EP2321077A1 - Corps cru et corps moulé léger en matériau céramique et/ou de poudre métallique et procédé pour produire ce corps - Google Patents

Corps cru et corps moulé léger en matériau céramique et/ou de poudre métallique et procédé pour produire ce corps

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Publication number
EP2321077A1
EP2321077A1 EP09701504A EP09701504A EP2321077A1 EP 2321077 A1 EP2321077 A1 EP 2321077A1 EP 09701504 A EP09701504 A EP 09701504A EP 09701504 A EP09701504 A EP 09701504A EP 2321077 A1 EP2321077 A1 EP 2321077A1
Authority
EP
European Patent Office
Prior art keywords
suspension
suspending agent
ceramic
green body
solidification
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.)
Ceased
Application number
EP09701504A
Other languages
German (de)
English (en)
Inventor
Tassilo Moritz
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.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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 Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Publication of EP2321077A1 publication Critical patent/EP2321077A1/fr
Ceased legal-status Critical Current

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    • 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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1125—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers involving a foaming process
    • 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
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/04—Clay; Kaolin
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • 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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • 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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers

Definitions

  • the invention relates to the fields of powder metallurgy and ceramics and relates to a lightweight green and a molded body of a ceramic and / or powder metallurgical material, such as in vehicle construction, aircraft or mechanical engineering as a filter body, filler, lightweight component, catalyst support, pore burners , Diesel soot filter or depth filter for metallic melts, noise and vibration damper, compression element or lightweight component can be used, and a method for its preparation.
  • Lightweight components are gaining in importance for a variety of designs in vehicle construction, aircraft construction or mechanical engineering for weight reduction. Due to their low density, foam structures are expected to be the lightweight components.
  • foam materials optionally as composite components with dense outer parts, can be achieved by the weight reduction in vehicle construction, a considerable saving in fuel consumption.
  • Metal foams are characterized by a low mass in combination with a high rigidity and a significant mechanical strength. They are used, inter alia, for thermal insulation, for noise and vibration damping or as compression elements, eg. B. used for "CrashT'-absorber.
  • EP 1 288 320 A2 describes a melt metallurgical process in which gas bubbles are introduced into a melt. The size of the bubbles is controlled by the adjustment of the Einströmparameter of the gas.
  • An apparatus for introducing gas into a foamable metal melt by means of a metal foam producing tube in which the size of the respective individual bubbles and the size of the gas bubbles are controlled by geometrical nozzle design and adjustment of the gas inflow parameters into the molten metal in AT 411 532 B.
  • AT 410 103 B describes a method for producing a lightweight molded body, wherein formed from a particle having molten metal by introducing gas or gas mixtures into this a metal foam, this at least partially introduced into a mold and its liquid phase is solidified in this.
  • a method and an apparatus for producing bodies of metal foam are described by a powder metallurgy method in which a PM semi-finished product inserted into an at least two-part mold of metal, ceramic or the like, and the closed mold is heated so far until the semifinished product melts, whereby the propellant incorporated in the PM semifinished product dissociates and gas is released, so that the melt of the matrix metal foams and fills the mold, after which the mold is cooled and the gas permeated by gas bubbles melt into a porous structure of lower specificity Density solidifies.
  • a powder metallurgical process for the production of porous metal bodies is also presented in DE 101 15 230 C2, in which a mixture which comprises a pulverulent metallic material which contains at least one metal and / or one metal alloy and a gas-releasing propellant-containing powder is compacted into a semifinished product.
  • This semifinished product is foamed under the action of temperature, wherein a propellant-containing powder is used, in which the temperature of the maximum decomposition is less than 120 K below the melting temperature of the metal or the solidus temperature of the metal alloy.
  • EP 1 338 661 B1 there is known a method of producing a foamed / porous metal by adding a foaming agent to a molten bath of a metal forming a matrix using a powder of a fluoride-coated carbonate compound as the foaming agent, such that the fluoride may destroy an oxide film covering the matrix metal and carbon dioxide formed by the carbonate compound and forming bubbles may form outside metal oxide shells between the bubbles and the matrix.
  • a process for the production of metal foam from a foamable metal-containing raw material and an effective on heating blowing agent, in particular from a known konnpakt believing mixture of metal powder and propellant powder, with heating to at least the melting or foaming temperature of the raw material and blowing agent is described in DE 197 34 394 C2 presented.
