EP1242642B1 - Verfahren zur herstellung von pulvermischungen bzw. verbundpulver - Google Patents

Verfahren zur herstellung von pulvermischungen bzw. verbundpulver Download PDF

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Publication number
EP1242642B1
EP1242642B1 EP00991157A EP00991157A EP1242642B1 EP 1242642 B1 EP1242642 B1 EP 1242642B1 EP 00991157 A EP00991157 A EP 00991157A EP 00991157 A EP00991157 A EP 00991157A EP 1242642 B1 EP1242642 B1 EP 1242642B1
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EP
European Patent Office
Prior art keywords
powder
type
metal
binder
metals
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Expired - Lifetime
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EP00991157A
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German (de)
English (en)
French (fr)
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EP1242642A1 (de
Inventor
Bernd Mende
Gerhard Gille
Ines Lamprecht
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • 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
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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 a process for the preparation of powder mixtures or composite powders which consist of at least two types of powder or solid phases in disperse form and which are used as precursors for particle composites or as wettable powders for surface coatings.
  • these composite powders contain high-melting metals (such as W and Mo) or hard materials (such as WC, TiC, TiN, Ti (C, N) TaC, NbC and Mo 2 C) or ceramic powders (such as TiB 2 and B 4 C) on the one hand and binding metals (such as Fe, Ni, Co, Cu and Sn) or mixed crystals and alloys of these binding metals on the other hand.
  • particle composites hard metals, cermets, heavy metals and Functional materials with special electrical (contact and switching materials) and thermal properties (heat sinks).
  • the effective properties of these particle composites e.g. Hardness, modulus of elasticity, Fracture toughness, strength and wear resistance, but also electrical and thermal conductivity are in addition to the properties and proportions of the phases especially by the degree of dispersion, the homogeneity and the topology of these Phases as determined by structural defects (pores, impurities).
  • This Structural characteristics of the particle composites are in turn due to the powdery Raw materials and their powder metallurgical processing (pressing, sintering) determined to compact materials.
  • Hard metals are particle composites from at least two phases, the WC hard material phase (97 - 70 m%) and the eutectic Co-WC binder metal phase (3 - 30 m%), which are formed by dissolving W and C in Co during liquid phase sintering and which WC particles bind.
  • the hard metals can include other hard material phases such as the cubic (W, Ti) and (W, Ta / Nb) mixed carbides with proportions from 1 to 15 m% included. If the hard metals are particularly corrosive, the Co-based binder is completely or partially replaced by Ni, Cr (Fe) alloys. VC and Cr 3 C 2 ⁇ 1 m%) to control grain growth and microstructure.
  • the hard material particles are carriers of hardness, wear resistance and high temperature properties, while the binder metals primarily determine fracture toughness, thermal shock resistance and flexural strength.
  • Hard metals are characterized in particular by very favorable combinations of hardness and toughness as well as high temperature stability and wear / corrosion resistance. This is achieved in that either the hard material particles are fully dispersed in the binder metal or, with decreasing binder metal content, two mutually penetrating phase regions of hard material and binder are formed. During sintering, this structure runs parallel to the compaction of the compact.
  • the densification during the sintering process takes place to 70-85% of the increase in density in the solid-phase sintering stage, ie the WC grains move into energetically preferred positions under the effect of the viscous flowing and wetting binder.
  • the eutectic composition is finally achieved and the binding metal melts through the simultaneous diffusion of W and C into the co-particles.
  • the state of the art of hard metal production can be found, for example, in SCHEDLER, Tungsten carbide for the practitioner, Düsseldorf 1988.
  • the carbide composition are the separately produced hard material and binder metal powders first weighed, mixed and ground.
  • the toilet powder is always carbide grade with their grain sizes in the range of 0.5 ... 50 ⁇ m mostly slightly agglomerated and must have sufficient chemical purity.
  • By varying the toilet grain sizes and the binder metal content between 3 and 30 m% can important properties such as hardness, toughness and Wear resistance varies greatly and is adapted to the specific application become.
