EP3041626A2 - Powdered metal component - Google Patents
Powdered metal componentInfo
- Publication number
- EP3041626A2 EP3041626A2 EP14777485.5A EP14777485A EP3041626A2 EP 3041626 A2 EP3041626 A2 EP 3041626A2 EP 14777485 A EP14777485 A EP 14777485A EP 3041626 A2 EP3041626 A2 EP 3041626A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- component
- pores
- powder
- oxide inclusions
- area
- 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- Withdrawn
Links
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G5/00—Incineration of waste; Incinerator constructions; Details, accessories or control therefor
- F23G5/32—Incineration of waste; Incinerator constructions; Details, accessories or control therefor the waste being subjected to a whirling movement, e.g. cyclonic incinerators
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F1/09—Mixtures of metallic powders
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
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- 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
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
- B22F3/162—Machining, working after consolidation
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/007—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of moulds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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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
- C04B7/00—Hydraulic cements
- C04B7/36—Manufacture of hydraulic cements in general
- C04B7/43—Heat treatment, e.g. precalcining, burning, melting; Cooling
- C04B7/434—Preheating with addition of fuel, e.g. calcining
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- C22C1/08—Alloys with open or closed pores
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- C22C27/06—Alloys based on chromium
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- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23C—METHODS OR APPARATUS FOR COMBUSTION USING FLUID FUEL OR SOLID FUEL SUSPENDED IN A CARRIER GAS OR AIR
- F23C3/00—Combustion apparatus characterised by the shape of the combustion chamber
- F23C3/006—Combustion apparatus characterised by the shape of the combustion chamber the chamber being arranged for cyclonic combustion
- F23C3/008—Combustion apparatus characterised by the shape of the combustion chamber the chamber being arranged for cyclonic combustion for pulverulent fuel
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- F23C—METHODS OR APPARATUS FOR COMBUSTION USING FLUID FUEL OR SOLID FUEL SUSPENDED IN A CARRIER GAS OR AIR
- F23C9/00—Combustion apparatus characterised by arrangements for returning combustion products or flue gases to the combustion chamber
- F23C9/06—Combustion apparatus characterised by arrangements for returning combustion products or flue gases to the combustion chamber for completing combustion
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/2016—Arrangements of preheating devices for the charge
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/2016—Arrangements of preheating devices for the charge
- F27B7/2025—Arrangements of preheating devices for the charge consisting of a single string of cyclones
- F27B7/2033—Arrangements of preheating devices for the charge consisting of a single string of cyclones with means for precalcining the raw material
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- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
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- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D99/00—Subject matter not provided for in other groups of this subclass
- F27D99/0001—Heating elements or systems
- F27D99/0033—Heating elements or systems using burners
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/50—Current conducting connections for cells or batteries
- H01M50/502—Interconnectors for connecting terminals of adjacent batteries; Interconnectors for connecting cells outside a battery casing
- H01M50/521—Interconnectors for connecting terminals of adjacent batteries; Interconnectors for connecting cells outside a battery casing characterised by the material
- H01M50/522—Inorganic material
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- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
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- H01M8/023—Porous and characterised by the material
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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- 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
- Y02E60/10—Energy storage using batteries
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- 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
Definitions
- the invention relates to a powder metallurgical component having a chromium content of at least 80% by weight, pores and / or oxide inclusions being present in the component, and a process for its production.
- the invention further relates to an interconnector for an electrochemical cell obtainable from such a powder metallurgical component and to an interconnector for an electrochemical cell which has a region with a chromium content of at least 80% by weight, pores and / or oxide inclusions being present in the region.
- the invention relates to the use of an interconnector for the production of an electrochemical cell.
- components so-called interconnectors, with high Cr contents are suitable , They can be produced, for example, from Cr-based alloys of the composition Cr5 FeY, as described in EP 0 578 855.
- These components essentially ensure the electrical contacting of the individual electrochemical cells, the guidance of the reaction gases and the separation of the reaction gases of adjacent cells. To ensure the separation of the gas spaces of adjacent cells, the components must have a high gas-tightness or low gas permeability.
