EP3541552A1 - Procédé de fabrication d'un corps moulé poreux et corps moulé poreux - Google Patents

Procédé de fabrication d'un corps moulé poreux et corps moulé poreux

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Publication number
EP3541552A1
EP3541552A1 EP19703129.7A EP19703129A EP3541552A1 EP 3541552 A1 EP3541552 A1 EP 3541552A1 EP 19703129 A EP19703129 A EP 19703129A EP 3541552 A1 EP3541552 A1 EP 3541552A1
Authority
EP
European Patent Office
Prior art keywords
temperature
spacer material
green compact
melting
melting temperature
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.)
Withdrawn
Application number
EP19703129.7A
Other languages
German (de)
English (en)
Inventor
Rudolf Zauner
Martin Fink
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.)
Verbund Solutions GmbH
Original Assignee
Verbund Solutions GmbH
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 Verbund Solutions GmbH filed Critical Verbund Solutions GmbH
Publication of EP3541552A1 publication Critical patent/EP3541552A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • 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
    • C04B35/111—Fine ceramics
    • 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
    • C04B35/46—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 titanium oxides or titanates
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal thereof
    • 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
    • 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
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • 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
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0232—Metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0236—Glass; Ceramics; Cermets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0241—Composites
    • H01M8/0243—Composites in the form of mixtures
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • C04B2111/00853—Uses not provided for elsewhere in C04B2111/00 in electrochemical cells or batteries, e.g. fuel cells
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606—Drying
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to a process for producing a porous shaped body with a defined pore size distribution. Furthermore, within the scope of the invention, a molded article produced according to the invention is also specified.
  • powder metallurgical production of metallic products from powders has been an established state of the art for many decades.
  • the main advantage of powder metallurgy compared with conventional melt metallurgical processes is that parts with complicated geometry as well as with high dimensional accuracy and surface quality can be produced quickly in large numbers and with almost 100% material utilization and therefore sustainable.
  • Powder metallurgy products usually differ little from those made by conventional metallurgical processes.
  • the usual way is the residual porosity of powdered materials produced slightly higher, which can lead to a slightly lower strength and toughness of such components, but not necessarily be a disadvantage.
  • powder technology processes such as pressing and sintering, casting (English: type casting) or powder injection molding (English: powder injection molding) are well known. These processes are used, for example, for the production of components of metal or ceramic powders or mixtures thereof, in particular if such components have a complex geometry.
  • US 2014/0211370 Al discloses the preparation of a catalyst electrode.
  • spacer coatings include organic and organic materials, ceramics, epoxy and polymer compounds are to be understood.
  • these spacer coatings are deposited on the electrochemically active sub strat für the anode (English: anode deposition substrates), remain on ferti conditions electrode component as an insulating layer and serve to direct electrical contact between the anode-side substrate layer and the cathode to avoid.
  • a disadvantage of this design is at least that no components with complex Geomet rien can be made. Furthermore, it is not possible to adjust the pore size distribution within the components in the production of such catalyst electro.
  • pore-forming agents for example, oxidizable materials such as graphite, coke and starch-containing materials are mentioned - listed.
  • pore formers with mean particle sizes between 100 nm (nanometers) and 10 ⁇ m (micrometers) can be used in the production of the thin metal layers, the pore formers being removed or burned during the subsequent sintering.
  • a disadvantage of this manufacturing method is at least that so thin only two-dimensional layers Kgs be made by powder metallurgy nen, but not three-dimensional body with complex geometry.
  • a method has become known in which a starting mixture which comprises, inter alia, inorganic particles as a carrier material, a spacer material and an organic binder material is mixed together ver together, then filled into a mold and together in this form is heated, wherein the binder material is melted and thus all components of the starting material are coated with the binder material.
  • document GB 2521 677 A discloses a membrane electrode in which layers of graphene are printed in layers by means of a printing process, preferably with a 3-D printer.
  • the present invention is therefore based on the objective of avoiding the known from the prior art disadvantages of processes for the production of porous moldings and to provide a novel production process, with which it is possible to adjust the porosity of a three-dimensional molded body.
  • a further object of the invention is to be able to produce moldings using the novel production method, which have, for example, sections or zones of zones, which zones have greater porosity than adjacent sections or layers of the same mold body.
  • the production process according to the invention should not be subject to material limitations and generally applicable to sinterable materials, that is to say for metallic and / or ceramic materials.