  • gas-releasing blowing agents for producing foams or composite metal foam components is likewise the subject of patents EP 0 804 982 A2, EP 1 392 875 B1, US Pat. No. 5,865,237, DE 11 64 102, DE 197 44 300, DE 101 27 716 A1, DE 199 27 837 C1, DE 100 45 494 C2 and DE 101 04 339 A1.
  • DE 101 31 041 C2 discloses a process for producing a foamed metal structure using a powder supply of metal particles, which comprises introducing the stock of metallic powder particles together with foaming agent particles into a propellant gas to form a gas / particle mixture; spinning the mixture at a critical particle velocity onto a metallic substrate; and simultaneously or subsequently exposing at least the coating on the substrate to a thermal pass that causes expansion of the foaming agent to be activated while the metal particles are softened under the influence of the expanding plastic deformation gases.
  • DE 10 2006 031 213 B3 discloses a process in which the stabilizing particles are produced in the preparation of the foamable starting material in an in situ reaction of molten reactive liquids and a molten metal, the molten metal being the constituents of the submicroscopic particles to be produced or nanoparticles are added at least as a fluoride salt, then mixed and heated above the melting temperature of the mixture components.
  • the molten metal is mixed with solid, granular particles, which are dissolved out after solidification of the melt with solvents and thereby leave behind in the melt cavities.
  • This prior art is z. As described in the following publications: WO 91/03578, WO 92/03582 and WO 92/21475.
  • a disadvantage of this method is that not all metallic or ceramic powder can be foamed with phosphoric acid, and phosphoric acid is not ecologically harmless. A possible uncontrolled release of hydrogen as a result of the reaction between acid and metal powder places further limits on this process.
  • EP 0 558 142 B1 describes a method for producing metallic foams, in which a foam material is metallized by treatment in an electrolytic nickel bath.
  • foam structures disadvantageously always include the presentation of an already created foam structure of a particular material, which is subsequently coated with metal.
  • foam structures are used as pore burners, diesel soot filters, depth filters for metallic melts or catalyst carrier body.
  • Ceramic foams are known methods for the production of ceramic foams via infiltration of a polymer foam with a suspension consisting of dispersed ceramic particles in a liquid such.
  • the polymer foam is burned out during sintering.
  • the ceramic particles form an exact image of the polymer foam.
  • Ceramic foams are also obtained via CVD processes by deposition on reticulated carbon foams.
  • EP 1 117 626 B1 describes a process for the production of synthetic bone material which consists of a large-pore foam ceramic whose open foam structure has pores with a modal diameter of> 100 ⁇ m. The method comprises:
  • a ceramic slurry containing a substantially homogeneous mixture of a particulate ceramic, an organic binder in a liquid carrier material and optionally one or more surfactants, wherein at least one of the surfactants is present, if the organic Binder does not function as a surfactant;
  • WO 03/008357 A2 works with an inorganic material, a metal powder or a metal paste, wherein in an aqueous ceramic mass a direct reaction with gas formation between the minerals (eg kaolinite) and the metal powder (eg. Aluminum) expires.
  • the pore formation process takes place at room temperature or at higher temperatures in about 2 to 60 minutes.
  • the resulting porous green compact is dried in the mold or using microwaves.
  • Another known method for producing an open-cell foam ceramic is the direct foaming by a blowing agent (product sheet foaming agent W 53 FL., Zschimmer & Schwarz GmbH & Co., Lahnstein). For this purpose, first a suspension of ceramic particles and water or a solvent is prepared.
  • this suspension a blowing agent and polymer components are added, then this suspension is poured into a mold and started the reaction of the blowing agent. This reaction leads to the development of gas bubbles, which lead to foaming of the suspension. Subsequently, the polymer components are crosslinked, whereby the foam solidifies. The polymer components are then burned out and the remaining foam is sintered.
  • the disadvantage of this method is that the foaming is difficult to control.
  • foam ceramic by direct foaming by means of air WO 97/45381.
  • a polymer component is added to a suspension of ceramic particles and water or a solvent.
  • air bubbles are introduced into the suspension by a high-speed special stirrer.
  • the foamy suspension is then introduced into a mold, and by crosslinking the polymer component, the foam solidifies.
  • the polymer component is burned out and the foam is sintered.
  • the object of the present invention is to provide a lightweight green and a molded body of a ceramic and / or powder metallurgical material, which has high mechanical strength and an adjustable pore structure and further in specifying a method for its preparation, with the lightweight green and molded body inexpensive and ecologically advantageous in a simple manner can be produced.
