US20070199410A1 - Method For The Production Of Fine Metal Powder, Alloy Powder And Composite Powder - Google Patents

Method For The Production Of Fine Metal Powder, Alloy Powder And Composite Powder Download PDF

Info

Publication number
US20070199410A1
US20070199410A1 US10/563,982 US56398204A US2007199410A1 US 20070199410 A1 US20070199410 A1 US 20070199410A1 US 56398204 A US56398204 A US 56398204A US 2007199410 A1 US2007199410 A1 US 2007199410A1
Authority
US
United States
Prior art keywords
powder
grinding
group
alloy
particle diameter
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.)
Abandoned
Application number
US10/563,982
Other languages
English (en)
Inventor
Rolland Scholl
Dietmar Fister
Christian Spieker
Lam Dinh
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HC Starck GmbH
Original Assignee
HC Starck GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HC Starck GmbH filed Critical HC Starck GmbH
Assigned to H.C. STARCK GMBH reassignment H.C. STARCK GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FISTER, DIETMAR, DINH, LAM NGO, SCHOLL, ROLAND, SPIEKER, CHRISTIAN
Assigned to H.C. STARCK GMBH & CO. KG reassignment H.C. STARCK GMBH & CO. KG CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: H.C. STARCK GMBH
Assigned to H. C. STARCK GMBH & CO. KG reassignment H. C. STARCK GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH
Assigned to BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH reassignment BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH CORRECTIVE ASSIGNMENT TO CORRECT THE THE ASSIGNEE NEED TO BE CHANGED TO BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH PREVIOUSLY RECORDED ON REEL 018766 FRAME 0488. ASSIGNOR(S) HEREBY CONFIRMS THE CHANGE OF NAME. Assignors: H.C. STARK GMBH
Assigned to H.C. STARCK GMBH reassignment H.C. STARCK GMBH MERGER (SEE DOCUMENT FOR DETAILS). Assignors: H.C. STARCK GMBH & CO. KG
Publication of US20070199410A1 publication Critical patent/US20070199410A1/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • 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

Definitions

  • the invention relates to a method for producing metal, alloy or composite powders with a mean particle diameter D50 of at most 25 ⁇ m, a starting powder firstly being formed into flake-like particles and these then being comminuted in the presence of grinding aids, and to metal, alloy or composite powders obtainable thereby.
  • the powder particles form directly from the produced melt droplets by solidification.
  • Powder production by atosation primarily has the drawback that large quantities of energy and atomising gas have to be used, and this renders the procedure very expensive.
  • production of fine powder from high melting alloys with a melting point>1,400° C. is not very economical as, on the one hand, the high melting point necessitates a very high application of energy for producing the melt and, on the other hand, the gas consumption greatly increases as the desired particle size decreases.
  • melt-spinning i.e. pouring a melt onto a cooled roll, whereby a thin, usually easily comminutable strip is produced
  • crucible melt extraction i.e. the immersion of a cooled profiled roll rotating at high speed into a molten metal, wherein particles or fibres are obtained.
  • a further important variant of powder production is the chemical method via reduction of metal oxides or metal salts.
  • alloy powders it is not possible to obtain alloy powders in this manner (W. Schatt, K.-P. Wieters in “Powder Metallurgy—Processing and Materials”, EPMA European Powder Metallurgy Association, 1997, 23 to 30).
  • Extremely fine particles which have particle sizes of less than one micrometre may also be produced by the combination of evaporation and condensation of metals and alloys and via gas phase reactions (W. Schatt, K.-P. Wieters in “Powder Metallurgy—Processing and Materials”, EPMA European Powder Metallurgy Association, 1997, 39 to 41). These methods are very expensive, however.
  • a method of fine comminution of relatively brittle pre-comminuted material that is particularly suitable in many cases involves the concept of gas contra-jet mills of which there are numerous commercial suppliers, for example Hosokawa-Alpine or Netzsch-Condux.
  • This method is prevalent and provides, in particular in the case of brittle materials, considerable advantages from industrial (low level of impurities, autogenic grinding) and financial perspectives compared to conventional mills using purely mechanical comminution, such as ball mills or agitated ball mills.
  • Jet mills attain their industrial and thus their financial limits with comminution of ductile starting powders, in other words materials that are difficult to comminute, and low designated particle sizes. This is explained by the decreasing kinetic energy of the powder particles being comminuted in the gas jet.