  • US-A-5 248 328 describes a method comprising a component (SE metal) via a precipitation in a suspension
  • SE metal component
  • Hard material or a binder metal is mixed in relatively small amounts.
  • hard material and binding metal are mixed and grind.
  • the different types of wet grinding are used today Powder components transferred into a finely divided mixture.
  • a grinding fluid serve organic liquids such as B. hexane, heptane, gasoline, tetralin, alcohol or acetone. Grinding liquid and medium (carbide balls) allow a highly disperse distribution of the powder particles, with increasing fineness and dispersity
  • organic grinding fluid it increases moisture and Gas absorption and oxidation of the powder.
  • After grinding it will Powder mixture by sieving from the grinding balls and by evaporation from the Grinding liquid separated, dried and granulated if necessary.
  • the grinding takes place mainly in attritors and ball mills, sometimes also in vibrating mills.
  • the currently dominant one that has been used on an industrial scale for around 20 years The form of drying is spray drying under inert gas, with simultaneous Granulation of the composite powder.
  • the dried and optionally granulated Mixtures are pressed, extruded or injection molded (MIM) into molded parts processed and then sintered.
  • the actual compression process are dewaxing, d. H. driving out pressing aids and presintering upstream for deoxidation and pre-compression. Sintering takes place either under vacuum or inert gas pressures up to 100 bar at temperatures between 1350 and 1500 ° C.
  • the hard material particles be electrolytically mixed to coat a coating of the binder metal in order to remove the complex grinding with all to overcome their disadvantages.
  • this procedure is cumbersome Handling is not suitable for the industrial scale and also has the disadvantage that only one metal, but not several mixed homogeneously on the Hard material particles can be applied since different metals in general have different electrochemical deposition potentials.
  • WO 95/26843 (EP-A 752 922, US-A 5 529 804) describes a process hard particles in polyols with reducing properties, e.g.
  • this method must be economically justifiable to achieve Yields of binder metals between 5 - 40 moles of reducing agent per mole Metal components are used and the resulting during the reduction volatile compounds (alkanals, alkanones, alkanoic acids) must be distilled off become. About the disposal of these unwanted by-products and the Remain the large amount of excess reducing agent, which is also by-products contains no information. The long reduction time required limits the throughput capacity of the process. These conditions inevitably lead to high procedural costs.
  • WO 97/11805 the process of reduction with polyols is described in WO 95/26843 modified to reduce the enormous excess of reducing agents and improve profitability.
  • the reduction reaction in liquid After consumption of a stoichiometric amount of polyol, based on the phase Metal insert, canceled to suppress the formation of unwanted by-products and to be able to recirculate the excess polyol.
  • the hard metal intermediate is filtered and then dry under hydrogen at 550 ° C and a very long reduction time of approx. 24 h to the finished composite powder reduced.
  • Ni-containing solution of the hard material suspended and by adding ammonia or a hydroxide is a metal compound on the surface of the hard material particles dejected.
  • this intermediate product reduced at elevated temperature under hydrogen.
  • the reduced amount used on polyols as solvents and reducing agents and the suppression of Side reactions must be carried out by means of a significantly longer reduction of the intermediate product can be compensated under hydrogen and at elevated temperature.
  • alcohols are also used to dissolve metal compounds therein to reduce metal or alloy powder or on an im Precipitate solvent-dispersed substrate as a metal film.
  • substrates include glass powder, Teflon, graphite, aluminum powder and fibers used.
  • US-A 5 352 269 describes the Spray Conversion Process (NANODYNE Inc.).
  • aqueous solutions e.g. B. W and Co contained in suitable concentrations and proportions and are prepared for example from ammonium metatungstate and cobalt chloride, spray dried.
  • the metals W and Co are mixed at the atomic level in the amorphous precursor powders formed in the process.
  • finely crystalline WC particles with coma dimensions of 20-50 nm are formed, which, however, are strongly agglomerated and interspersed with cobalt areas or are bound and have a diameter of approx.
  • composite powder with very good homogeneity, dispersity and possibly also special topology of the components / phases produced thereby can be that the desired binder metal powder (phases) in submitted Suspensions that already like the other components of the composite powder contain high-melting metal or hard material or ceramic powder, as Oxalate can be felled.