- interconnectors in the prior art in a cost effective manner via a powder metallurgical net-shape or near net-shape process technology, which includes the steps Pulveransatzfertigung, powder presses, presintering, optionally a Kalibrierpressen and sintering under reducing atmosphere.
- a powder metallurgical net-shape or near net-shape process technology which includes the steps Pulveransatzfertigung, powder presses, presintering, optionally a Kalibrierpressen and sintering under reducing atmosphere.
- Using currently commercially available Cr powder such interconnectors do not yet have sufficient gas tightness after the sintering process.
- the resulting Cr 2 O 3 or mixed oxides of Cr and Al have a larger volume than the metallic matrix, so that the porosity is closed in the course of the oxidation process. Not all pores are necessarily filled to the core with oxide, but at least an edge layer of about 0.2 mm thickness is closed.
- the resulting Oxide layer on the component surface is removed again in a subsequent process, at least in the area of the electrical contact surfaces, for example by a sandblasting process in order to ensure optimum metallic contact between the electrochemical cell and the interconnector at the start of operation of a fuel cell stack.
- High porosity or even only high porosity components require either high temperature oxidation or very long hold times to form a sufficient amount of oxide inclusion with the major component chromium oxide, especially if large open pores are included in the component. High oxidation temperatures and long hold times are associated with corresponding manufacturing costs.
- a high degree of oxide inclusion results in a change in the desired physical device properties (e.g., coefficient of thermal expansion, thermal conductivity, fracture behavior), as these are increasingly determined not only by the metallic matrix but also by the pore filler. This change can affect the component globally or even only selected component areas, which makes the component inhomogeneous.
- desired physical device properties e.g., coefficient of thermal expansion, thermal conductivity, fracture behavior
- the object of the present invention is therefore to remedy this situation and to provide a powder metallurgical component in which the described disadvantages are reduced.
- the powder metallurgical component should have a low gas permeability, be inexpensive to produce and at the same time be as free as possible of undesirable impurities such as chromium nitrides.
- a powder metallurgical component having a chromium content of at least 80% by weight, wherein in the component at least one Microstructure component from the group pores and oxide inclusions is present, which is characterized in that the number per unit area of the sum of pores and oxide inclusions along a sectional area through the component in at least one area is at least 10,000 per mm 2 .
- pores and / or oxide inclusions are present in the component.
- pores occur that are partially filled with oxide inclusions. Partially filled pores are subsumed under pores below. Partially filled pores are therefore counted as a pore.
- Oxide inclusions can occur in the component due to oxidation of chromium, possibly other metals present and addition of metal oxides. During the oxidation process, it is also possible for other compounds, for example nitrides, to form, which can likewise form part of the oxide inclusions.
- oxide inclusions is therefore to be understood as inclusions whose main constituent (> 50 mol.%) Is metal oxides and which may also contain nitrides in addition.
- the main constituent of the oxide inclusions are preferably chromium oxides, the chromium oxide content preferably being at least 90 mol%.
- such a component has a significantly higher total number of pores and oxide inclusions at approximately the same porosity, so that the pore volume is distributed over more and therefore finer pores.
- the invention is based inter alia on the finding that the pore size has a decisive influence on the component.
- the number of large pores should be as low as possible, since such pores filled with Cr 2 O 3 have a negative influence on the component, for example, in terms of delay or the coefficient of thermal expansion.
- the number of the sum of pores and oxide inclusions along the cut surface is at least 20,000, preferably at least 40,000, more preferably at least 60,000 per mm 2 . In a preferred embodiment, it is provided that the number of the sum of pores and oxide inclusions along the cut surface is at least 90,000 per mm 2 . The larger the number of pores per area before the oxidation process, the more effectively and economically they can be closed by oxidation.
- the chromium content in the range is at least 90% by weight.
- a high chromium content increases the thermal conductivity and thus contributes to a homogeneous temperature distribution in the system.
- a high chromium content lowers the thermal expansion coefficient so that it is better adapted to currently available electrolyte materials such as fully stabilized zirconium oxides.