  • Very fine particles may be obtained, for example, by combining grinding steps with hydrogenation and dehydrogenation reactions, including the combination of reaction products to form the desired phase composition of the powder (I. R. Harris, C. Noble, T. Bailey, Journal of the Less Common Metals, 106 (1985), L1 to L4).
  • this method is limited to alloys which contain elements that may form stable hydrides. Mechanical influences on the comminution in the form of lattice defects or other defects may thus be substantially avoided. This is particularly important if the functional properties of the powder particles, for example the crystallites, critically affect the properties of the powder product, such as in NdFeB permanent magnets.
  • the coldstream process was developed for producing products of this type, metallic particles subjected to intense cooling being centriged at extremely high speeds of up to 1 Mach via a venturi tube onto a cooled panel. It is thus allegedly possible to produce a product with a particle size between 5 and 10 ⁇ m (W. Schatt, K.-P. Wieters in “Powder Metallurgy—Processing and Materials”, EPMA European Powder Metallurgy Association, 1997, 9 to 10).
  • the act of accelerating the starting powder to the speed of sound necessitates an extremely high application of energy in this method.
  • abrasion problems may occur and, owing to the interaction between particles and counterplate, critical impurities are introduced into the grinding stock.
  • a further method for producing fine powder from ductile material is mechanical alloying.
  • agglomerates are obtained by intensive grinding treatment, which agglomerates are made up of crystallites that are approximately 10 to 0.01 ⁇ m in size.
  • the metallic ductile material changes as a result of the high mechanical stress in such a way that fine individual particles may possibly form. These contain the composition typical of the alloy.
  • the drawback of this process is that considerable impurities are sometimes introduced, primarily by abrasion. Usually, however, it is precisely the uncontrolled abrasion that is an obstacle to industrial use.
  • discrete superfine particles are only produced after a very long grinding period. Fine metal and alloy powders therefore cannot be economically produced by mere mechanical alloying.
  • the object of the present invention therefore consists in providing a process for producing fine, in particular ductile, metal, alloy or composite powders, the method being particularly suitable for producing alloys, i.e. multi-component systems, and allowing fundamental properties, such as particle size, particle size distribution, sintering activity, impurity content or particle morphology to be purposefully adjusted or influenced.
  • the object is achieved according to the invention by a two-stage method, a starting powder firstly being formed into flake-like particles and these then being comminuted in the presence of grinding aids.
  • the invention therefore relates to a method for producing metal, alloy or composite powders with a mean particle diameter D50 of at most 25 ⁇ m, determined using the particle measuring apparatus Microtrac® X 100 to ASTM C 1070-01, from a starting powder with a greater mean particle diameter, wherein
  • the particle measuring apparatus Microtrac® X 100 is commercially available from Honeywell, U.S.A.
  • the particle diameter and the particle thickness are determined using a light-optical microscope.
  • the flake-like powder particles are firstly mixed with a viscous, transparent epoxy resin in a ratio of 2 volume fractions resin and 1 volume fraction flakes.
  • the air bubbles introduced during mixing are then expelled by evacuation of this mixture.
  • the then bubble-free mixture is poured over a planar substrate and then rolled out using a roller.
  • the flake-like particles are thus oriented in the flow field between roller and substrate.
  • the preferred position manifests itself in that the surface normals of the flakes are oriented on average parallel to the surface normals of the planar substrate, in other words the flakes are arranged in layers on average flat on the substrate.
  • suitable samples of suitable dimensions are worked from the epoxy resin plate on the substrate.
  • the samples are microscopically examined perpendicularly and parallel to the substrate.
  • the particle thicknesses are determined using the microscope with a calibrated lens, which microscope was also used to determine the particle diameter. Care should be taken that only particles located optimally parallel to the substrate are measured. As the particles are completely surrounded by the transparent resin, selecting suitably oriented particles and reliably assigning the limitations of the particles to be evaluated do not present any difficulties.
  • at least 50 particles are measured and an average formed from the measured values. This average represents the particle thickness of the flake-like particles.
  • the particle diameter to particle thickness ratio is calculated from the previously ascertained values.
  • ductile metal, alloy or composite powders may be produced with the method according to the invention.
  • Ductile metal, alloy or composite powders are in his case taken to mean those powders which, in the event of mechanical stress until the yield point is reached, undergo plastic expansion or deformation before significant material damage (material embrittlement, material rupture) occurs.