  • the present invention relates to a method according to claim 1.
  • Metals with melting points above 2000 ° C. such as molybdenum, tungsten, tantalum, niobium and / or rhenium, are used as the high-melting metals.
  • molybdenum and tungsten have gained technical importance.
  • tungsten carbide, titanium carbide, titanium nitride, titanium carbonitride, tantalum carbide, niobium carbide, molybdenum carbide and / or their mixed metal carbides and / or mixed metal carbonitrides are suitable as hard materials, optionally with the addition of vanadium carbide and chromium carbide.
  • TiB 2 or B 4 C are suitable as ceramic powders. Powders and mixtures of high-melting metals, hard materials and / or ceramic powders can also be used.
  • the first type of powder can in particular be in the form of finely divided powders with medium Particle diameters down to more than 10 ⁇ m can be used.
  • Cobalt, nickel, iron, copper and tin are used as binding metals and their alloys used
  • the binder metals are used as precursor compounds in the form of their water-soluble salts and their mixtures used in aqueous solution.
  • Suitable salts are chlorides, sulfates, nitrates or complex salts. by virtue of Chlorides and sulfates are generally preferred for ease of availability.
  • Oxalic acid or water-soluble oxalates such as are suitable for the precipitation as oxalate Ammonium oxalate or sodium oxalate.
  • the oxalic acid component can be aqueous Solution or suspension can be used.
  • the first type of powder can be in the aqueous solution of the precursor compound the second type of powder and an aqueous solution or Suspension of the oxalic acid component are added. It is also possible to Oxalic acid component in powder form in the suspension, which is the first type of powder contains to stir.
  • the first type of powder can also be in the aqueous solution or Suspension of the oxalic acid component and the aqueous solution of the precursor compound for the second type of powder.
  • the two suspensions or the suspension are mixed with the Solution with vigorous stirring.
  • the precipitation can be carried out continuously by simultaneous, continuous introduction into a flow reactor with continuous withdrawal of the precipitate. It can also be carried out discontinuously by presenting those containing the first powder type Suspension and initiation of the second precipitation partner take place. It can it to ensure a uniform precipitation over the precipitation reactor volume be expedient, the oxalate component in the form of a solid powder in the suspension from the first type of powder and solution of the precursor compound for the second type of powder stir in so that the oxalate component can be evenly distributed, before the precipitation occurs through its dissolution. You can also use the depot effect the use of a solid oxalate component the particle size for the precipitate Taxes.
  • the oxalic acid component is preferably 1.02 to 1.2 times stoichiometric Amount based on the precursor compound used for the second type of powder.
  • the concentration of the oxalic acid component in the precipitation suspension can be 0.05 to 1.05 mol / l, particularly preferably more than 0.6, particularly preferably be more than 0.8 mol / l.
  • the solid mixture consists of precipitate and the first type of powder separated from the mother liquor. This can be done by filtration, centrifugation or Decanting is done.
  • the solid mixture of the first type of powder and precipitate is treated under a reducing gas atmosphere at temperatures of preferably 350 to 650 ° C.
  • Hydrogen or a hydrogen / inert gas mixture is preferably used as the reducing gas, more preferably a nitrogen-hydrogen mixture.
  • the oxalate is completely broken down into gaseous components, some of which promote the reduction (H 2 O, CO 2 ; CO), and the second type of powder is produced by reduction to metal.
  • the oxalate decomposition and reduction can be in the moving or static bed, for example in tube furnaces or rotary tube furnaces or push-through furnaces continuously or be carried out discontinuously and under flowing, reducing gases. Any are also suitable for carrying out solid gas reactions suitable reactors, such as fluidized bed furnaces.
  • powder mixtures or composite powders obtainable according to the invention some of the powders of the first and second types as separate (“powder mixture”), partly as adhering (“composite powder”) components in extremely uniform Distribution essentially without formation of agglomerates. she can be processed without any further treatment.