- the density over the entire component thickness is less than 95% of the theoretical density in the region of the component. In a further embodiment, it may be provided that in the region of the component the density over the entire component thickness is between 70% and 95% of the theoretical density. This value range ensures good mechanical stability of the component.
- the pores and oxide inclusions have an equivalent diameter of not more than 12 ⁇ m at a sectional area in at least one area. This has a positive effect on the mechanical properties of the component and allows a fast closure of the open pores in the course of the oxidation process.
- the invention is based inter alia on the finding that the oxidation process can have a negative effect on the homogeneity of the component with regard to distortion and thermal expansion.
- the oxidation process for closing the pores can be shortened, so that the oxide content is reduced. Therefore, it can be provided in one embodiment that the total oxygen content in this range is ⁇ 20 000 [g of O per 1 g of component.
- the total nitrogen content in this range is ⁇ 2000 pg per 1 g component and / or that the content of Al 2 0 3 ⁇ 500 [ig per 1 g component.
- a low nitrogen content has a positive effect on the properties of the component in use for electrochemical cells in that a lower distortion occurs and the thermal expansion coefficient is uniform over the component thickness.
- the oxygen content increases along the component thickness from the middle to the edges.
- a porous component is produced whose pore size distribution depends essentially on the physical properties of the metal powder, such as the specific surface area, as well as the pressing and sintering conditions.
- the component preferably has at least one of the abovementioned properties, in particular the number of pore / oxide inclusions, size / area of the pores / oxide inclusions or oxygen / nitrogen content in a range which, based on the total volume of the component, is greater than 25 Vol.%, Particularly preferably greater than 75 vol.% Is.
- such a component can be produced by a method described below, so that the method also solves the problem set out above.
- the method comprises the steps:
- the BET surface can be adjusted, for example, by grinding chromium powder or a chromium alloy. Powder batches with BET surface areas of up to 0.5 m 2 / g were used to produce the component. Between step (ii) pressing the powder batch into a compact and step (iv) sintering the compact at 1100 to 1500 ° C, a step (iii) pre-sintering the compact at 600 to 000 ° C may be provided.
- the sintering step and if present also or instead of the pre-sintering step can be carried out under a hydrogen atmosphere.
- a Kalibrierpressvorgang can be provided between the pre-sintering step and the sintering step.
- This Kalibrierpressvorgang can be made at a specific pressure of 500 to 1000 MPa.
- a pressing aid in an amount of 0.1% by weight to 5% by weight, based on the amount of powder added, is added to the powder batch prior to pressing.
- a pressing aid is e.g. a wax in question.
- the oxygen source can be any oxygen source. Studies have shown that it can be selected for example from the group H 2 0, 0 2 , C0 2 or mixtures thereof.
- the pore diameter in particular the maximum pore diameter, can be significantly reduced. This significantly less chromium oxide is formed in the pores of the component in order to achieve the required gas tightness. In the Idealfail, the oxidation process can be completely dispensed with if only closed porosity is present after sintering.
- the insert is provided as an interconnector for an electrochemical cell.
- the interconnector points a chromium content of at least 80 wt.% And pores and / or oxide inclusions, wherein the number per unit area of the sum of pores and oxide inclusions at a sectional area through the interconnector in at least one area is at least 10,000 per mm 2 .
- the interconnector preferably has one or more of the following properties:
- the number per unit area of the sum of pores and oxide inclusions is> 90 000 per mm 2 at a sectional area.
- the chromium content is> 90% by weight.
- the density over the entire component thickness is between 70% and 95% of the theoretical density.
- At least 90% of the pores and oxide inclusions have an area of not more than 100 pm 2 .
- the total oxygen content is in a range ⁇ 20 000 pg per 1 g component.
- the total nitrogen content is in an area ⁇ 2000 pg per 1 g component.
- the content of Al 2 O 3 is in a range ⁇ 500 pg per 1 g component.
- the oxygen content increases over the component thickness from the middle to the edges of the interconnector.
- the described invention also comprises a powder metallurgically produced interconnector made of Cr or of a Cr-containing alloy which, compared to the prior art, has a significantly finer microstructure, above all a finer pore structure.
