EP1073778B1 - Procede de realisation d'une couche metallique frittee a porosite ouverte - Google Patents

Procede de realisation d'une couche metallique frittee a porosite ouverte Download PDF

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Publication number
EP1073778B1
EP1073778B1 EP98922732A EP98922732A EP1073778B1 EP 1073778 B1 EP1073778 B1 EP 1073778B1 EP 98922732 A EP98922732 A EP 98922732A EP 98922732 A EP98922732 A EP 98922732A EP 1073778 B1 EP1073778 B1 EP 1073778B1
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EP
European Patent Office
Prior art keywords
layer
suspension
process according
sintered
support
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
EP98922732A
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German (de)
English (en)
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EP1073778A1 (fr
Inventor
Peter Neumann
Andreas Kuhstoss
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GKN Sinter Metals GmbH
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GKN Sinter Metals GmbH
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    • 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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • 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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/087—Coating with metal alloys or metal elements only

Definitions

  • the invention relates to a method for producing a thin metal layer with open porosity from a sinterable Metal powder.
  • Filter body made of ceramic material must be made relatively thick due to the risk of breakage Filter body made of pressed and sintered metal powders are proportionate for manufacturing reasons thick. Because of the thickness that cannot be reduced, especially with fine-pored material, correspondingly large flow resistances on. The use of plastics as Filter material is limited by its lower strength and the low temperature resistance.
  • metallic materials as a porous layer known in the form of fabrics made from metal fibers or fleeces.
  • EP-B-0 525 325 describes a method for producing porous, metallic sintered workpieces known in the first a metal powder is suspended in a carrier liquid, which consists of a binder dissolved in a solvent and which is adjusted so that the suspension is pourable is. This suspension is poured into a mold. Subsequently the solvent is evaporated off so that the remaining binder the metal powder in the through the Form predetermined geometry is solidified and a manageable Green body forms. After separating from the mold the green body is sintered in the usual way.
  • This previously known Process is preferably proportional to the production Thick-walled sintered parts are provided due to their geometry better than a casting process in the conventional method by pressing a metal powder have it made into a mold. Thin-layered, open, Porous parts cannot be produced with this process.
  • the invention is based on the object, the known To improve the process so that even thin, porous, and provided required, self-supporting metal layers are also produced can be.
  • the sinterable powder with a predetermined Size distribution of the powder particles in a carrier liquid, formed by one with an evaporable solvent liquefied binder that is suspended Suspension in at least one thin layer on a carrier body applied, dried and the green layer thus formed is sintered, the layer thickness of the applied Suspension at least the thickness s of the to be generated Corresponds to the metal layer after sintering, where s is at least corresponds to 3 times the average diameter D of the powder particles, with D 1 ⁇ m to 50 ⁇ m, the layer thickness of the finished metal layer is a maximum of 500 microns.
  • the size of the porosity can influenced by the particle size of the metal powder used be so that there are very thin porous metal layers have the pore size specified. Because in the making Inhomogeneities and voids can occur the layer thickness is at least 3 times the diameter D of the Correspond to powder particles. By the ratio mentioned between the layer thickness s and the particle diameter D. ensured that there were always several "layers" of powder particles are stacked and continuous "holes" that larger than the desired porosity can be avoided. It is particularly expedient here if the layer thickness s 5 to 15 times, preferably 10 to 15 times Diameter D of the powder particles. "Through holes" can be avoided.
  • Diameter D is the mean particle diameter to understand the metal powder used.
  • Powder in The meaning of the invention is not only powders made of pure metals, but also powders from metal alloys and / or powder mixtures made of different metals and metal alloys to understand.
  • this includes steels, preferably Chrome-nickel steels, bronzes, nickel-based alloys such as Hastalloy, Inconel or the like, where powder mixtures can also contain high-melting components, such as platinum or the like.
  • the one to use Metal powder and its particle size is different from each Depending on the application.