  • the lightweight green body according to the invention of a ceramic and / or powder metallurgical material consists of an at least highly porous structure of three-dimensionally interconnected webs, which consists entirely of ceramic particles and / or metal particles and optionally from binder particles and known excipients and additives for the sintering of ceramic and or powder metallurgy materials, wherein no materials for generating the at least high porosity are present, and wherein the webs have the solidification structures of a sublimated suspending agent.
  • the lightweight, highly porous material is a foam.
  • Ceramic materials are alumina, zirconia, mixed oxides, aluminum nitride, silicon nitride, silicon carbide, magnesia, silica, porcelain, molybdenum, steatite, cords, or other siliceous materials.
  • binders organic temporary binders are present, which are still advantageously starch, polysaccharides, celluloses and cellulose derivatives, acrylates, polyvinyl butyral, polyvinyl alcohol, polyethylene glycol or sugars are present.
  • glass powders, oxides or oxide mixtures, carbon-supplying organic compounds are present as known auxiliaries and additives. It is also advantageous if, in the case of water as suspending agent, the webs of the green body have the structures of the sublimated ice crystals.
  • the webs of the green body have the structures of the gel structure.
  • the green body can be processed by means of physical and / or chemical methods.
  • the green body can be processed by means of mechanical methods.
  • the inventive lightweight molded body of an at least highly porous ceramic and / or powder metallurgical material consists of an at least highly porous structure of three-dimensionally interconnected webs, which consist entirely of a sintered ceramic and / or powder metallurgical material and substantially no pores and / or cavities, wherein there are no cracks, voids and pores of removed materials to produce the at least high porosity.
  • the three-dimensionally interconnected webs made of alumina, zirconia, mixed oxides, aluminum nitride, silicon nitride, silicon carbide, magnesium oxide, silica, porcelain, molybdenum, steatite, cordierite or other silicate materials.
  • the three-dimensionally interconnected webs made of steels, titanium, aluminum or iron.
  • the density of the three-dimensional interconnected sintered web material > 80% of the theoretical density.
  • a suspension of at least one ceramic and / or powder metallurgical material made from at least one binder and optionally from known auxiliaries and additives for the sintering of ceramic and / or powder metallurgical materials and from at least one suspending agent, wherein a suspending agent is used, which below the melting temperature of the ceramic and / or subliming powder metallurgical materials, subsequently either exposing the suspension to a vacuum until at least solidification / solidification / freezing of the suspending agent, or exposing the suspension to a temperature reduction until complete solidification / solidification / freezing of the suspending agent, then the solidified / solidified / frozen suspension of a suspension Pressure reduction is subjected to a negative pressure, wherein during the pressure reduction, the temperature is increased to the melting point of the suspending agent at the respective pressure, then the suspension to the negative pressure to min first, to solidify / solid
  • the ceramic materials used are alumina, zirconium oxide, mixed oxides, aluminum nitride, silicon nitride, silicon carbide, magnesium oxide, silicon oxide, porcelain, molybdenum, steatite, cordite or other silicate materials.
  • organic, temporary binders are used as binders.
  • starch, polysaccharides, celluloses and cellulose derivatives, acrylates, polyvinyl butyral, polyvinyl alcohol, polyethylene glycol or sugars are used as organic, temporary binders.
  • glass powders, oxides or oxide mixtures, carbon-supplying organic compounds are used as known auxiliaries and additives.
  • suspension is introduced into a vacuum chamber or a freeze dryer.
  • suspension is simultaneously exposed to a negative pressure and temperatures below the solidification pressure and the solidification temperature of the suspending agent.
  • the solidified suspension is heated to the sublimation temperature of the suspending agent or slightly above it.
  • the sublimated suspending agent is completely removed from the green body and its spatial environment.
  • the suspension is poured into a mold and exposed to the negative pressure in this form, and subsequently the suspending agent is sublimated from the solidified suspension in the mold and removed.
  • the solidified suspension undergoes physical or chemical processing prior to sublimation.
  • the viscosity of the suspension controls the size and distribution of the pores or cells between the webs, with a higher-viscosity suspension having a smaller size and distribution of the pores or cells between the webs.
  • a green body of a ceramic and / or powder metallurgical material consists of an at least highly porous structure of three-dimensionally interconnected webs, which consists entirely of ceramic particles and or metal particles and optionally of binder particles and known excipients and additives for the sintering of ceramic and / or powder metallurgical materials, wherein no materials for producing the at least high porosity are present, and wherein the webs have the solidification structures of a sublimed suspending agent, at temperatures is sintered below the melting temperature of the ceramic and / or powder metallurgical materials.
