EP0956173B1 - Granules de poudre metallique, leur procede de preparation et leur utilisation - Google Patents
Granules de poudre metallique, leur procede de preparation et leur utilisation Download PDFInfo
- Publication number
- EP0956173B1 EP0956173B1 EP96939034A EP96939034A EP0956173B1 EP 0956173 B1 EP0956173 B1 EP 0956173B1 EP 96939034 A EP96939034 A EP 96939034A EP 96939034 A EP96939034 A EP 96939034A EP 0956173 B1 EP0956173 B1 EP 0956173B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- metal powder
- granulation
- granulated
- binder
- hydrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000008187 granular material Substances 0.000 title claims abstract description 69
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 38
- 239000002184 metal Substances 0.000 title claims abstract description 38
- 239000000843 powder Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000002739 metals Chemical class 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 4
- 150000001242 acetic acid derivatives Chemical class 0.000 claims abstract description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims abstract description 3
- 150000004679 hydroxides Chemical class 0.000 claims abstract description 3
- 150000003891 oxalate salts Chemical class 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 27
- 238000005469 granulation Methods 0.000 claims description 18
- 230000003179 granulation Effects 0.000 claims description 18
- 238000007906 compression Methods 0.000 claims description 10
- 230000006835 compression Effects 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 229910003460 diamond Inorganic materials 0.000 claims description 5
- 239000010432 diamond Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 150000004675 formic acid derivatives Chemical class 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 238000009477 fluid bed granulation Methods 0.000 claims 1
- 150000002484 inorganic compounds Chemical class 0.000 claims 1
- 229910010272 inorganic material Inorganic materials 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- -1 hydrogenocarbonates Chemical class 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102100029360 Hematopoietic cell signal transducer Human genes 0.000 description 1
- 101000990188 Homo sapiens Hematopoietic cell signal transducer Proteins 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910021446 cobalt carbonate Inorganic materials 0.000 description 1
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000019809 paraffin wax Nutrition 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 229920002717 polyvinylpyridine Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
Images
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
- 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
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
- B22F1/12—Metallic powder containing non-metallic particles
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
-
- 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
Definitions
- the present invention relates to metal powder granules composed of one or more the metals Co, Cu, Ni, W and Mo, a process for its production as well as its use.
- Granules of the metals Co, Cu, Ni, W and Mo have a variety of uses as sintered materials.
- copper metal granules suitable for making copper sliding contacts for motors tungsten granules find possible uses for the production of W / Cu drinking contacts, Ni and Mo granules can be used for corresponding semi-finished product applications.
- Cobalt metal powder granules are used as binder components in Composite sintered bodies e.g. Hard metals and diamond tools.
- DE-A 43 43 594 discloses that free-flowing metal powder granules by atomizing and sieving suitable grain areas can. However, these granules are for the manufacture of diamond tools not suitable.
- EP-A-399 375 describes the production of a free-flowing tungsten carbide-cobalt metal powder granulate.
- the fine components are the starting components Powder agglomerated together with a binder and a solvent.
- the binder is then removed thermally and the agglomerate, in order to obtain the desired flowability, at 2500 ° C. in Aftertreated plasma.
- Fine cobalt metal powders can be made using this process but do not granulate, because at temperatures above the melting point processing problems similar to those of processing atomized powders occur.
- EP-A 0 659 508 describes the production of metal powder granules general formula RFeB or RCo, where R is for rare earth metals or compounds, B stands for boron and Fe for iron. After that, first an alloy of the components and these by grinding to the desired fineness brought. Then binders and solvents are added and the Slurry dried in a spray dryer. Disadvantage of this method - especially for the production of diamond tools - is that initially the Metals are alloyed and by melting fine cobalt metal powder their characteristic properties, as described in DE-A 43 43 594, lose. It is therefore the most suitable for the production of cobalt metal powder granules State of the art, e.g.
- the granules obtained in this way have a rounded grain shape.
- the surface is relatively dense with no large pores or gas outlet openings.
- the bulk density determined according to ASTM B 329 is relatively high at 2.0-2.4 g / cm 3 (Table 2). 1 shows the scanning electronic (SEM) image of a commercially available granulate from Eurotungstene, Grenoble France, in FIG. 2 that of a commercially available granulate from Hoboken Overpelt, Belgium.
- SEM scanning electronic
- the compression behavior can be described quantitatively by measuring the compression factor F comp .