  • the consistency of the to be set via the carrier liquid Suspension essentially depends on how the suspension is applied to the support body. When pouring, if necessary with subsequent wiping of an excess from the cast suspension layer, the suspension can set in a somewhat viscous consistency become. In a so-called. Pouring foil or spraying a fluid consistency must be specified.
  • the carrier liquid through a with an evaporable Solvent liquefied binder is formed. This ensures that the green layer as a result the adhesion of the individual powder particles to one another has sufficient strength over the binder.
  • the suspension in several thin sub-layers one after the other is applied to the carrier body.
  • the individual Sub-layers of suspensions with different size distributions for the metal powder used and / or different Use metal powders. This allows it for example, on the one hand to use metal powder that the Sintered metal layer has a particularly good porosity on the other hand, it is also possible to have at least one metal layer manufacture that in their metal composition has particularly favorable properties for the application, for example, has catalytic properties.
  • the partial layer applied in each case at least dried before applying the next sub-layer becomes. This ensures that the first applied sub-layer is sufficiently solidified so that it by the application method, for example by spraying the next sub-layer is not deformed. on the other hand is due to the remaining solvent content in the previously applied, dried partial layer represents that the next sub-layer is reliable and is connected with the same packing density and the finished Green layer has the desired strength.
  • the suspension as a layer on a flat, flexible Carrier body applied and after drying as a green layer separated from the carrier body and separated into one membrane-like, porous finished part is sintered.
  • This procedure is that first a proportionate large green layer can be produced can, from which after drying by punching or cutting Pieces of film and green sheet in the desired shape can be produced. With these sections peeled off the green sheet from the support body and then sintered as an independent part.
  • Can as a carrier plastic or metal foils are used here.
  • the Carrier body is expedient before the suspension is applied coated with a release agent.
  • the suspension as a layer a high-temperature resistant, preferably flat support body is applied, dried on this, sintered and then as a membrane-like, porous, metallic finished part is removed from the carrier body.
  • a carrier body used as a carrier body one is a material that does not bond during sintering with the green layer on the support body, as is the case, for example, with ceramic materials If this is the case, this procedure offers the possibility of membrane-like metallic porous finished parts industrially with a low Share of manual work with extensive automation to manufacture.
  • the particular advantage here is that the dry, still sensitive green layer to carry out the sintering process is not lifted off the carrier body and must be handled here, but that they only after the Sintering is removed.
  • the suspension can be poured or spraying can be applied to the carrier body.
  • a contour mask of the suspension on the carrier body is launched. This makes it possible to apply the suspension to apply the carrier already in the intended final contour, so that a subsequent cutting process is omitted.
  • Another advantage of using a contour mask is in that the applied in particular by a spraying process Suspension also in that limited by the contour mask Edge area has the predetermined layer thickness.
  • the finished sintered porous membrane is calibrated by rolling.
  • the pore size in the The metal layer defines shrink because of the small Thick not only the surface areas, but the metal layer overall "deformed". But that's also given the opportunity to start with something greater thickness and a somewhat coarser and therefore cheaper Produce metal powder and then by the rolling process to reproducibly reduce the pore size.
  • the carrier body is also part of the finished part and accordingly the metal layer is solid with it is to be connected is in a different embodiment provided that the suspension on at least one surface of a metallic carrier body applied, dried and the green layer then sintered firmly onto the carrier body becomes.
  • the carrier body can in turn be a Sintered molded part, also a porous sintered molded part with coarser Pore structure.
  • the suspension can in turn be cast by thin film, Spray or dip on the surface of the Carrier body are applied.
  • the metal layer can ever depending on the intended use on the outer wall and / or the inner wall be applied.