- a powder metallurgically produced interconnector made of Cr or of a Cr-containing alloy which, compared to the prior art, has a significantly finer microstructure, above all a finer pore structure.
- the invention relates to an electrochemical cell interconnector having a region with a chromium content of at least 80% by weight, with pores and / or oxide inclusions being present in the region, which is characterized in that
- the range has a density between 70% and 95% of the theoretical density
- the total oxygen content is in the range of ⁇ 20 000 pg per 1 g
- the gas permeability in the range ⁇ 10 ml / min at a test pressure of 2.75 bar and a temperature of 20 ° C.
- the gas permeability is determined by differential pressure method. In this case, a positive pressure of 2.75 bar is given up on one side of the component.
- the test gas is air and the temperature is 20 ° C.
- the test circuit is closed and after a settling phase of a few seconds, the pressure drop over the test time is measured. Via a calibrated test leak in an otherwise tight test circuit, a factor for the conversion of the pressure loss per time into a volume flow (unit ml / min) can take place. This conversion makes the measurement independent of the volume of the test cycle.
- the number of the sum of pores and oxide inclusions at a sectional area through the region is at least 10,000 per mm 2 . In one embodiment, it is provided that the number of the sum of pores and oxide inclusions along the cut surface is at least 20,000, preferably at least 40,000, more preferably at least 60,000 per mm 2 . In a preferred embodiment, it is provided that the number of the sum of pores and oxide inclusions along the cut surface is at least 90,000 per mm 2 . The larger the number of pores per area, the more economically the pores can be closed by oxidation.
- the chromium content is at least 90% by weight.
- At least 90% of the pores and oxide inclusions present have a maximum equivalent pore diameter of not more than 12 ⁇ m along the cut surface.
- At least 90% of the pores and oxide inclusions present have an area of not more than 100 ⁇ m 2 along the cut surface.
- the total nitrogen content in the range is ⁇ 2000 pg per 1 g. Furthermore, it can be provided that the content of Al 2 O 3 in the range is ⁇ 500 pg per 1 g.
- Fig. 1 a to 1c show three different areas of inventive
- Fig. 2 shows the maximum equivalent diameter (equivalent pore diameter) of pores and oxide inclusions of the three areas of Figs. 1a to
- Fig. 3 shows the oxygen content (O-concentration) of the component in
- FIG. 4 shows the nitrogen content (N concentration) of the component in FIG.
- FIGS. 5a to 8b show a comparison between a device according to the invention
- FIGS. 5a-6b show SEM images; Figures 7a, 7b describe equivalent diameters of pores and chromium oxide inclusions; Fig. 8a, 8b describe the pore area distribution.
- Embodiment 1 (Simple Pressing):
- Chromium powder for a powder batch can be obtained as follows. Pigment grade Cr 2 O 3 (Nippon Denko ND812) is well blended with crystalline synthetic graphite powder (Timcal Timrex KS6). The carbon content of the mixture thus prepared is 2.85 moles per mole of Cr 2 O 3 . 200 g of this mixture are heated in an aluminum oxide crucible in a flow reactor at a heating rate of 10 K / min to 800 ° C and then at a heating rate of 2 K / min to 1050 ° C. The heating was carried out under the action of H 2 , wherein the H 2 pressure was adjusted so that in the temperature range 800 ° C to 1050 ° C, the mass spectrometry measured CH 4 - partial pressure was> 5 mbar.
- the total pressure was about 1 bar. Thereafter, the reaction mixture was heated to 1350 ° C at a heating rate of 10 K / min. The holding time at 1350 ° C was 180 min. Heating from 1050 ° C to 1350 ° C and holding at 350 ° C was carried out with supply of dry hydrogen with a dew point ⁇ -40 ° C, the pressure was about 1 bar. The oven cooling was also under H2 with a dew point ⁇ -40 ° C. After reaction, a metallic "sponge" is obtained, which can be easily deagglomerated to a powder, and the oxygen content in one experiment was 503 pg / g.