  • the powders are suitable for the production of hard metals, cermets, heavy metals, metal-bonded diamond tools or electrotechnical functional materials by sintem, optionally using organic binders for the production sinterable green body. They are also suitable for surface coating parts and tools, for example by thermal or plasma spraying or for processing by extrusion or metal injection molding (MIM).
  • MIM metal injection molding
  • a hard metal test was carried out with this powder without any other treatment according to the following procedure: producing a green body with a pressure of 150 MPa, heating the green body in vacuo at a rate of 20 K / min to 1100 ° C., holding for 60 minutes at this temperature, further heating at a rate of 20 K / min to 1400 ° C, holding for 45 minutes at this temperature, cooling to 1100 ° C, holding for 60 minutes at this temperature and then cooling to room temperature.
  • tungsten carbide of the DS 80 type (supplier HCStarck) and 1 g of carbon black were homogeneously dispersed over a period of 60 minutes in a suspension of 465.4 g of oxalic acid dihydrate in 1.6 l of deionized water. Then 2 l of Co solution with 893.4 g of CoCl 2 * 6H 2 O were added quickly and the mixture was stirred for a further 10 min to complete the precipitation. After filtration and washing of the precipitate with deionized water (until chloride was no longer detectable in the outlet), the mixture was spray-dried and then in a tubular oven for 90 min at 420 ° C.
  • the resulting composite powder contained 8.24% Co, 5.63% total carbon, 0.06% carbon free (according to DIN ISO 3908), 0.395% oxygen and 0.0175% nitrogen.
  • the SEM images show a well deagglomerated mixture (FIG. 3) in SEI mode and a very uniform distribution of the cobalt in the composite powder (FIG. 4) in the case of emergence-dispersive evaluation.
  • a hard metal test was carried out with this powder under conditions similar to those in Example 1 and the following properties were measured on the resulting sintered body: density 14.71 g / cm 3 , coercive force 19.1 kA / m or 240 Oe, hardness HV30 1626 kg / mm 2 or HRA 92.0 , magnetic saturation 157.8 G cm 3 / g or 15.8 ⁇ Tm 3 / kg, low porosity A00 B02 C00 and a homogeneous, microdisperse structure.
  • the resulting composite powder contained 3.60% Co, 2.50% Ni, 2.56% Fe, 5.53% total carbon, 0.07% carbon free, 0.596% oxygen and 0.0176% nitrogen.
  • the SEM analysis shows a well deagglomerated composite powder (Fig. 5) with an even distribution of Fe, Co and Ni (Fig. 6-8).
  • the resulting composite powder had the following chemical composition: 4.46% Ni, 4.26% Fe, 5.52% total carbon, 0.08% carbon-free, 0.653% oxygen, 0.0196% nitrogen, the rest tungsten.
  • the SEM analysis shows a well deagglomerated powder (FIG. 9) with a uniform Fe and Ni distribution (FIGS. 10 and 11).
  • tungsten metal powder grade HC 100, supplier HCStarck
  • tungsten metal powder grade HC 100, supplier HCStarck
  • a solution of 1.592 kg of CuS0 4 * 5H 2 O in 6 l of deionized water was added and the precipitated suspension formed was stirred for a further 30 minutes to complete the precipitation and homogenize the suspension.
  • the precipitate was subsequently filtered, washed free of anions with deionized water, then spray-dried and reduced in a tubular oven at 500 ° C. for 120 minutes under hydrogen.
  • the resulting composite powder contained 80.78% W and 18.86% Cu in addition to a residual oxygen content of 0.37%.
  • the SEM analysis shows a very fine-grained powder (FIG. 12) and, in the case of energy-dispersive evaluation, a uniform distribution of the copper in the tungsten powder matrix (FIG. 13).