  • the metallic carrier body is replaced by a tubular one Carrier body formed, then is in an embodiment of the invention Process provided that when applying the Suspension and at least during part of the dry season the carrier body is rotated about the pipe axis. This is ensures that the layer thickness until the solidification Get suspension as a green layer on the support body remains. It is useful here, especially when thin-film casting and when spraying when the suspension exits defined in addition to the rotation relative to the surface is moved.
  • one is made from one sinterable metal powder and a carrier liquid formed suspension with the help of a spray or pouring head 1 on a carrier body 2 in the form of a larger film section from a plastic or metal foil as a thin Layer 3 is applied.
  • the one with a thin suspension layer 3 coated carrier body 2 is here by a larger film section then in a drying facility 4 guided, in the heat of the carrier liquid, evaporated, for example, ethanol or isopropanol becomes.
  • a binder dissolved in the carrier liquid remains in the thin to increase the green strength Layer.
  • the die-cut is also punched out Part 2.1 of the carrier film is peeled off from the green sheet 3.1, which are then introduced as green compact 3.2 into a sintering furnace 9 and there among those for the respective powder composition specified conditions is sintered. From the Sintering furnace 9 can then produce the finished part 3.3 in the form of a solid thin metal layer with open porosity removed become.
  • a mask 10 which with a cutout 11 is provided which corresponds to the desired final contour corresponds to the porous metal layer part to be produced. Then - as described with reference to FIG. 1 - the support body 2.2 provided with a corresponding mask With the help of a spray or pouring head 1 with the metal suspension sprayed so that on the support body 2.2 through the cutout 11 the mask 10 delimited a corresponding area, thin suspension layer 3 is applied.
  • a spray or pouring head 1 with the metal suspension sprayed so that on the support body 2.2 through the cutout 11 the mask 10 delimited a corresponding area, thin suspension layer 3 is applied.
  • Mask 10 with a corresponding plurality of cutouts 11 be provided.
  • the mask 10 is removed, so that the carrier body 2.2 with the remaining thin Suspension layer 3 are introduced into the drying oven 4 can, in which the carrier liquid is evaporated.
  • the carrier body 2.2 the green layer 3 removed which is shown schematically here a bending of the carrier body 2.2 on the edge of a cutting edge 12 is indicated, so that subsequently the isolated green body is sintered again in the sintering furnace 9.
  • the finished part 3.3 in the form of a solid, thin Metal layer with open porosity can be removed.
  • the stamping step 5 is omitted because through the mask 10 with its cutout 11 the required contour already exists. The carrier body remains intact and can be used again.
  • the method shown schematically in FIG. 3 corresponds in its sequence up to the process step of drying in Drying oven 4 the method described with reference to FIG. 2, so that reference is made to the previous description can.
  • the only difference is that the carrier body 2.2 made of a high temperature resistant material there is no connection with the on the sintering Carrier body located green layer 3 comes in as this for example in the case of a ceramic material.
  • the carrier body 2.2 with the green compact 3.2 on it in the sintering furnace 9 introduced and also together with the carrier body 2.2 removed from the sintering furnace 9 again. Only that done sintered, porous metal layer part 3.3. is then from the carrier body 2.2 decreased.
  • the method described with reference to FIG. 3 also offers furthermore the advantage that initially only one layer the temperature-resistant support body 2.2 applied and on the Carrier body is sintered. Then the ready sintered, still on the carrier body 2.2 porous metal layer, a further layer of an optionally differently composed suspension applied then - as described above - dried and sintered. The sintering process results in a firm bond between the first and the second as well as each further, in metal layer applied in this way.
  • the advantage is there in doing so in that the second and each additional one still to be applied Metal layer in terms of its different composition also sintered under other temperature conditions can be.
  • a high powder metal composition Sintering temperature as a porous layer and then sintering metal powder compositions in the second and each additional layer to sinter as a porous layer, which is due to their compositions at lower temperatures have to be sintered. This ensures that the desired by adapted sintering conditions Porosity of the individual layers is preserved.
  • Contour masks are also given the option of applying the suspension in the spray process after each Form the main layer additional overflows in the edge area perform so as to have a porous metal layer part reinforced edge.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Filtering Materials (AREA)