  • Another object of the invention is to provide a body according to the method produced with a defined pore size distribution, which can be used as a three-dimensional component in fuel cells or electrolyzer cells.
  • a process according to the invention for the production of a porous shaped body comprises at least the following process steps:
  • -A- providing a pulverulent carrier material which comprises at least one metal powder and / or at least one ceramic powder or mixtures thereof;
  • -B- providing a spacer material having a melting temperature of the spacer material
  • -C- providing a low-melting binder material, wherein the melting temperature of the binder material below the melting temperature of the spacer material is selected
  • different powdery carrier materials which comprise at least one metal powder and / or at least one ceramic powder or mixtures thereof, can be used in the production method according to the invention in accordance with method step -A-.
  • a low-melting binder material for coating the spacer material is provided, wherein the melting temperature of the binder material below the melting temperature of the spacer material is selected, so that the particle shape of the spacer material he remains and thus the pore size distribution can be adjusted via the particle size distribution of the spacer material.
  • the coating of the spacer material with the low-melting binder material takes place with the most uniform possible layer thickness.
  • who used for coating (English: Coating), for example, spray coating method.
  • the coating material is applied to the surface of the particles to be coated.
  • the product properties such as the layer thickness, can be specifically influenced and optimized.
  • the particles to be coated are agitated in the fluidized bed and sprayed with the molten coating material.
  • the orders of Beschich tion is expedient at temperatures below the melting temperature of Spacerma terials.
  • a mischag gregat such as a mill or a mixer homogeneously mixed.
  • the further molding of the molding material into a moldable feedstock may be required in order to produce this feedstock in
  • the mixing temperature for further molding the molding material into a moldable starting material can be selected appropriately above the melting temperature of the binder material and below the melting temperature of the spacer material
  • a controlled tempera tion guide is required to first at a low mixing temperature below the melting temperature of the binder material, the molding material h produce, which is then heated at an elevated Mi schungstemperatur with mixing, stirring and / or kneading to a moldable insert material, which then has sufficient plastic properties for use in example in an injection molding process.
  • this process step of producing a moldable feedstock as a template for a casting or injection molding process can also be carried out in a separate, additional shaping unit.
  • the shaping of a green lings from the molding compound is carried out at a plasticizing temperature, which is selected below the melting temperature of the spacer material. If, for example, a plastic material having a melting temperature of approximately 220 ° C. is used as the spacer material, then it is appropriate in such a case if a plasticizing temperature of 100 ° C. to 200 ° C., preferably of 100 ° C. to 200 ° C., for the shaping of a green body from the molding composition 130 ° C to 190 ° C, is selected.
  • a green compact can be formed with "net shape" properties, ie with a complex three-dimensional geometry that exactly corresponds to the predetermined contours of the template body and the device no further Nachbearbei needed.
  • the green compact obtained is cooled after the molding step.
  • the cooling is carried out expediently at ambient tempera ture or at room temperature or ambient temperature.
  • the cold or cooled green compact is subjected to a multi-stage heat treatment process.
  • the cooled green compact is charged into a debindering furnace for removing the binder material - the so-called "debinding" - this is recorded in method step -H- Removal of the binder material the green body is at a first holding temperature below the melting temperature of the spacer material and above the melting temperature of the binder material.
  • a chemical (solvent) debinding can also be carried out before this thermal debinding step.
  • This optional method step -H'- will be discussed in more detail below.
  • the further method steps -I- to -K- which include sintering the green body at a second holding temperature, removing the spacer material at a third holding temperature, and sintering the intermediate product thus obtained into a completely sintered porous shaped body having a defined pore size distribution , are also part of the multi-stage heat treatment process.
  • the successive heat treatment steps are carried out at increasing temperature levels of the successive holding temperatures.
  • the selected sintering temperature which in any case is selected above the holding temperatures, is significantly dependent on the selected starting product of the pulverulent carrier material.
  • the green compact may also be subjected to a multi-stage debinding process, if necessary. It should be noted that the integrity or dimensional stability of the Formkör pers is not adversely affected by the removal of the components.
  • a first chemical debinding step at low temperature with the aid of a solvent or solvent mixture, at- For example, hexane or heptane are removed in wax-based binder systems or water in glycol-based systems, the low-melting binder material.
  • debinding takes around six hours at room temperature for a powder with an average particle size of 15 microns.