- F comp ( ⁇ p - ⁇ O ) / ⁇ p with ( ⁇ 0 ), the bulk density in g / cm 3 of the cobalt metal powder granulate in the original state and ( ⁇ p ) the density in g / cm 3 after pressing.
- Binder used granules remain in the granules (see Table 1).
- binder is understood to mean a film-forming substance which, if appropriate, is dissolved in a solvent and is added to the starting components in a suitable granulation process in such a way that the powder surface is wetted, or if appropriate after removal of the solvent, by forming a surface film on the primary grains these are held together. This produces granules of sufficient mechanical strength.
- substances can also be used as binders, which ensure the mechanical strength of the granulate particles through capillary forces.
- the heating-up time can be extended. This can be a Reduce production by up to 25%.
- the heating times not prolonged, carbon nests are observed in the hot-pressed segments through cracking processes of the binders. This often leads to one significant deterioration in tool quality.
- Another disadvantage is the use of organic solvents, which after the granulation are carefully removed by evaporation. First of all, that is Removal of the solvents by the thermal treatment is expensive.
- organic solvents has significant disadvantages with regard to environmental compatibility, plant safety and the energy balance. The Working with organic solvents often requires considerable equipment Expenditure on suction and disposal facilities, as well as on filters to prevent the emission of organic solvents during granulation.
- the systems must be explosion-proof, which in turn increases investment costs.
- a binder-free metal powder granulate which consists of one or more of the metals Co, Cu, Ni, W and Mo, with a maximum of 10% by weight ⁇ 50 ⁇ m according to ASTM B214 and the total carbon content less than 0. 1 wt .-%, particularly preferably less than 400 ppm.
- This binder-free metal powder granulate is the subject of this invention.
- the surface and grain shape of the product according to the invention has been significantly optimized.
- 3 shows the SEM image of the metal powder granules according to the invention using the example of a cobalt metal powder granules according to the invention. It has a cracked, jagged structure that facilitates the formation of positive connections.
- the granulate according to the invention is very porous. This significantly reduces the resistance to deformation during cold pressing.
- the porous structure is reflected in the bulk weight.
- the cobalt metal powder granulate preferably has a low bulk density between 0.5 to 1.5 g / cm 3 , determined according to ASTM B 329. In a particularly preferred embodiment, it has a compression factor F comp of at least 60% and at most 80%. This high compression factor leads to excellent compressibility.
- cold pressed sintered bodies can be produced at a pressure of 667 kg / cm 2 , which have excellent mechanical edge stability.
- Table 2 below shows the bulk density of the product according to the invention in its original state ( ⁇ 0 ), the density after pressing ( ⁇ p ) and the compression factor F comp in comparison to commercially available granules.
- Typical bulk density in original condition ( ⁇ 0 ), after pressing with 667 kg / cm 2 ( ⁇ p ) and the compression factor of the cobalt metal powder granulate according to the invention in comparison to commercially available products Manufacturer HCST Goslar / Germany EUROTUNGSTENE Grenoble / France HOBOKEN Overpelt / Belgium HOBOKEN Overpelt / Belgium product cobalt metal powder granules according to the invention Cobalt metal powder granulate ultrafine Cobalt metal powder granules extrafein soft granulated Cobalt metal powder granules extrafine hard granulated Bulk density ( ⁇ 0 ) (g / cm 3 ) 1.03 2.13 2.4 2.4 Compression density ( ⁇ p ) (g / cm 3 ) 3.
- the green compacts were produced in a uniaxial, hydraulic press with a load of 2.5 t and a square ram area of 2.25 cm 2 and a weight of 6 g
- This invention further relates to a method for producing the metal powder granules according to the invention. It is a process for the production of binder-free metal powder granules from one or several of the metals Co, Cu, Ni, W and Mo, being the starting component a metal compound from one or more of the groups of metal oxides, hydroxides, carbonates, bicarbonates, oxalates, acetates and formates with Binder and optionally additionally with 40% - 80% solvent is granulated to the solids content and the granules thermally by addition in a hydrogen-containing gas atmosphere to the metal powder granules is reduced, the binder and optionally the solvent is removed without residue.
- the method according to the invention thus opens up a possibility of solvents to use, which consist of organic compounds and / or water can, being particularly preferred, but not limited to, water as Solvent is used.
- solvents consist of organic compounds and / or water can, being particularly preferred, but not limited to, water as Solvent is used.