  • Plastic material changes of this type are dependent on the material and are in the range of 0.1 per cent up to several 100 per cent, based on the starting length.
  • the degree of ductility i.e. the capacity of materials to plastically, i.e. permanently, deform under the effect of mechanical stress may be determined or described by mechanical tensile or pressure testing.
  • a tensile sample is produced from the material to be assessed. This may be, for example, a cylindrical sample which, halfway along its length, has a reduction in diameter of approximately 30 to 50% over a length of approximately 30 to 50% of the total sample length.
  • the tensile sample is fixed in a fixing device of an electromechanical or electrohydraulic tensile testing machine.
  • Length sensors are installed on average of the sample over a measuring length which is approximately 10% of the overall sample length, before actual mechanical testing. These sensors allow the increase in the length to be followed in the selected measuring length during application of a mechanical tensile stress. The stress is increased until the sample fractures and the plastic content of the change in length is evaluated using the stress-strain recording. Materials which achieve a plastic change in length of at least 0.1% in an arrangement of this type will be called ductile in the context of this specification.
  • Fine ductile alloy powders which have a degree of ductility of at least 5% are preferably produced by the method according to the invention.
  • the capacity for comminution of alloy or metal powders that cannot be comminuted further per se is improved by the use of mechanically, mechanochemically and/or chemically acting grinding aids which are purposefully added or produced in the grinding process.
  • a fundamental aspect of this approach is that the chemical “desired composition” of the powder thus produced cannot be changed overall or influenced even such that the processing properties, such as the sintering behaviour or flowability, are improved.
  • the method according to the invention is suitable for producing a wide variety of fine metal, alloy or composite powders with a mean particle diameter D50 of at most 25 ⁇ m.
  • metal, alloy or composite powders of a composition corresponding to formula I hA-iB-jC-kD (I) may be obtained, wherein
  • h preferably represents 50 to 80% by weight, in particular preferably 60 to 80% by weight.
  • i preferably represents 15 to 40% by weight, in particular preferably 18 to 40% by weight.
  • j preferably represents 0 to 15% by weight, in particular preferably 5 to 10% by weight.
  • k preferably represents 0 to 5% by weight, in particular preferably 0 to 2% by weight.
  • the metal, alloy or composite powders produced according to the invention are distinguished by a small mean particle diameter D50.
  • the mean particle diameter D50 is preferably at most 15 ⁇ m, determined to ASTM C 1070-01 (measuring apparatus: Microtrac® X 100).
  • powders which already have the composition of the desired metal, alloy or composite powder may be used as the starting powder.
  • the composition of the produced metal, alloy or composite powder may also be influenced by the choice of grinding aid, if this remains in the product.
  • Powders with spherical or irregularly shaped particles and a mean particle diameter D50, determined to ASTM C 1070-01 of greater than 25 ⁇ m, preferably 30 to 2,000 ⁇ m, in particular preferably 30 to 1,000 ⁇ m, are preferably used as the starting powders.
  • the required starting powders may be obtained, for example, by atomisation of molten metals and, if necessary, subsequent screening or sifting.
  • the starting powder is firstly subjected to a deformation step.
  • the deformation step may be carried out in known devices, for example in a rolling mill, an eddy mill, a high-energy mill or an attritor or an agitated ball mill.
  • the process engineering parameters in particular as a result of the effect of mechanical stresses which are sufficient to achieve plastic deformation of the material or the powder particles, the individual particles are deformed, so they ultimately have a flake-like form, the thickness of the flakes preferably being 1 to 20 ⁇ m.
  • This may take place, for example, by one-off stressing in a roller or a hammer mill, by repeated stressing in “small” deformation steps, for example by percussive grinding in an eddy mill or a Simoloyer®, or by a combination of percussive and frictional grinding, for example in an attritor or a ball mill.
  • the high material stress during this deformation may lead to structural damage and/or material embrittlement which may be used in the following steps for comminuting the material.
  • Known molten metallurgical fast solidification processes may also be used for producing strips or “flakes”. These, like the mechanically produced flakes, are then suitable for comminution grinding described below.
  • the grinding media and the other grinding conditions are preferably selected such that the impurities as a result of abrasion and/or reactions with oxygen or nitrogen are as small as possible and below the critical value for the application of the product or are within the specification relevant to the material.