  • the chemical Lierestoffentbind réelle he prefers to follow at room temperature, since at elevated temperature, the dimensional stability of her forthcoming molding could suffer due to the too rapid debinding process.
  • the chemical removal of the binder component leads to a shaped body with initial porosity, which is selected by the subsequent thermal debindering at a temperature above the melting temperature of the binder material and below the melting temperature of the spacer material.
  • a reducing eg by supplying hydrogen
  • neutral eg by supplying nitrogen
  • oxidizing eg by supplying air
  • a vacuum atmosphere by evacuation of the binder Entbind ceremoniessapparates example, a binder removal furnace
  • the optional chemical debinding come as a solvent for dissolving out the low-melting binder material - depending on the binder material - for example, orgasmic African solvents such as heptane in question.
  • the green compact is preferential, at temperatures between 25 ° C and 60 ° C for a period of about 4 to 8 hours in a solvent bath and then exemplified at temperatures between tween 25 ° C and 60 ° C for a period of 0 , Dried for 5 to 2 hours to remove solvent residues.
  • the periods of time for the chemical dissolution of the binder material may also be rejected from these periods of time mentioned by way of example.
  • organic solvents such as heptane as a solvent for the dissolution of the spacer material in question.
  • water-soluble spacer material for example, water can be used as a solvent.
  • the previously debetted green compact at temperatures, for example, from 25 ° C to 60 ° C currency rend a period of about 4 to 8 hours in a corresponding solvent bath is immersed and then at temperatures, for example, from 25 ° C to 60 ° C while egg ner Drying time of 0.5 to 2 hours dried.
  • the spacer material is not a plastic or plastic mixture, but for example, an oxide-ceramic powder is used with a significantly higher melting temperature than plastic, the following applies:
  • the high sintering temperatures can be used as a spacer material, for example, an oxide ceramic powder such as alumina Al2O3 or silica S1O2 or zirconia ZrCh.
  • the procedure can be carried out in such a case until the process step -I- same as when using plastic as a spacer material. Thereafter - that is, after the step -I- and the Ansintern the already at least partially debetted green compact - takes place in this case, advantageously, a cooling of the sintered green compact to ambient temperature or at room tempera ture.
  • the cooled, sintered green compact is subsequently immersed in a solvent bath which has, for example, a strongly alkaline solution, for example sodium hydroxide solution or potassium hydroxide solution or mixtures thereof, as the solvent.
  • a detachment of the spacer material - for example of oxide ceramics - takes place.
  • the green compact is in the solvent bath, which, for example, sodium hydroxide solution or potassium hydroxide solution or mixtures thereof from, expediently for about 3 to 8 hours.
  • the time periods for the chemical detachment of the spacer material from these exemplary periods of time may also be rejected. This is followed by process step -J-.
  • the pulverulent carrier material may contain particles having a particle size of from 0.1 ⁇ m to 300 ⁇ m, preferably from 1 ⁇ m to 150 ⁇ m, particularly preferably from 5 mm to 50 mm. wherein the particles are present in a defined particle size distribution.
  • the definition and characterization of the particle size distribution or particle size distribution can be carried out expediently by specifying characteristic particle sizes such as Dio, D50 and D90 or by specifying D50 and the standard deviation of the particle size distribution.
  • the D 50 value here means that 50% of the particles of a heap are smaller than the specified value, which in the case of a spherical particle corresponds to its diameter and, in the case of particles which deviate from the spherical shape, is to be converted into equivalence diameter ,
  • the Dio value of the particle size distribution of a powder means that 10% of the particles of the powder are smaller than the given Dio value.
  • the pulverulent carrier material can also be used with a particle size distribution deviating from the Gaussian distribution, for example with a bimodal or complex particle size distribution.
  • the powdery carrier material used can be, for example, inter alia the following metallic and / or ceramic materials or mixtures thereof: aluminum oxide Al 2 O 3; Aluminum silicate Al 2 O 3 -SiO 2; Aluminum nitride A1N; Bronze Cu-SN; Hard metals and mixtures thereof, for example tungsten carbide-cobalt-hard WC-Co; Copper Cu; Ferritic Materials FesCh; Iron Fe and, for example, iron compounds Fe-Si, Fe-P, Fe-Ni-Co; Molybdenum Mo; Molybdenum-copper Mo-Cu; Nickel Ni; Nickel-iron Ni-Fe; Nickel base alloys Ni-Cr-Mo, silica S1O2; Silicon carbide SiC; Silicon nitride S13N4; Spinel gO-ApO,; Steel of all microstructure and alloy composition such as Fe-C, Fe-C-Cu, Fe-Ni-C, Fe-Cr-Ni (stainless), Fe-Co-Cr-WVC
  • powdery support materials As manufacturing methods for such powdery support materials come example, methods comprising gas atomization, water atomization, oxide reduction, Plasma atomization, precipitation, CVP (chemical vapor deposition), PVD (physical vapor deposition), grinding and / or chemical production via one or more chemical reactions in question.