- the added binders are either without solvent or dissolved in the solvent or suspended or used emulsified.
- the binders and solvents can be inorganic or be organic compounds consisting of one or more of the elements carbon, Hydrogen, oxygen, nitrogen and sulfur built up and free of Halogens and, with the exception of traces that are unavoidable due to manufacture, free of metals are.
- binders and solvents can also be added Temperatures of less than 650 ° C are removed thermally without residue.
- a binder one or more of the following compounds are particularly suitable: Paraffin oils, paraffin waxes, polyvinyl acetates, polyvinyl alcohols, polyacrylamides, Methyl cellulose, glycerin, polyetylene glycols, linseed oils, polyvinyl pyridine.
- the use of polyvinyl alcohol as a binder is particularly preferred and water as a solvent.
- the granulation of the starting component is achieved according to the invention in that the granulations as plates, build-up, Spray dryer, fluidized bed, press granulation or granulation in high speed Mixers is carried out.
- the method according to the invention is particularly preferably carried out continuously or discontinuously in a ring mixer granulator.
- granules are particularly preferably subsequently in a hydrogen containing gas atmosphere at temperatures from 400 ° C to 1100 ° C, especially from 400 - 650 ° C, reduced to metal powder granules.
- a hydrogen containing gas atmosphere at temperatures from 400 ° C to 1100 ° C, especially from 400 - 650 ° C, reduced to metal powder granules.
- Binder and, if necessary, the solvent are removed without residue.
- Another embodiment variant of the method according to the invention consists in that the granulate after the granulation step first at temperatures of 50 ° C is dried to 400 ° C and then at temperatures from 400 ° C to 1100 ° C in a hydrogen-containing gas atmosphere to the metal powder granulate is reduced.
- the metal powder granules according to the invention are ideal for Manufacture of sintered and composite sintered bodies. Subject of this invention is thus also the use of the metal powder granules according to the invention as Binder component in sintered bodies or composite sintered bodies made of hard powder and / or diamond powder and binders.
- the compression factor F comp was determined with the aid of a uniaxial, hydraulic press with a load of 2.5 t with a press ram area of 2.25 m 2 and a weight of 6 g.
- Properties of the granules containing cobalt described in the examples example Total carbon content (ppm) Bulk density (g / cm3) Sieve analysis according to ASTM B 214 (%) + 1000 ⁇ m - 1000 ⁇ m + 50 ⁇ m - 50 ⁇ m 1 200 1.4 3.4 90.5 6.1 2 360 1.2 6.9 91.0 2.1 3rd 310 0.8 4.5 89.9 5.6 4th 80 1.0 0.2 96.1 3.7
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Glanulating (AREA)
Claims (13)
- Granulé de poudre métallique constitué d'un ou de plusieurs des métaux Co, Cu, Ni, W et Mo, caractérisé en ce qu'il contient au maximum 10% en poids de fraction inférieure à 50 µm, suivant ASTM B 214 et que la teneur en carbone totale s'élève à moins de 0,1% en poids.
- Granulé de poudre métallique suivant la revendication 1, caractérisé en ce que la teneur en carbone totale s'élève de manière particulièrement préférée, à moins de 400 ppm.
- Granulé de poudre métallique suivant la revendication 1 ou 2, caractérisé en ce que le granulé présente une structure poreuse, fendillée, crevassée.
- Granulé de poudre métallique de cobalt suivant l'une ou plusieurs des revendications 1 à 3, caractérisé en ce qu'il présente une masse volumique apparente suivant ASTM B 329 située dans l'intervalle allant de 0,5 à 1,5 g/cm3, de manière particulièrement préférée 1,0 à 1,2 g/cm3.
- Granulé de poudre métallique de cobalt suivant l'une ou plusieurs des revendications 1 à 4, caractérisé en ce qu'il présente un taux de tassement Fcomp. d'au moins 60% et d'au plus 80%.
- Procédé de préparation d'un granulé de poudre métallique suivant l'une ou plusieurs des revendications 1 à 5, caractérisé en ce que l'on granule comme composants de départ, un composé métallique parmi un ou plusieurs du groupe des oxydes, hydroxydes, carbonates, hydrogénocarbonates, oxalates, acétates, formiates avec un liant et facultativement, 40 à 80% de solvant, sur base de la teneur en matière solide, et on réduit le granulé thermiquement dans une atmosphère gazeuse contenant de l'hydrogène, en granulé de poudre métallique, où le liant et facultativement, le solvant sont éliminés sans résidu.