  • the flake-like particles are produced in a fast solidification step, for example by what is known as “melt spinning”, directly from the melt by cooling on or between one or more, preferably cooled roller(s), so flakes are directly formed.
  • the flake-like particles obtained in the deformation step are subjected to comminution grinding.
  • the particle diameter to particle thickness ratio changes, primary particles with a particle diameter to particle thickness ratio of 1:1 to 10:1 usually being obtained and, on the other hand, the desired mean particle diameter of at most 25 ⁇ m is adjusted without particle agglomerates that are difficult to comminute occurring again.
  • Comminution grinding may take place for example in a mill, for instance an eccentric mill, but also in Gutbett rolls, extruders or similar devices which bring about material shattering owing to different movement and stress rates in the flake.
  • comminution grinding is carried in the presence of a grinding aid.
  • a grinding aid Liquid grinding aids, waxes and/or brittle powder for example, may be used as the grinding aid.
  • the grinding aids may act mechanically, chemically or mechanochemically.
  • the grinding aid may be paraffin oil, paraffin wax, metal powder, alloy powder, metal sulphides, metal salts, salts of organic acids and/or hard material powder.
  • Brittle powder or phases act as mechanical grinding aids and may be used, for example, in the form of alloy, element, hard material, carbide, silicide, oxide, boride, nitride or salt powder.
  • pre-comminuted element and/or alloy powders are used which, together with the starting powder used, which is difficult to comminute, produce the desired composition of the product powder.
  • Brittle powders used are preferably those which comprise binary, ternary and/or higher compositions of the elements A, B, C and/or D that occur in the starting alloy used, A, B, C and D having the meanings given above.
  • Liquid and/or easily deformable grinding aids for example waxes, may also be used.
  • Other examples include hydrocarbons, such as hexane, alcohols, amines or aqueous media. These are preferably compounds which may be required for the following steps of further processing and/or which may be easily removed after comminution grinding.
  • grinding aids are used which enter a targeted chemical reaction with the starting powder to achieve the grinding progress and/or for adjusting a specific chemical composition.
  • These may be, for example, decomposable chemical compounds, of which only one or more constituents are required for adjusting a desired composition, it being possible to substantially remove at least one component or constituent by a thermal process.
  • Reducible and/or decomposable compounds such as hydrides, oxides, sulphides, salts and sugars are mentioned as examples which are at least partially removed from the grinding stock in a subsequent processing step and/or powder metallurgical processing of the product powder, the remaining residue chemically complementing the powder composition in the desired manner.
  • the grinding aid is not added separately but is produced in situ during comminution grinding.
  • the procedure may, for example, be such that the grinding aid is produced by adding a reactive gas which reacts under the conditions of comminution grinding with the starting powder while forming a brittle phase. Hydrogen is preferably used as the reactive gas.
  • the brittle phases which are produced during treatment with the reactive gas may usually be removed again by appropriate method steps after comminution grinding or during processing of the fine metal, alloy or composite powder obtained.
  • grinding aids which are not removed, or are only partially removed, from the metal, alloy or composite powder produced according to the invention, they are preferably selected such that the remaining constituents affect a property of the material in a desired manner, such as improving the mechanical properties, reducing the corrodibility, increasing the hardness and improving the abrasion behaviour or the frictional and sliding properties.
  • a hard material is mentioned here by way of example, which is increased in content in a subsequent step to the extent that the hard material may be further processed with the alloy component to form a hard metal or a hard material alloy composite.
  • the primary particles of the metal, alloy or composite powder produced have, according to the invention, a mean particle diameter D50, determined to ASTM C 1070-01 (Microtrac® X 100), of at most 25 ⁇ m.
  • the known interactions between superfine particles can lead to the formation of relatively coarse secondary particles (agglomerates), of which the particle diameter is far greater than the desired mean particle diameter of at most 25 ⁇ m, despite the use of grinding aids.
  • a deagglomeration step therefore preferably follows comminution grinding, during which the agglomerates are broken open and the primary particles liberated.
  • Deagglomeration may, for example, take place by applying shear forces in the form of mechanical and/or thermal stresses and/or by removing separation layers previously introduced in the process between primary particles.
  • the deagglomeration methods to be applied in particular are oriented toward the degree of agglomeration, the intended used and the susceptibility to oxidation of the superfine powder and the admissible impurities in the finished product.