  • gas atomization water atomization, oxide reduction, Plasma atomization, precipitation, CVP (chemical vapor deposition), PVD (physical vapor deposition), grinding and / or chemical production via one or more chemical reactions in question.
  • CVP chemical vapor deposition
  • PVD physical vapor deposition
  • the shape of the pulverulent carrier material can also influence the packing density as well as the range of the adjustable porosity of the starting material or of the porous shaped body to be produced.
  • packing densities of up to 64% can be achieved.
  • packing densities of the pulverulent carrier material of up to 68% can be achieved.
  • packing densities of only around 50% are achieved.
  • a spacer material can be used in a production process, which contains a powdered plastic or a plastic mixture, wherein the melting temperature of the spacer material from 100 ° C to 350 ° C, preferably from 150 ° C to 250 ° C, is.
  • Suitable spacer materials are, for example, powders with low sintering activation and low sintering temperature.
  • polyolefins such as polypropylene PP (with a melting temperature of about 150 ° C.) or polyethylene PE (melting temperature of about 170 ° C.) or mixtures thereof can be used as spacer materials in the context of the production process according to the invention.
  • other plastics such as polystyrene (with a melting temperature of about 180 ° C) come into question.
  • plastics with a higher melting point can be selected as suitable spacer materials such.
  • Teflon ® PTFE (with a melting temperature of about 325 ° C) or polyamides (with melting temperatures greater than 200 ° C).
  • a spacer material such as polyvinylbutrial or methyl cellulose.
  • Spacermate materials have the advantage of becoming glassy before the viscosity drops significantly when heated.
  • the melting point or the melting temperature of the selected spacer material is crucial for the further temperature guidance during debinding and presintering.
  • the spacer material may comprise a powdery oxide ceramic or an oxide ceramic mixture.
  • a spacer material offers the advantage that carrier materials with low sintering activity, which require high sintering temperatures, for example sintering temperatures above 1000 ° C., can also be processed with the production method according to the invention.
  • oxide ceramic powders such as aluminum oxide Al 2 O 3, silicon oxide SIO 2 or zirconium oxide ZrCE can be used as the spacer material.
  • the melting temperature of the spacer material can advantageously also be above the sintering temperature of the carrier material.
  • the spacer material is removed in such a case according to the method step by chemical removal of the spacer material using at least one solvent or solvent mixture.
  • a binder mate rial be used, which binder material contains a low-melting wax and / or a low-melting organic compound or mixtures thereof, wherein the melting temperature of the binder material of 30 ° C to 100 ° C, preferably of 50 ° C. up to 80 ° C, is.
  • the low-melting binder component may be, for example, a paraffin wax having a melting temperature between 50 ° and 60 ° C.
  • a paraffin wax having a melting temperature between 50 ° and 60 ° C.
  • carnauba wax having a melting temperature of about 80 ° C
  • stearic acid with a melting temperature of about 75 ° C
  • other low-melting and non-toxic organic compounds such as glycols, or mixtures thereof.
  • such binder components can be removed thermally and / or chemically in later process steps.
  • the coated Spa cermaterial a volume fraction of the spacer material of 70% to 95% and a Volu share of the binder material from 5% to 30% include.
  • the composition of the coated spacer material can be, for example, 70% polypropylene, 20% paraffin wax, 10% stearic acid.
  • the coating of the spacer material with the low-melting binder material as a coating material takes place with the most uniform possible layer thickness of the spacer core particles to form a coated spacer material.
  • mixed gashates such as fluidized bed spray coater.
  • the coating should at temperatures below the melting temperature of the low melting binder material conditions suc conditions.
  • the particle size distribution of the spacer material determines the porosity distribution to be set and should preferably be in the same or similar size range as those the powdered carrier material in order to ensure the most homogeneous possible mixing with similar surface ratios.
  • an undesired agglomeration of carrier material and coated spacer material can be minimized.
