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 PDF

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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
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EP
European Patent Office
Prior art keywords
metal powder
granulation
granulated
binder
hydrogen
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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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EP96939034A
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German (de)
English (en)
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EP0956173A1 (fr
Inventor
Matthias HÖHNE
Benno Gries
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HC Starck GmbH
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HC Starck GmbH
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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

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  • 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)

  1. 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.
  2. 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.
  3. Granulé de poudre métallique suivant la revendication 1 ou 2, caractérisé en ce que le granulé présente une structure poreuse, fendillée, crevassée.
  4. 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.
  5. 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%.
  6. 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.
  7. 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.
  8. 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.
  9. 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.
  10. 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.
  11. 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.
  12. 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.
  13. 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.
EP96939034A 1995-11-27 1996-11-14 Granules de poudre metallique, leur procede de preparation et leur utilisation Expired - Lifetime EP0956173B1 (fr)

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

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EP0956173A1 EP0956173A1 (fr) 1999-11-17
EP0956173B1 true EP0956173B1 (fr) 2001-02-28

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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)

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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
CN110026560B (zh) * 2018-08-27 2022-04-29 南方科技大学 纳米铜颗粒及其制备方法和应用
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
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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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