- a powder mixture consisting of 95 wt .-% fine Cr powder (having a BET surface area of> 0.05 m 2 / g, granulated to a more free-flowing powder having a particle size fraction of 45 - 250 pm) and 5 wt .-% of a FeY master alloy (alloy with 0.8 wt .-% Y, particle size ⁇ 100 pm) prepared.
- an oxidation of the component is carried out at 950 ° C for a period of 10 to 30 hours in order to close any residual porosity so far that the permeability is sufficiently low.
- the surface of the oxidized component is freed from the oxide layer by an all-round sandblasting process.
- Embodiment 2 (Double Pressing):
- the compact is prepared as in Example 1: First, a powder mixture consisting of 95 wt .-% fine Cr powder (having a BET surface area of> 0.05 m 2 / g, granulated to a more free-flowing powder fraction 45th - 250 pm) and 5 wt .-% of a FeY master alloy (alloy with 0.8 wt .-% Y, grain size ⁇ 100 pm) prepared.
- pre-sintering of the compact at 900 ° C. for 20 minutes (time at maximum temperature) under water atmosphere in a band oven for the purpose the dewaxing of the compact.
- a sizing press of the presintered component is provided at a specific pressing pressure of 500 to 1000 MPa.
- FIGS. 1 a to 1 c the microstructure and in particular the pore structure of the components according to the invention are significantly finer (lower row) than those of the reference component according to the prior art (upper row). This visual impression could also be numerically recorded and confirmed.
- the maximum pore diameter is significantly reduced in the embodiment according to the invention (FIG. 2).
- the components were subjected to the same oxidation program, although the components of the invention would require less oxidation time or a lower oxidation temperature to achieve the same gas tightness.
- the "dark objects” must be defined as pores in the detection setting, for example due to partial pore filling with oxide, the entire pore may not be recognized as an object It is the "fill holes” option to capture the pore and thus its surface as a related object.
- the "Remove edge particles” option does not include incomplete pores in the edge area of the image area in the evaluation.
- the analysis was always carried out by means of carrier gas heat extraction.
- 0.2 to 0.5 g of sample were weighed in a platinum crucible and the oxygen in Inert gas stream extracted.
- the extraction temperature is about 2000 ° C.
- the extraction time depends on the oxygen content of the sample, but is at least 40 seconds.
- the released oxygen reacts with carbon and forms CO / C0 2 , which is analyzed by IR spectrometry.
- the determination of the nitrogen concentration was carried out together with the oxygen measurement.
- the determination of the concentration in this case takes place via the thermal conductivity of the released gas stream.
- FIGS. 5a and 5b show components in section as a SEM diagram.
- FIGS. 6a and 6b show a detailed view. Visible in the component according to the invention, the larger pore / oxide inclusion number at the same time lower pore / oxide inclusion size.
- Figs. 7a and 7b show the distribution of the equivalent diameter.
- the arithmetic mean of the component according to the invention is 2.0 ⁇ compared to 7.0 ⁇ in the prior art.
- the bandwidth is between 0.3 and 13.0 ⁇ or 0.6 and 63.7 ⁇ .
- 8a and 8b show the pore surface distribution, which in the component according to the invention in the arithmetic mean at 7.3 ⁇ 2 compared to 107 ⁇ 2 in the prior art.
- the scattering is between 0.05 to 133.1 ⁇ 2 in the component according to the invention compared to 0.31 to 3182 ⁇ 2 in the prior art.
- the pore density is according to the invention in the arithmetic mean at 132 957 mm “2 compared with 810 mm “ 2 in the prior art.
- the spread is between 79 327 and 211 800 mm “2 or 715 and 895 mm “ 2 .
- the values indicated in FIGS. 2, 7 and 8 subsume pores and oxide inclusions, as can be seen from the description of the measurement.