  • the mixing temperature for mixing the pulverulent carrier material with the spacer material coated is selected to a molding compound below the melting temperature of the binder material.
  • This type of premix is suitable, for example, for uniaxial pressing and sintering processes for the production of green shapes with simple geometry as well as green shapes for "net shape” shaped bodies with complex geometries Room temperature or at a pressing temperature below the melting temperature of the spacer material.
  • the mixing temperature for forming the molding compound is therefore kept below the melting temperature of the binder material so that the shape of the spacer particles is retained, since these determine the later pore size distribution of the porous molding to be produced.
  • V ersion in a procedural the mixture temperature for the further molding the molding material to a moldable feedstock above the melting temperature of the binder material and below the melting temperature of the spacer material ren be selected.
  • the mixed molding material in the case of the production of moldings with a complex geometry, so-called complex "Netshape" shaped bodies, it may be necessary for the mixed molding material to be further processed into a moldable feedstock so that this feedstock can continue to be injection molded or cast
  • the mixing temperature for further molding the molding material into a moldable starting material can be selected appropriately above the melting temperature of the binder material and below the melting temperature of the spacer material. gregat as the mixing of the molding material done.
  • this process step of producing a moldable feedstock as a template for a casting or injection molding process can also be carried out in a separate, additional shaping aggregate.
  • the shaping of a green compact from the molding composition can be carried out by a casting process, preferably by an injection molding process, more preferably by a multi-component injection molding process.
  • the molding compound is heated to a so-called moldable feedstock after mixing in a plasticizing unit such as an extruder or a kneader at a temperature of 100 ° C. for 10 to 30 minutes further processed.
  • a plasticizing unit such as an extruder or a kneader
  • the moldable feed corresponds to the molding compound.
  • additives containing surface-active substances such as phthalates (for example dimethyl phthalate), acrylates (for example ammonium polyacrylate) or olefin sulfonates may be added.
  • typical injection molding temperatures may be between 130 ° and 190 ° C., typically at 150 ° C.
  • the injection pressure in the injection molding process can range between 1.5 and 60 MPa, typically 30 MPa.
  • the mold temperature of the injection mold is, for example, between the room temperature and 70 ° C, but typically at room temperature.
  • the product-contacting parts of the extrusion and plasticizing unit of the injection molding apparatus and the injection molding tool are expediently designed with a wear-resistant coating.
  • a homogeneously mixing mixing unit are selected to give a homogeneous molding composition for producing a green compact having a homogeneous pore size distribution to it for mixing the powdered carrier material with the coated Spacermate-.
  • a homogeneous mixing mixing unit for example, a mill or mixer such as extruders or batch kneaders can be used, which are operated depending on the task in example continuously or semi-continuously.
  • V of the invention ersion can drive at a Ver for mixing the powdered carrier material with the coated spacer material is a means of separating acting separating unit are selected to obtain a inhomo gene molding composition for producing a green compact with a locally different pore size distribution.
  • separator acting mixing unit for example, a separator, centrifugal mixers, cyclone or a centrifugal casting plant can be used.
  • a separating mixing unit leads to a desired segre gation between the powdery carrier material and the coated spacer material, for example, by density differences between the carrier material and spacer material are utilized, in order subsequently to lead to a graded pore size distribution.
  • This can be advantageous if the sintered porous end product should exhibit this property of a pore size distribution with a sectionwise and / or layerwise gradient, in order to specifically control, for example, the residence time of educts and products in chemical reactions.
  • surface-active substances in a small volume fraction of from 0.1 to 2%, preferably of 0.5%, can be added to the molding composition.
  • Surface-active substances reduce the interfacial tension of two phases - in this case the interfacial tension between the support material and the coated spacer material - and cause these two materials to remain finely mixed and the support material to be easier to deagglomerate.
  • a porous shaped body having a defined pore size distribution wherein the porous shaped body is a sintered shaped body and at least one section, preferably at least one layer, with a material adjacent thereto having changed Po has porosity, wherein the pore size distribution of the shaped body of the particle size distribution of the spacer material used corresponds.
  • a porous shaped body produced by the process according to the invention may advantageously have local areas in its structure, which in sections - or preferably in layers - has a changed porosity.
  • the term "changed porosity" is understood to mean a relative difference in porosity of a region or section of the molded article in relation to another region or section of the same shaped article.
  • a first section or a first layer of the shaped body may have a first porosity
  • a second section adjacent thereto or a second layer of the shaped body has a second porosity which is different from the first porosity.