- Procédé suivant la revendication 6, caractérisé en ce que comme liant et facultativement, solvant on met en oeuvre des composés organiques ou inorganiques, qui sont élaborés à partir d'un ou de plusieurs des éléments carbone, hydrogène, oxygène, azote et soufre et sont exempts d'halogène et de métal.
- Procédé suivant l'une ou plusieurs des revendications 6 et 7, caractérisé en ce que le liant et facultativement, le solvant peuvent être thermiquement éliminés sans résidu à des températures inférieures à 650°C.
- Procédé suivant l'une ou plusieurs des revendications 6 à 8, caractérisé en ce que la granulation est réalisée sous forme d'une granulation à accumulation, granulation par séchage par pulvérisation, à lit fluidisé, granulation à disque, granulation par compression ou granulation dans un mélangeur à haute vitesse.
- Procédé suivant la revendication 9, caractérisé en ce que la granulation dans un mélangeur à haute vitesse est réalisée en tant que granulation à mélangeur annulaire.
- Procédé suivant l'une ou plusieurs des revendications 6 à 10, caractérisé en ce que les granulés sont réduits dans une atmosphère gazeuse contenant de l'hydrogène, à des températures allant de 400 à 1100°C, de préférence de 400 à 650°C, en granulé de poudre métallique.
- Procédé suivant l'une ou plusieurs des revendications 6 à 11, caractérisé en ce que le granulé est d'abord thermiquement séché à des températures allant de 50 à 400°C et que le granulé est ensuite réduit dans une atmosphère gazeuse contenant de l'hydrogène, en granulé de poudre métallique, à des températures allant de 400 à 1100°C.
- Utilisation des granulés de poudre métallique suivant l'une ou plusieurs des revendications 1 à 5 comme composant liant dans des comprimés frittés ou des comprimés frittés composites, préparés à partir de poudres de matières dures et/ou d'égrisé et de liant.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19544107 | 1995-11-27 | ||
DE19544107A DE19544107C1 (de) | 1995-11-27 | 1995-11-27 | Metallpulver-Granulat, Verfahren zu seiner Herstellung sowie dessen Verwendung |
PCT/EP1996/004983 WO1997019777A1 (fr) | 1995-11-27 | 1996-11-14 | Granules de poudre metallique, leur procede de preparation et leur utilisation |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0956173A1 EP0956173A1 (fr) | 1999-11-17 |
EP0956173B1 true EP0956173B1 (fr) | 2001-02-28 |
Family
ID=7778486
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP96939034A Expired - Lifetime EP0956173B1 (fr) | 1995-11-27 | 1996-11-14 | Granules de poudre metallique, leur procede de preparation et leur utilisation |
Country Status (13)
Country | Link |
---|---|
US (1) | US6126712A (fr) |
EP (1) | EP0956173B1 (fr) |
JP (2) | JP4240534B2 (fr) |
KR (1) | KR100439361B1 (fr) |
CN (1) | CN1090068C (fr) |
AT (1) | ATE199340T1 (fr) |
AU (1) | AU702983B2 (fr) |
CA (1) | CA2238281C (fr) |
DE (2) | DE19544107C1 (fr) |
ES (1) | ES2155209T3 (fr) |
HK (1) | HK1017630A1 (fr) |
PT (1) | PT956173E (fr) |
WO (1) | WO1997019777A1 (fr) |
Families Citing this family (30)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19544107C1 (de) * | 1995-11-27 | 1997-04-30 | Starck H C Gmbh Co Kg | Metallpulver-Granulat, Verfahren zu seiner Herstellung sowie dessen Verwendung |
EP1257377A4 (fr) * | 2000-02-22 | 2004-04-21 | Omg Americas Inc | Conversion rapide de composes contenant du metal en metaux ou oxydes metalliques |
KR100374705B1 (ko) * | 2000-06-19 | 2003-03-04 | 한국기계연구원 | 탄화텅스텐/코발트계 초경합금의 제조방법 |
US7674401B2 (en) | 2001-12-18 | 2010-03-09 | Asahi Kasei Kabushiki Kaisha | Method of producing a thin conductive metal film |