Abstract
Description
Claims
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ATGM280/2013U AT14143U1 (en) | 2013-09-02 | 2013-09-02 | Powder metallurgical component |
PCT/AT2014/000161 WO2015027257A2 (en) | 2013-09-02 | 2014-08-19 | Powdered metal component |
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EP3041626A2 true EP3041626A2 (en) | 2016-07-13 |
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EP14777485.5A Withdrawn EP3041626A2 (en) | 2013-09-02 | 2014-08-19 | Powdered metal component |
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US (1) | US10211465B2 (en) |
EP (1) | EP3041626A2 (en) |
JP (1) | JP2016532783A (en) |
KR (1) | KR20160052541A (en) |
CN (1) | CN105517733B (en) |
AT (1) | AT14143U1 (en) |
CA (1) | CA2920784A1 (en) |
TW (1) | TWI623625B (en) |
WO (1) | WO2015027257A2 (en) |
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AT386612B (en) * | 1987-01-28 | 1988-09-26 | Plansee Metallwerk | CRISP-RESISTANT ALLOY FROM MELTING-MELTING METAL AND METHOD FOR THEIR PRODUCTION |
JPH04505986A (en) | 1989-05-31 | 1992-10-15 | シーメンス アクチエンゲゼルシヤフト | Manufacturing method of CuCr contact material for vacuum electromagnetic contactor and attached contact material |
JPH0747793B2 (en) * | 1991-04-26 | 1995-05-24 | 株式会社クボタ | Oxide dispersion strengthened heat resistant sintered alloy |
ATE137361T1 (en) | 1992-07-16 | 1996-05-15 | Siemens Ag | MATERIAL FOR THE METALLIC COMPONENTS OF HIGH TEMPERATURE FUEL CELL SYSTEMS |
JP2898475B2 (en) * | 1992-07-21 | 1999-06-02 | 株式会社クボタ | Manufacturing method of oxide dispersion strengthened heat-resistant alloy sintered body |
US5320181A (en) * | 1992-09-28 | 1994-06-14 | Wellheads & Safety Control, Inc. | Combination check valve & back pressure valve |
JPH0820809A (en) * | 1994-07-07 | 1996-01-23 | Akira Honda | Production of chromium-base alloy powder |
AT4737U1 (en) | 2001-01-15 | 2001-11-26 | Plansee Ag | POWDER METALLURGICAL METHOD FOR PRODUCING HIGH-DENSITY MOLDED PARTS |
JP4025615B2 (en) | 2002-10-08 | 2007-12-26 | 勇 内田 | Fuel cell capable of fuel regeneration, power generation method and fuel regeneration method |
AT11555U1 (en) * | 2009-03-12 | 2010-12-15 | Plansee Se | INTERCONNECTOR OF A FIXED ELECTROLYTE HIGH TEMPERATURE FUEL CELL |
US10040121B2 (en) | 2009-12-09 | 2018-08-07 | Porite Taiwan Co., Ltd. | Method for forming an interconnect of a solid oxide fuel cell |
WO2013074918A1 (en) * | 2011-11-18 | 2013-05-23 | Bloom Energy Corporation | Fuel cell interconnects and methods of fabrication |
-
2013
- 2013-09-02 AT ATGM280/2013U patent/AT14143U1/en not_active IP Right Cessation
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- 2014-08-19 CN CN201480048403.1A patent/CN105517733B/en not_active Expired - Fee Related
- 2014-08-19 EP EP14777485.5A patent/EP3041626A2/en not_active Withdrawn
- 2014-08-19 CA CA2920784A patent/CA2920784A1/en not_active Abandoned
- 2014-08-19 JP JP2016537047A patent/JP2016532783A/en active Pending
- 2014-08-19 WO PCT/AT2014/000161 patent/WO2015027257A2/en active Application Filing
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TW201510235A (en) | 2015-03-16 |
TWI623625B (en) | 2018-05-11 |
KR20160052541A (en) | 2016-05-12 |
CN105517733B (en) | 2019-02-01 |
US20160211531A1 (en) | 2016-07-21 |
AT14143U1 (en) | 2015-05-15 |
WO2015027257A3 (en) | 2015-04-30 |
US10211465B2 (en) | 2019-02-19 |
WO2015027257A2 (en) | 2015-03-05 |
JP2016532783A (en) | 2016-10-20 |
CA2920784A1 (en) | 2015-03-05 |
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