  • a section having a first porosity or a first pore size distribution may, for example, have a greater or a smaller degree of pincer than another, second section having a second porosity or a second pore size distribution.
  • the boundaries between the regions or sections with altered or different porosity can be precisely delimited, for example, depending on the intended use of the porous body.
  • such sections or layers can be produced with locally different or changed porosity, for example in an injection molding process by the use of an injection molding device with more than one plasticizing unit - the so-called Multi-component injection molding.
  • plasticizing units can be filled in each case with different starting materials, which can then be metered into the cavity of the injection molding apparatus by sequential injection. By sequential release of the cavity in the injection mold, the areas with different material properties can be precisely defined.
  • injection moldings or green ling and subsequently porous moldings with local or layered different porosity can be produced.
  • a porous shaped body produced according to the invention can be used as a gas diffusion layer of an electrolyzer or a fuel cell.
  • a porous shaped body according to the invention in so-called membrane electrode assemblies (MEA) of electrolysers or fuel cells, which consist of porous layers and where reaction site and rate, educt / product flow and removal must be influenced by porosity be used.
  • MEA membrane electrode assemblies
  • the shaped body may comprise at least one sintered material selected from the group consisting of titanium, titanium alloys, acid-resistant oxide ceramics, aluminum oxide and / or zirconium oxide. Such sintered materials are sintered at comparatively high temperatures, for example, from 1400 ° C. to 1700 ° C.
  • FIGS. 2A to 2C individual feedstocks, in FIG. 2D a molding compound as the first mixture product, in FIG. 2E a green compact, and in FIG. 2F a completely sintered porous shaped body;
  • FIG. 3 shows a temperature profile of a first method variant according to the invention
  • - Fig. 4 is a temperature profile of a second method V ersion according to the invention, wherein a combined thermal and chemical removal of the binder material is provided; such as - Figure 5 is a temperature profile ⁇ a third method V ersion according to the invention is seen in which a combined thermal and chemical removal of the spacer material before.
  • FIG. 1 is a schematic process flow diagram of an inventive method with the following method steps -A- to -K-:
  • a pulverulent carrier material 10 which comprises at least one metal powder and / or at least one ceramic powder or mixtures thereof.
  • a spacer material 20 having a melting temperature Ts, 2o of the spacer material 20 is provided.
  • a plastic material is used as the spacer material 20, which has a melting temperature Ts, 2o of 200 ° C.
  • a low-melting binder material 30 is provided, where at the melting temperature Ts, 3o of the binder material 30 below the melting tempera ture Ts, 2o of the spacer material 20 is selected.
  • a wax is used as the binder material 30, which has a melting temperature Ts, 3o of 70 ° C.
  • the spacer material 20 is coated with the low-melting binder material 30, wherein a coated spacer material 40 is obtained.
  • the Be coating is carried out expediently at a coating temperature TB, 4O above the melting temperature Ts, 3o of the binder material 30 - here in the example so at a Beschich processing temperature T B, 4 O just above 70 ° C, for example at 80 ° C, and well below the melting temperature Ts, 2o of the spacer material 20 of 200 ° C.
  • a fluidized bed spray coater is used here.
  • the beschich ended spacer material 40 includes, for example, a volume fraction of the spacer material 20 of 80% and a volume fraction of the binder material 30 of 20%.
  • the mixing of the powdery carrier material 10 with the already coated spacer material 40 takes place to form a molding compound 50 in a Mischag gregat at a mixing temperature TM, 5O.
  • the mixing temperature TM, SO for mixing the carrier material 10 with the coated spacer material 40 to the molding compound 50 is here selected below the melting temperature Ts, 3o of the binder material 30 and is for example 50 ° C. This prevents that the wax coating of the coated spacer material 40 chosen here as an example begins to melt and the coated spacer material agglomerates.
  • the already mixed molding compound 50 can also be further shaped even at an increased mixing temperature to form a moldable feedstock, for example for use in an injection molding process.
  • the mixture temperature can also be selected above the melting temperature Ts, 3o of the binder material 30 and below the melting temperature Ts, 2o of the spacer material 20.
  • At least one additive 45 may be added to the molding compound 50. This option is illustrated in FIG. 1 by a dashed arrow 45.
  • process step -F- is the shaping of a green compact 60 from the molding compound 50 at a plasticizing temperature T p, 6 o, which is below the melting temperature Ts, 2o of the spacer material 20 is carried out.