  • Deagglomeration may, for example, take place by mechanical methods, for instance by treatment in a gas contrajet mill, screening, sieving or treatment in an attritor, a kneader or a rotor-stator dispergator.
  • a stress field as generated in ultrasound treatment
  • thermal treatment for example dissolution or conversion of a previously introduced separating layer between the primary particles by cryo- or high-temperature treatments, or a chemical conversion of introduced or purposefully produced phases, is also possible.
  • Deagglomeration is preferably carried out in the presence of one or more liquids, dispersing aids and/or binders.
  • a slurry, a paste, a kneading compound or a suspension with a solids content between 1 and 95% by weight may thus be obtained.
  • Solids contents between 30 and 95% by weight may be directly processed by known powder technological processes such as injection moulding, film casting, coating, and hot-moulding, and are then reacted in suitable steps of drying, releasing and sintering to form an end product.
  • a gas contrajet mill which is operated under inert gases, such as argon or nitrogen, is preferably used for deagglomeration of particularly oxygen-sensitive powders.
  • the metal, alloy or composite powders produced according to the invention are distinguished from conventional powders with identical mean particle diameters and identical chemical composition which are produced, for example, by atomisation, by a range of particular properties.
  • the invention therefore also relates to metal, alloy or composite powders with a mean particle diameter D50 of at most 25 ⁇ m, determined using the particle measuring apparatus Microtrac® X 100 to ASTM C 1070-01, which are obtainable by the method according to the invention.
  • the metal, alloy and composite powders according to the invention exhibit, for example, excellent sintering behaviour.
  • the same sintering densities may be attained as in powders produced by atomisation.
  • higher sintering densities may be achieved at the same sintering temperature.
  • This increased sintering activity is also exhibited, for example, in the fact that, until the maximum contraction is attained, the contraction during the sintering process is greater than in conventionally produced powders.
  • the invention therefore also relates to metal, alloy or composite powders with a mean particle diameter D50 of at most 25 ⁇ m, determined using the particle measuring device Microtrac® X 100 to ASTM C 1070-01, wherein, until the maximum contraction is attained, the contraction, determined using a dilatometer to DIN 51045-1 has at least 1.05 times the contraction of a metal, alloy or composite powder with identical chemical composition and identical mean particle diameter D50, the powder to be investigated being compressed to a compressed density of 50% of the theoretical density before the contraction is measured.
  • the powder to be investigated may be compressed by adding conventional compression-assisting agents, such as paraffin wax or other waxes or salt or organic acids, for example zinc stearate,
  • Metal alloy or composite powders which are produced by atomisation and by comparison with which the powders according to the invention have improved sintering behaviour are to be taken to mean those powders which are produced by conventional atomisation known to the person skilled in the art.
  • the advantageous sintering behaviour of the metal, alloy or composite powders according to the invention may also be recognised in the course of sintering and contraction curves, as shown, for example, in FIG. 7 .
  • FIG. 7 shows, for a comparison powder (V) and a powder (PZD) according to the invention, the course of the contraction S or the contraction rate AS in each case in relative units as a function of the temperature T N standardised to the respective sintering temperature T S .
  • the comparison powder (V) is a product produced by atomisation under inert conditions and with a composition corresponding to that of the material described in Example 1 and the morphology of this powder.
  • the particle size distribution (D50 approximately 8.4 ⁇ m) corresponds to that as shown in FIG. 5 .
  • the powder (PZD) according to the invention is a powder produced according to Example 1 with the morphology illustrated in FIG. 6 and an oxygen content of 0.4% by weight.
  • microwax as the compression-facilitating additive powder compacts were produced from the two powders in a compression mould by applying a single-axle pressure of 400 to 600 mPa.
  • the green density was in both cases approx. 40% of the theoretical density.
  • These compacts were accordingly sintered individually in a dilatometer to DIN 51045-1 under protective gas conditions and using argon as the process gas. Heating at a rate of approx. 1 K/min (corresponding to approx. 6 * 10 ⁇ 4 *T S /min where T S : approx. 1,600 K) took place in the process.
  • the push rod of the dilatometer does not exert any pressure on the sample which supplies a measurable quantity for sintering contraction in the temperature range that is of interest for sintering (approx. 0.5 T S to approx. 0.95 T S ).
  • the organic pressing aid is expelled to a temperature of approximately 0.45 * T S .
  • the actual sintering process takes place thereafter by further heating at the same heating rate from approx. 0.5 T S to approx. 0.99 T S .
