controlled atmosphere, or under a reducing atmosphere, for example hydrogen, hydrogenated nitrogen, argon or hydrogenated argon, so as to avoid the oxidation of the material.
  • the sintering temperature depends on the particle size and the nature of the metal powders and ceramic reinforcements. For example, for a copper metal powder, the temperature is between 700 ° C and 1080 ° C; for aluminum, the temperature is between 450 ° C and 650 ° C.
  • the second variant of the densification step is shown in FIG. 3B.
  • the film B is introduced into a rolling mill 10, placed in an annealing furnace 11.
  • the film B is then hot rolled in the furnace 11 under a controlled atmosphere.
  • This mode of densification by hot rolling and annealing of the film makes it possible to improve the densification of the material under the action of pressure and temperature.
  • This variant is therefore particularly well suited to metal / ceramic composites which are poorly densified by natural sintering and composites made of ductile metals, such as copper, aluminum or gold.

Claims (13)

  1. Herstellungsverfahren von dünnen Folien aus einem Verbund Metall / Keramik, dadurch gekennzeichnet, dass es aus Folgendem besteht:
    a) Zubereitung einer Suspension (S) in einem organischen Lösungsmittel ausgehend von einer deutlich homogenen Mischung aus keramischen Verstärkungen aus Metallpartikeln, einem Bindemittel, einem Weichmacher und einem Dispergiermittel, wobei die Metallpartikel wenigstens zu 5 % aus der Masse der Suspension gebildet werden
    b) Durchführen eines Bandgießens der Suspension (S) zum Bilden einer dünnen Folie (B) und anschließender Durchführung eines Ablösens dieser dünnen Folie;
    c) Realisierung der Verdichtung der dünnen abgelösten Folie in einem Ofen.
  2. Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, dass die Suspension (S) eine zwischen 0,5 und 3 Pa.s inbegriffene Viskosität hat.
  3. Verfahren gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Suspension (S) durch Vermischen folgender Elemente realisiert wird:
    - wenigstens eines Metallpulvers und wenigstens einer keramischen Verstärkung, die beide rund 30 bis 60 % des Gesamtvolumens der Suspension bilden;
    - eines rund 15 bis 45 % des Volumens der Suspension bildenden organischen Lösungsmittels;
    - eines rund 30 bis 70 % des Volumens der Suspension bildenden Bindemittels und eines Weichmachers;
    - eines rund 0,1 bis 2 % der Masse der keramischen Verstärkungen und Metallpulver bildenden Dispergiermittels; und
    - von rund 0,01 bis 2 % der Masse der keramischen Verstärkungen und der Metallpulver darstellenden Zusatzstoffe.
  4. Verfahren gemäß Anspruch 1 bis 3, in dem das Bindemittel eine in Wasser nicht lösliche, aus Polyalkoholen, Vinylkomponenten, Acrylkomponenten und deren Mischungen ausgewählte Komponente ist.
  5. Verfahren gemäß Anspruch 1 bis 4, in dem das organische Lösungsmittel aus Ketonen, Alkoholen und deren Mischungen ausgewählt ist.
  6. Verfahren gemäß Anspruch 1 bis 5, in dem das Dispergiermittel aus Tensiden, Makromolekülen, wie z. B. Fischöl, Phosphorestern, Polyacrylaten, Sulfonaten, Perfluoraten und Säuren mit kohlenstoffhaltigen Ketten mit 2 bis 30 Kohlenstoffatomen ausgewählt ist.
  7. Verfahren gemäß Anspruch 3 bis 6, dadurch gekennzeichnet, dass das Metallpulver ein Kupfer-, Aluminium-, Silber-, Gold-, Nickel-, Titan-, Chrom-, Zinkpulver oder eine Legierung aus zwei oder mehreren dieser Metalle ist.
  8. Verfahren gemäß Anspruch 3 bis 7, dadurch gekennzeichnet, dass die keramische Verstärkung ein Graphit-, Karbid-, Nitrid- oder Oxydpulver und / oder eine kurze Graphit-, Karbid-, Nitrid- oder Oxydfaser ist.
  9. Verfahren gemäß Anspruch 1 bis 8, dadurch gekennzeichnet, dass die Verdichtung der Folie aus einem Frittieren der Folie in einem Ofen besteht.
  10. Verfahren gemäß Anspruch 1 bis 8, dadurch gekennzeichnet, dass die Verdichtung der Folie aus einem Warmwalzen und einem Nachhärten der Folie besteht.
  11. Verfahren gemäß Anspruch 3 bis 10, dadurch gekennzeichnet, dass die Zubereitung der Suspension aus Folgendem besteht:
    - im Zermahlen im Krug oder durch gegenseitiges Zerreiben der Metall- und Keramikpulver mit dem Lösungsmittel und dem Dispergiermittel; und dann
    - im Hinzufügen eines Bindemittels und eines Weichmachers zu dieser Substanz und im Vermischen damit.
  12. Zubereitungsverfahren eines Stücks aus Verbundmaterial mit geschichteter Struktur, in der mehrere dünne Folien gemäß den Stufen a) und b) des Anspruchs 1 gebildet werden, die genannten dünnen Folien gestapelt werden und der Stapel einer Thermokompression unterzogen wird.
  13. Verfahren gemäß Anspruch 12, in dem die dünnen Folien unterschiedliche Zusammensetzungen haben.
EP01999450A 2000-12-08 2001-12-06 Herstellungsverfahren für dünne bänder aus metall/keramik-kompositmaterial Expired - Lifetime EP1343600B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0015984 2000-12-08
FR0015984A FR2818015B1 (fr) 2000-12-08 2000-12-08 Procede de fabrication de films minces en composite metal/ceramique
PCT/FR2001/003855 WO2002045888A1 (fr) 2000-12-08 2001-12-06 Procede de fabrication de films minces en composite metal/ceramique

Publications (2)

Publication Number Publication Date
EP1343600A1 EP1343600A1 (de) 2003-09-17
EP1343600B1 true EP1343600B1 (de) 2007-04-25

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US (2) US7585456B2 (de)
EP (1) EP1343600B1 (de)
JP (1) JP4146228B2 (de)
KR (1) KR100847129B1 (de)
CN (1) CN1247352C (de)
AT (1) ATE360493T1 (de)
AU (1) AU2002216188A1 (de)
DE (1) DE60128133T2 (de)
FR (1) FR2818015B1 (de)
WO (1) WO2002045888A1 (de)

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Publication number Publication date
US20040013556A1 (en) 2004-01-22
CN1247352C (zh) 2006-03-29
US7871562B2 (en) 2011-01-18
FR2818015B1 (fr) 2003-09-26
FR2818015A1 (fr) 2002-06-14
JP4146228B2 (ja) 2008-09-10
JP2004515648A (ja) 2004-05-27
DE60128133D1 (de) 2007-06-06
EP1343600A1 (de) 2003-09-17
ATE360493T1 (de) 2007-05-15
DE60128133T2 (de) 2007-12-27
WO2002045888A1 (fr) 2002-06-13
KR20030069179A (ko) 2003-08-25
AU2002216188A1 (en) 2002-06-18
CN1479659A (zh) 2004-03-03
US20090208645A1 (en) 2009-08-20
US7585456B2 (en) 2009-09-08
KR100847129B1 (ko) 2008-07-18

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