  • a plasticization temperature T p, 6 o of 150 ° C. is chosen for the starting materials exemplified here.
  • process step -G- then the cooling of the green compact 60 to ambient temperature Tu, 6o or room temperature.
  • the binder material 30 of the green compact 60 is thermally removed at a first holding temperature TH, 70.
  • the green compact 60 is charged, for example, in a debinding furnace, whereby a green compact 70 with at least partially removed binder material 30 is obtained.
  • the first holding temperature TH, 7O is to below the melting temperature Ts, 2o of the spacer material 20 and above the melting temperature Ts, 3o of the Bin dermaterials 30 selected.
  • the first holding temperature TH, 7O is selected, for example, at 190 ° C.
  • a chemical removal of the binder material 30 is used carried out at least one solvent or solvent mixture.
  • the green compact 60 is immersed in a solvent bath (eluted) for at least one hour at a solvent temperature T L, 70 ° C. and then dried, before it is left green with 70 'already chemically removed binder material according to process step -H - Ther is debindered mixed.
  • the solvent removal is carried out for example at a solvent temperature T L, 7 O of 25 ° C for a period of 6 hours before the green compact 70 'is then dried for one hour at 25 ° C.
  • T L solvent temperature
  • step -H'- are the green compact in Fig. 1 60, which is supplied to the solvent bath, and the chemically debonded green compact 70 ', which is then thermally debinded in process step -H-, each symbolized by dashed arrows.
  • step -I- the sintering of the at least partially debinded green body 70 is performed at a second holding temperature T H, so, the second holding temperature T H, so above the melting temperature Ts of the spacer material 20 as well as above the first holding temperature T H, 7 O is selected.
  • a sintered green compact 80 is obtained.
  • the second holding temperature T H for example at 500 ° C., is selected for the sintering.
  • the thermal removal of the spacer material 20 from the sintered green compact 80 then takes place at a third holding temperature TH, 9O, wherein the third holding temperature TH, 9O above the second holding temperature TH, is selected here and here, for example 650 ° C is selected.
  • a third holding temperature TH, 9O above the second holding temperature TH, is selected here and here, for example 650 ° C is selected.
  • an intermediate product 90 having at least partially removed spacer material 20 is obtained.
  • the green compact 80 in accordance with method step -I-) and before ther mixing removal of the spacer material 20 (according to method step -J-) in a further, optional process step additionally chemical removal of the spacer material 20 is carried out using at least one solvent or solvent mixture.
  • the sintered green compact 80 can be eluted at a solvent temperature TL, 9O of 10 ° C to 80 ° C for at least one hour in a solvent bath and then dried. For example, this chemical removal of the spacer material in the solvent bath at a solvent temperature TL, 9O of 35 ° C for a period of 6 hours take the.
  • the intermediate product 90 ' in which already the Spacermate rial was removed by elution chemically, for example, dried for one hour at 35 ° C.
  • the sintered green compact 80 fed to the solvent bath and the intermediate product 90 ', which is subsequently thermally freed of remaining spacer material in process step -J-, are each symbolized by dashed arrows.
  • the sintering of the intermediate product 90 takes place at a sintering temperature Ts, 100, which is selected above the third holding temperature TH, 9O, to form a porous shaped body 100 with a defined pore size distribution.
  • the pore size distribution corresponds to the particle size distribution of the spacer material 20 used.
  • Ts, 100 example, for example, a temperature of about 800 ° C under hydrogen atmosphere while maintaining a holding time of one hour for the carrier material copper selected.
  • FIG. 2 shows in FIG. 2A a possible powdery carrier material 10 which is suitable for use in the method according to the invention, for example copper.
  • FIG. 2B shows a possible spacer material 20, namely polyamide or silicon oxide.
  • Figure 2C shows a possible low melting binder material 30 suitable for use in the method of the invention, for example a wax-stearic acid mixture.
  • FIG. 2D shows a molding compound 50 as a first mixture product of the pulverulent carrier material 10 with the previously prepared coated spacer material.
  • a green compact 60 is illustrated as molded from the molding compound 50 in a molding step.
  • FIG. 2F shows a completely sintered porous shaped body 100.
  • Fig. 3 shows a temperature course of a first method V variant according to the invention.
  • the shaping of a green body 60 from the molding compound 50 takes place at a plasticizing temperature T p, 6 o of 150 ° C.