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP00991157A 1999-12-22 2000-12-11 Verfahren zur herstellung von pulvermischungen bzw. verbundpulver Expired - Lifetime EP1242642B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19962015 1999-12-22
DE19962015A DE19962015A1 (de) 1999-12-22 1999-12-22 Pulvermischungen bzw. Verbundpulver, Verfahren zu ihrer Herstellung und ihre Verwendung in Verbundwerkstoffen
PCT/EP2000/012484 WO2001046484A1 (de) 1999-12-22 2000-12-11 Pulvermischungen bzw. verbundpulver, verfahren zu ihrer herstellung und ihre verwendung in verbundwerkstoffen

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EP1242642A1 EP1242642A1 (de) 2002-09-25
EP1242642B1 true EP1242642B1 (de) 2003-10-01

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Country Status (16)

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US (1) US6887296B2 (pt)
EP (1) EP1242642B1 (pt)
JP (1) JP4969008B2 (pt)
KR (1) KR100747805B1 (pt)
CN (1) CN1159464C (pt)
AT (1) ATE251228T1 (pt)
AU (1) AU3156401A (pt)
CA (1) CA2394844A1 (pt)
CZ (1) CZ20022198A3 (pt)
DE (2) DE19962015A1 (pt)
ES (1) ES2208465T3 (pt)
IL (1) IL149808A (pt)
PL (1) PL356370A1 (pt)
PT (1) PT1242642E (pt)
TW (1) TWI232211B (pt)
WO (1) WO2001046484A1 (pt)

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CN107385302A (zh) * 2017-07-24 2017-11-24 苏州宏久航空防热材料科技有限公司 一种高硬度Ti（C,N）基金属陶瓷刀具复合材料
EP3527306A1 (de) * 2018-02-14 2019-08-21 H.C. Starck Tungsten GmbH Pulver umfassend beschichtete hartstoffpartikel
KR20210012013A (ko) 2018-05-30 2021-02-02 헬라 노벨 메탈스 엘엘씨 금속 화합물로부터의 미세 금속 분말의 제조 방법
US20210260652A1 (en) * 2018-06-20 2021-08-26 Desktop Metal, Inc. Methods and compositions for the preparation of powders for binder-based three-dimensional additive metal manufacturing
CN109175396B (zh) * 2018-11-15 2021-07-06 中南大学 一种纳米包覆复合粉末的制备方法
CN109530177B (zh) * 2018-11-26 2021-08-31 吉林大学 一种梯度功能化金刚石复合材料及其制备方法和应用
CN110014163A (zh) * 2019-04-19 2019-07-16 广东省材料与加工研究所 钨合金粉末及其制备方法和应用
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CN111745155B (zh) * 2020-07-10 2022-07-12 郑州机械研究所有限公司 低熔包覆合金粉末及其制备方法和铁基金刚石胎体
CN112935241A (zh) * 2021-01-23 2021-06-11 晋城鸿刃科技有限公司 成型剂以及硬质合金的成型方法
KR102305040B1 (ko) * 2021-06-23 2021-09-24 주식회사 스카이에스티 법랑분말과 Fe계 비정질 합금분말을 포함하는 혼합분말 및 이를 이용한 코팅방법
KR102305041B1 (ko) * 2021-06-23 2021-09-24 주식회사 스카이에스티 혼합분말을 이용한 백주철금속의 코팅방법
CN113857474A (zh) * 2021-09-01 2021-12-31 河海大学 一种添加Ce元素的WC表面包覆Co粉末制备方法
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ES2208465T3 (es) 2004-06-16
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TWI232211B (en) 2005-05-11
DE50003952D1 (de) 2003-11-06
WO2001046484A1 (de) 2001-06-28
PT1242642E (pt) 2004-02-27
JP4969008B2 (ja) 2012-07-04
IL149808A (en) 2005-09-25
KR100747805B1 (ko) 2007-08-08
CA2394844A1 (en) 2001-06-28
AU3156401A (en) 2001-07-03
EP1242642A1 (de) 2002-09-25
JP2003518195A (ja) 2003-06-03
DE19962015A1 (de) 2001-06-28
PL356370A1 (en) 2004-06-28
IL149808A0 (en) 2002-11-10
US20030000340A1 (en) 2003-01-02
CN1159464C (zh) 2004-07-28
CN1413268A (zh) 2003-04-23
US6887296B2 (en) 2005-05-03
CZ20022198A3 (cs) 2003-03-12

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