  • the lightweight green and form body according to the invention have a structure of open and closed pores or cells, which are formed by the webs.
  • the webs are made of a ceramic and / or powder metallurgical material, wherein the green body still binder and / or auxiliaries and additives for the sintering of the materials may be present.
  • the lightweight green and molded articles of the invention consist of a foamed or porous body having a specific mass of from 10 to 90% of the pure material having a plurality of closed, isolated or open, partially interconnected, generally spherical pores or cells or a combination of two pore types with pore sizes in the range of 10 microns to 10 mm, wherein all these pores or cells are formed by the webs. These pores are not the pores that are in the web material.
  • the lightweight moldings according to the invention differ in that they obtain their final strength via sintering. While the metallic foams have a solidification structure, the structures according to the invention of the shaped bodies show a material-typical sintered structure.
  • the structures according to the invention of the green and shaped bodies have no phosphate binder phases in the microstructure.
  • the structures according to the invention of the green and shaped bodies are characterized by the fact that they have no hollow webs, which represent replicas of the burned-off polymer structures.
  • the structures of the green bodies according to the invention can be distinguished from all other ceramic and metallic foam structures in that the webs of the green bodies have surface features and pores resulting from the solidification of the suspending agent and the often associated crystal growth. These characteristic structures of erosion can be detected, for example, in a scanning electron microscope and give an indication of the genesis of the respective foamed, porous structure (Figs. 1 - 5).
  • Figure 1 Bar of a non-sintered aluminum oxide foam structure with pores of ice crystals
  • Figure 2 Bar of an unsintered aluminum oxide foam structure with pores of ice crystals
  • Figure 3 Bar of a non-sintered aluminum oxide foam structure with pores of ice crystals
  • Figure 4 Bar of a unsintered steel foam structure with pores of ice crystals
  • Figure 5 Bar of a non-sintered Steel foam structure with pores of ice crystals From ceramic and / or powder metallurgical materials is with a
  • Suspending agent and optionally binders and / or auxiliaries or additives for the sintering of the materials produced a suspension having solids contents of> 1 to 98 vol .-%.
  • Such a suspension used according to the invention can be used on the basis of
  • Solid contents have a viscosity of slightly liquid to pasty.
  • the suspension can be stirred advantageously.
  • the amount of introduced air or other gases in the suspension and the viscosity of the suspension can control the number and size of pores or cells formed by the webs.
  • the suspension is filled into molds, hollow component structures or vessels and transferred to a device in which the suspension can be exposed to a negative pressure.
  • a vacuum vessel or a freeze dryer is advantageously advantageously a vacuum vessel or a freeze dryer.
  • the suspension produced while it is subjected to a negative pressure until at least solidification / solidification / freezing of the suspending agent, foamed.
  • the negative pressure By applying the negative pressure, the air or other gases inevitably present in the suspension is removed / sucked out of the suspension.
  • the suspension foams up and results in a lightweight highly porous structure up to a foam structure.
  • the foaming of the suspension can also be achieved by advantageously solidifying / solidifying / freezing the suspension in a mold, a hollow component structure or a vessel.
  • This solidified / solidified / frozen suspension is then subjected to a reduced pressure, whereby the solidified / solidified / frozen suspension is heated above the melting temperature of the suspending agent.
  • the suspension can foam again.
  • a balance between pressure and temperature is again achieved, so that the foamed suspension is then solidified / solidified / frozen again.
  • the sublimation of the suspending agent is carried out and the green body is produced.
  • the suspension of the ceramic and / or metallic powders with a gel-forming substance such as colloidal or polymeric sols, agar or gelatin are added.
  • a negative pressure to the suspension during the evacuation of the vessel, the formation of bubbles in the suspension, which leads to the inventive lightweight porous to foamed structure.
  • the ambient pressure for example to pressures ⁇ 600 Pa
  • the equilibrium conditions are achieved, which causes solidification / solidification / freezing of the structure.
  • the gel formation causes an additional solidification of the structure.
  • the solidified / solidified / frozen foam is then subjected to sublimation conditions and the suspending agent is removed to form the green body.
  • the foam structure according to the invention can also be removed from the vacuum vessel after solidification / solidification / freezing under ambient pressure and warmed to room temperature.
  • the foamed or porous structure is not yet dried at this time, and the pore space between the lands is filled with the suspending agent, preferably water or solvent, the resulting gel imparts solid properties to the molding.