  • the heating of the molding compound 50 to the selected plasticizing temperature T p, 6 o takes place here scho nend for two hours.
  • step -G- the rapid cooling of green body 60 to ambient temperature Tu, 6 o, takes place here, for example, at 20 ° C.
  • procedural step -H- the binder material 30 of the green compact 60 is thermally removed at a first tempering temperature TH, 70 of 190 ° C.
  • the green compact 60 is charged in a debinder oven for about two hours.
  • a chemical removal of the binder material 30 is used carried out at least one solvent or Fösungsmittelgemisches.
  • the green compact 60 is immersed (eluted) in a solvent bath for six hours at a solution medium temperature T L, 70 of 25 ° C. and subsequently dried at 25 ° C.
  • ther mix is debindered.
  • the sintering of the at least partially debinded green compact 70 takes place according to method step -I- at a second holding temperature TH, which is selected here at 500 ° C., for example.
  • the thermal removal of the spacer material 20 then takes place from the sintered green compact 80 at a third holding temperature TH, 9O, which is selected here, for example, at 650 ° C.
  • a chemical removal of the spacer material 20 is carried out using at least one solvent or solvent mixture.
  • a solvent temperature TL, 9O of 35 ° C and a elution time of 6 hours is selected.
  • the intermediate product 90 ' in which the spacer material has already been removed by elution chemically, for example, dried for one hour at 35 ° C.
  • the sintering of the intermediate product 90 takes place at a sintering temperature Ts, 100, which is here selected in each case at around 800 ° C. under a hydrogen atmosphere in compliance with a holding time of one hour for the carrier material copper.
  • Tu 6 o ambient temperature; eg room temperature

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Abstract

L'invention concerne un procédé de fabrication d'un corps moulé poreux (100) dont les étapes de procédé consistent au moins : -A- à préparer un matériau porteur (10) en poudre, lequel comprend au moins une poudre métallique et/ou une poudre céramique ; -B- à préparer un matériau d'entretoise (20) ; -C- à préparer un matériau liant (30) à faible point de fusion dont la température de fusion (Ts, 30) est sélectionnée en dessous de celle (Ts, 20) du matériau d'entretoise (20) ; -D- à recouvrir le matériau d'entretoise (20) du matériau liant (30) ; -E- à mélanger le matériau porteur (10) au matériau d'entretoise (40) recouvert de manière à ce qui'ils forment une masse de moulage (50) ; -F- à fabriquer par formage un comprimé cru (60) à partir de la masse de moulage (50) à une température de plastification (Tp, 60) inférieure à la température de fusion (Ts, 20) du matériau d'entretoise (20) ; -G- à refroidir le comprimé cru (60) ; -H- à éliminer le matériau liant (30) du comprimé cru (60) à une première température de maintien (TH, 70) ; -I- à fritter partiellement le comprimé cru sans liant (70) à une deuxième température de maintien (TH, 80) ; -J- à éliminer le matériau d'entretoise (20) du comprimé cru partiellement fritté (80) à une troisième température de maintien (TH, 90) ; -K- à fritter complètement le produit intermédiaire (90) à une température de frittage (Ts, 100) en un corps moulé (100) dont la répartition de taille de pores définie correspond à la répartition de taille de particules du matériau d'entretoise (20).
EP19703129.7A 2018-02-12 2019-02-12 Procédé de fabrication d'un corps moulé poreux et corps moulé poreux Withdrawn EP3541552A1 (fr)

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EP18156319.8A EP3524375A1 (fr) 2018-02-12 2018-02-12 Procédé de fabrication d'un corps moulé poreux ainsi que corps moulé poreux
PCT/EP2019/053392 WO2019155078A1 (fr) 2018-02-12 2019-02-12 Procédé de fabrication d'un corps moulé poreux et corps moulé poreux

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CN113909498B (zh) * 2021-10-12 2023-09-01 南方科技大学 一种多孔材料及其制备方法与应用
CN116949309B (zh) * 2023-09-20 2023-12-01 江苏美特林科特殊合金股份有限公司 一种制备多孔高温合金的方法

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US9079136B2 (en) 2009-05-21 2015-07-14 Battelle Memorial Institute Thin, porous metal sheets and methods for making the same
US20140211370A1 (en) 2013-01-25 2014-07-31 Ionova Technologies, Inc. Electrochemical Cell, Related Material, Process for Production, and Use Thereof
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