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WO2012169258A1 (fr) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène |
WO2012169256A1 (fr) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène |
WO2014104177A1 (fr) | 2012-12-27 | 2014-07-03 | 昭和電工株式会社 | Corps de conversion chimique pour électrode positive de condensateur au niobium et procédé de production associé |
CN105658582B (zh) | 2013-08-19 | 2019-04-19 | 犹他大学研究基金会 | 制备钛产品 |
EP3142816A4 (fr) | 2014-05-13 | 2017-12-27 | University Of Utah Research Foundation | Production de poudres métalliques sensiblement sphériques |
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CN107442771B (zh) * | 2017-09-12 | 2024-04-05 | 浙江奥真电子科技有限公司 | 一种粉末冶金制品的原料传输装置 |
CA3101795C (fr) | 2018-05-30 | 2023-10-10 | Hela Novel Metals Llc | Procedes de production de poudres metalliques fines a partir de composes metalliques |
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CN110079691B (zh) * | 2019-06-14 | 2020-11-06 | 安泰天龙钨钼科技有限公司 | 一种低钼含量钼铜合金及其制备方法 |
CN110079690B (zh) * | 2019-06-14 | 2020-11-06 | 安泰天龙钨钼科技有限公司 | 一种高钼含量钼铜合金及其制备方法 |
US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
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CN113427004B (zh) * | 2020-03-23 | 2023-09-01 | 精工爱普生株式会社 | 触变注射成形用材料的制造方法 |
CN112872363A (zh) * | 2021-01-12 | 2021-06-01 | 江西理工大学 | 一种稀土钴镍复合粉的制备方法 |
CN115430839B (zh) * | 2022-08-25 | 2023-07-07 | 云南电网有限责任公司电力科学研究院 | 镍钼金属间化合物的制备方法及制得的镍钼金属间化合物 |
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-
1995
- 1995-11-27 DE DE19544107A patent/DE19544107C1/de not_active Expired - Fee Related
-
1996
- 1996-11-14 US US09/077,279 patent/US6126712A/en not_active Expired - Lifetime
- 1996-11-14 AT AT96939034T patent/ATE199340T1/de active
- 1996-11-14 CN CN96198573A patent/CN1090068C/zh not_active Expired - Lifetime
- 1996-11-14 WO PCT/EP1996/004983 patent/WO1997019777A1/fr active IP Right Grant
- 1996-11-14 KR KR10-1998-0703925A patent/KR100439361B1/ko not_active IP Right Cessation
- 1996-11-14 DE DE59606529T patent/DE59606529D1/de not_active Expired - Lifetime
- 1996-11-14 JP JP52011297A patent/JP4240534B2/ja not_active Expired - Fee Related
- 1996-11-14 ES ES96939034T patent/ES2155209T3/es not_active Expired - Lifetime
- 1996-11-14 AU AU76838/96A patent/AU702983B2/en not_active Ceased
- 1996-11-14 EP EP96939034A patent/EP0956173B1/fr not_active Expired - Lifetime
- 1996-11-14 CA CA002238281A patent/CA2238281C/fr not_active Expired - Fee Related
- 1996-11-14 PT PT96939034T patent/PT956173E/pt unknown
-
1999
- 1999-05-14 HK HK99102161A patent/HK1017630A1/xx not_active IP Right Cessation
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2008
- 2008-06-18 JP JP2008159500A patent/JP2008285759A/ja active Pending
Also Published As
Publication number | Publication date |
---|---|
ATE199340T1 (de) | 2001-03-15 |
KR19990071649A (ko) | 1999-09-27 |
EP0956173A1 (fr) | 1999-11-17 |
ES2155209T3 (es) | 2001-05-01 |
DE19544107C1 (de) | 1997-04-30 |
CA2238281C (fr) | 2006-04-11 |
KR100439361B1 (ko) | 2004-07-16 |
PT956173E (pt) | 2001-08-30 |
CA2238281A1 (fr) | 1997-06-05 |
HK1017630A1 (en) | 1999-11-26 |
JP4240534B2 (ja) | 2009-03-18 |
JP2000500826A (ja) | 2000-01-25 |
WO1997019777A1 (fr) | 1997-06-05 |
AU702983B2 (en) | 1999-03-11 |
CN1090068C (zh) | 2002-09-04 |
US6126712A (en) | 2000-10-03 |
JP2008285759A (ja) | 2008-11-27 |
AU7683896A (en) | 1997-06-19 |
DE59606529D1 (de) | 2001-04-05 |
CN1202846A (zh) | 1998-12-23 |
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