  • the residual moisture can now be removed from the structure by conventional drying methods, such as evaporation or evaporation drying, whereby the green body according to the invention is formed.
  • the green body according to the invention is subsequently subjected to a sintering process which leads to the solidification of the ceramic or metallic powder particles and gives the foam structure its final solid-state properties.
  • the suspension can be immediately filled in a mold and these are evacuated, so that the resulting green body is also a molded green body.
  • an aqueous based suspending agent is used.
  • water As suspending agent for the suspension of organic solvents, for.
  • cyclohexane or cyclohexanol As tertiary butyl alcohol, cyclohexane or cyclohexanol use. According to the state diagrams of these solvents compared to that of the water, the properties of vapor pressure, melting point and boiling point then change, which must be taken into account during the process.
  • the solvents used must meet the condition that the pressure in a known device can be lowered below the equilibrium pressure of the melting temperature of the solvent. Only then can the phase transition to the solid be completed. If there is no such device, the solvent can not be used as the suspending agent.
  • the evacuation is carried out in a vacuum vessel or a freeze dryer.
  • the solidification / solidification / freezing of the suspending agent Due to the further lowering of the pressure until solidification / solidification / freezing of the suspending agent, this solidifies / freezes / freezes and the lightweight, highly porous structure until foam structure of the suspension is maintained.
  • the solidification / solidification / freezing of the suspending agent is achieved by the achievement of an equilibrium pressure which corresponds to the temperature at the freezing point of the suspending agent.
  • the solidification / solidification / freezing of the suspending agent is, as it were, the solidification or the freezing of the suspending agent.
  • the solidified or solidified or frozen foamed suspension as a green body can now also be processed by means of physical or chemical processes, wherein care must be taken during this processing that the suspending agent does not melt, ie loses the solidified state.
  • the solidified / solidified / frozen suspending agent of the green bodies according to the invention is sublimated.
  • the pressure and temperature are adjusted so that in any case no liquefaction of the suspending agent can take place and, at the same time, the suspending agent is sublimated as completely as possible.
  • the sublimed suspending agent is removed from the founding body and from its spatial environment. This can advantageously be done in a freeze dryer, from which the gaseous suspending agent is removed by suction.
  • the green body according to the invention can be exposed to the ambient conditions.
  • the sublimation, as well as the foaming and the solidification / solidification / freezing of the suspending agent, can be controlled by pressure and temperature.
  • Solidification / solidification / freezing of the suspending agent and sublimation are known for the suspending agents which can be used according to the invention.
  • the pressure at room temperature is lowered to ⁇ 600 Pa, which corresponds to the triple point of the water.
  • foaming of the aqueous suspension is achieved and, at the same time, the water freezes upon reaching this pressure.
  • the green body with the frozen foam structure is then exposed to a pressure of 4 to 250 Pa.
  • the water sublimates at a shelf temperature of 20 - 25 0 C.
  • the sublimation rate can be increased when the temperature is raised to 40 - 60 0 C. This can be done for example via an additional heat source, eg. B. be supported by a heat radiator, by induction heating, by microwave energy or by a hot plate.
  • customary temporary binders can be added to the suspension.
  • the suspensions can advantageously be added to the Ge Hyundaitician-degrading substances, such as. As glycerol, ethanol, acetone, isopropanol. In this way, a foaming of the suspensions can be achieved even at lower ambient pressures than ⁇ 600 Pa.
  • the green and shaped bodies according to the invention are produced in the highest degree environmentally friendly, since no propellants must be used for gas formation. Furthermore, the method described works very energy-saving, since the production of highly porous to foam structure is not carried out in the melt or by thermal decomposition of the blowing agent, but at temperatures around the freezing point of the suspending agent.
  • the size and distribution of the pores or cells formed by the webs can be adjusted precisely by regulating the pressure and temperature of the suspension.
  • the pore or cell volume can be controlled via the preparation of the suspension, the viscosity of the suspension, the solids content of the suspensions and likewise via the process control of pressure and temperature.
  • the formation of the pores and cells can be abruptly interrupted by the pressure control by solidification / solidification / freezing of the suspension.
  • the foam structures do not require burning out of a polymer for the cell structure or an organic spacer, as cell formers advantageously steam and ceramic full webs can be achieved.
  • a thermal treatment of the material for foaming due to blowing agent decomposition is not required.