Claims (13)

  1. Procédé de réalisation d'une couche métallique mince à porosité ouverte à partir d'une poudre métallique frittable de métaux purs, d'alliages de métaux et/ou de mélanges de poudres composés de métaux et d'alliages de métaux différents, caractérisé en ce que la poudre métallique est mise en suspension avec une répartition dimensionnelle donnée des particules de poudre dans un liquide de support formé par un liant rendu liquide à l'aide d'un solvant pouvant s'évaporer, que la suspension est appliquée en au moins une couche mince sur un corps de support et séchée, et que la couche de vert ainsi obtenue est frittée, l'épaisseur de couche de la suspension appliquée correspondant au moins à l'épaisseur s de la couche métallique à réaliser après le frittage, s correspondant au moins 3 fois au diamètre D moyen des particules de poudre, avec D = de 1 µm à 50 µm, l'épaisseur de couche de la couche métallique terminée étant de 500 µm maximum.
  2. Procédé selon la revendication 1, caractérisé en ce que la suspension est appliquée sur le corps de support en plusieurs couches partielles successives.
  3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que pour les différentes couches partielles, des suspensions présentant des répartitions dimensionnelles différentes et/ou des métaux différents sont respectivement utilisées.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que chaque couche partielle respective est au moins partiellement séchée avant l'application de la couche partielle suivante.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que chaque couche partielle respective est frittée avant l'application de la couche partielle suivante.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que la suspension est appliquée sous forme de couche sur un corps de support plat flexible, qu'après séchage elle est séparée du corps de support sous forme de couche de vert, puis frittée séparément pour obtenir une pièce finie poreuse du type membrane.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que la suspension est appliquée en forme de couche sur un corps de support, de préférence plat, résistant à des températures élevées, qu'elle est séchée et frittée sur celui-ci, puis retirée du corps de support en tant que pièce finie métallique poreuse du type membrane.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce qu'un masque à contours est placé sur le corps de support avant l'application de la suspension.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que la suspension est appliquée sur au moins l'une des parois d'un corps de support métallique tubulaire et séchée, et que la couche de vert ainsi constituée est ensuite frittée solidement sur le corps de support.
  10. Procédé selon la revendication 9, caractérisé en ce que lors de l'application de la suspension et au moins pendant une partie du temps de séchage, le corps de support tubulaire est mis en rotation autour de l'axe de tube.
  11. Procédé selon l'une des revendications 1 à 10, caractérisé en ce que la suspension est appliquée sur le corps de support par coulage en couche mince, pulvérisation ou immersion.
  12. Procédé selon l'une des revendications 1 à 11, caractérisé en ce que, lors de l'application de la suspension, la sortie de suspension est déplacée par rapport au corps de support.
  13. Procédé selon l'une des revendications 1 à 12, caractérisé en ce qu'après frittage la membrane poreuse est calibrée par laminage.
EP98922732A 1998-04-17 1998-04-17 Procede de realisation d'une couche metallique frittee a porosite ouverte Expired - Lifetime EP1073778B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP1998/002254 WO1999054524A1 (fr) 1998-04-17 1998-04-17 Procede de realisation d'une couche metallique frittee a porosite ouverte

Publications (2)

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EP1073778A1 EP1073778A1 (fr) 2001-02-07
EP1073778B1 true EP1073778B1 (fr) 2002-01-30

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US (1) US6652804B1 (fr)
EP (1) EP1073778B1 (fr)
JP (1) JP2002512308A (fr)
KR (1) KR20010041043A (fr)
AT (1) ATE212681T1 (fr)
DE (1) DE59802992D1 (fr)
ES (1) ES2171025T3 (fr)
WO (1) WO1999054524A1 (fr)

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US5592686A (en) * 1995-07-25 1997-01-07 Third; Christine E. Porous metal structures and processes for their production
CA2190238A1 (fr) * 1996-07-15 1998-01-15 Ryutaro Motoki Filtres de metal fritte
EP0852298B1 (fr) * 1996-12-14 2003-03-19 Federal-Mogul Deva GmbH Matériau pour paliers lisses et procédé de fabrication d'un tel matériau

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DE59802992D1 (de) 2002-03-14
JP2002512308A (ja) 2002-04-23
US6652804B1 (en) 2003-11-25
KR20010041043A (ko) 2001-05-15
ATE212681T1 (de) 2002-02-15
WO1999054524A1 (fr) 1999-10-28
ES2171025T3 (es) 2002-08-16
EP1073778A1 (fr) 2001-02-07

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