  • the shaped bodies are sintered at temperatures below the melting temperatures of the components. This results in no melting phase, whereby the highly porous to foam structure is maintained and on the other hand, no conversion processes of the materials can take place.
  • the invention will be explained in more detail below with reference to several exemplary embodiments.
  • a condenser Dolapix CE64 Zschimmer & Schwarz
  • 10 ml of 15% Moviol solution are added to the suspension.
  • % are introduced into a cylindrical silicone rubber mold (0 25 mm) at room temperature and positioned on the footprint of a freeze dryer (Gamma 20, Martin Christ).
  • the pressure in the vacuum chamber of the freeze dryer is lowered to a pressure of 125 Pa, which corresponds to an equilibrium temperature of the ice of -18 0 C.
  • the suspension is foamed.
  • the surface heater is set to 30 0 C and the freeze-drying started.
  • the lyophilization process is stopped and the dried foam sample removed as a green body.
  • the temporary binder is removed at 500 ° C.
  • the sintering is carried out in air at a heating rate of 3 K / min at 1700 0 C for 1 h hold time.
  • the foamed structure thus obtained has a density of 56% of the density of alumina (3.99 g / cm 3 ).
  • the proportion of open porosity between the webs is 35%.
  • the pressure in the vacuum chamber of the freeze dryer is lowered to a pressure of 125 Pa, which corresponds to an equilibrium temperature of the ice of -18 0 C.
  • the suspension is foamed.
  • the surface heating is set to 30 0 C and the freeze-drying started.
  • the Gefhrertrocknungsvon is terminated and removed the dried foam sample.
  • the temporary binder is removed at 500 ° C.
  • the sintering is carried out in air at a heating rate of 3 K / min at 1700 0 C for 1 h hold time.
  • the resulting foamed structure has a density of 45% of the density of alumina (3.99 g / cm 3 ).
  • the proportion of open porosity between the lands is 48%.
  • the pressure in the vacuum chamber of the freeze dryer is lowered immediately thereafter to 125 Pa.
  • the frozen samples will be frozen by contact with the warmer shelves Melting point of the water heated, causing a foaming of the suspension is effected.
  • the shelf heating is set to 30 ° C and freeze-drying is started.
  • the lyophilization process is stopped and the dried foam sample removed.
  • the removal of the temporary binder was carried out at 700 0 C under Ar atmosphere with 5% H 2 .
  • the sintering is carried out under hydrogen at a heating rate of 3 K / min at 1380 0 C for 1 h hold time.
  • the density of the sintered foam structure is 2.87 g / cm 3 , which corresponds to 36.8% of the theoretical density of steel grade 17-4 at 7.8 g / cm 3 .
  • the proportion of open porosity between the webs is 60%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Composite Materials (AREA)
  • Dispersion Chemistry (AREA)
  • Metallurgy (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention se rapporte au domaine des céramiques, et concerne un corps cru et un corps moulé léger, utilisable par exemple dans la construction de véhicules, et un procédé pour produire ce corps. L'invention porte sur un corps cru et un corps moulé légers présentant des résistances mécaniques élevées et une structure de pores modulable. L'ébauche crue selon l'invention est constitué d'une structure au moins hautement poreuse, formée de brins tridimensionnels reliés les uns aux autres, entièrement composés de particules de céramique et/ou de particules métalliques, ces brins présentant des structures résultant de la solidification d'un agent de suspension sublimé. Le procédé selon l'invention consiste à produire une suspension d'un matériau céramique et/ou d'un matériau de poudre métallique et d'un agent de suspension, à mettre la suspension en dépression jusqu'à durcissement/solidification/gel de l'agent de suspension, puis à sublimer et éliminer l'agent de suspension, de façon à conserver la structure durcie de la suspension.
EP09701504A 2008-01-18 2009-01-13 Corps cru et corps moulé léger en matériau céramique et/ou de poudre métallique et procédé pour produire ce corps Ceased EP2321077A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008000100A DE102008000100B4 (de) 2008-01-18 2008-01-18 Verfahren zur Herstellung eines leichtgewichtigen Grünkörpers, danach hergestellter leichtgewichtiger Grünkörper und Verfahren zur Herstellung eines leichtgewichtigen Formkörpers
PCT/EP2009/050300 WO2009090159A1 (fr) 2008-01-18 2009-01-13 Corps cru et corps moulé léger en matériau céramique et/ou de poudre métallique et procédé pour produire ce corps

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EP2321077A1 true EP2321077A1 (fr) 2011-05-18

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EP (1) EP2321077A1 (fr)
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