  • the metal, alloy and composite powders according to the invention are distinguished, owing to a particular particle morphology with rough particle surface, moreover by outstanding compression behaviour and, owing to a comparatively broad particle size distribution, by high compressed density. This manifests itself in that compacts made of atomised powder have a lower bending strength, under otherwise identical production conditions, than the compacts made of powders according to the invention and with the same chemical composition and mean particle size D50.
  • a further improvement in the compression behaviour may be achieved if powder mixtures comprising 1 to 95% by weight metal, alloy or composite powders according to the invention and 99 to 5% by weight atomised powder are used.
  • the sintering behaviour of powders produced according to the invention may also be purposefully influenced by the choice of grinding aid.
  • one or more alloys which, owing to their low melting point compared to the starting alloy form liquid phases during heating which improve the particle rearrangement and the material diffusion and thus the sintering behaviour and the contraction behaviour and thus allow higher sintering densities to be attained at the same sintering temperature or at lower sintering temperatures the same sintering density as may be achieved with the comparison powders, may be used as the grinding aid.
  • Chemically decomposable compounds, of which the decomposition products with the basic material produce liquid phases or phases with increased diffusion coefficients which facilitate compression, may also be used.
  • X-ray analyses of the metal, alloy or composite powders according to the invention show a propagation of X-ray reflexes compared with X-ray reflexes that are obtained for powders with the same mean particle diameter and the same chemical composition which were obtained by atomisation.
  • the propagation is demonstrated by the propagation of half widths.
  • the half widths of the X-ray reflexes are propagated by a factor >1.05. This is caused by the mechanical stressed stated of the particles, the existence of a higher dislocation density, i.e. disturbances to the solid in the atomic range, and the crystallite size in the particles.
  • alloy- and/or process-induced phases occur in the diffractograms in addition to the propagations of the X-ray reflexes of the main phase, which phases are significant for the contraction properties.
  • the method according to the invention allows production of metal, alloy and composite powders, in which oxygen, nitrogen, carbon, boron and silicon contents are purposefully adjusted.
  • Oxide and/or nitride phases may form in the case of introduction of oxygen or nitrogen as a result of the high application of energy. Phases of this type may be desirable for specific applications as they may lead to strengthening of material. This effect is known as the “particle dispersion strengthening” effect (PDS effect).
  • PDS effect particle dispersion strengthening
  • the introduction of such phases is often associated with a deterioration in the processing properties (for example compressibility, sintering activity). Owing to the generally inert properties of the dispersoids with respect to the alloy components, the latter may therefore have a sintering-inhibiting effect.
  • phases are immediately superfinely distributed in the produced powder.
  • the phases formed (for example oxides, nitrides, carbides, borides) are therefore much more finely and homogeneously distributed in the metal, alloy and composite powders according to the invention than in conventionally produced powders. This again leads to increased sintering activity compared with discretely introduced phases of the same kind.
  • the processing properties of the metal, alloy and composite powders according to the invention may often be improved even further by adding metal, alloy or composite powders conventionally produced, in particular by atomisation.
  • MIM metal powder injection moulding
  • the invention therefore also relates to mixtures containing 1 to 95% by weight of a metal, alloy or composite powder and 99 to 5% by weight of a conventionally produced metal, alloy or composite powder.
  • the mixtures according to the invention preferably contain 10 to 70% by weight of a metal, alloy or composite powder according to the invention and 90 to 30% by weight of a conventionally produced metal, alloy or composite powder.
  • the conventionally produced metal, alloy or composite powder according to the invention is preferably a powder which has been produced by atomisation.
  • the conventionally produced metal, alloy or composite powder may have the same chemical composition as the PZD powder contained in the mixture. Mixtures of this type are distinguished from pure PZD powders in particular by a further improvement in compression behaviour.
  • PZD powder and conventionally produced powder have a different chemical composition in the mixture.
  • the composition may be purposefully changed and as a result specific powder properties and consequently the material properties may be purposefully adjusted.
  • the mean particle diameters D50 given in the examples were determined using a Microtrac® X 100 from Honeywell, U.S.A. to ASTM C 1070-01.
  • the alloy powder obtained was screened between 53 and 25 ⁇ m. The density was approx. 8.2 g/cm 3 .
  • the staring powder had substantially spherical particles, as may clearly be seen in FIG. 1 (scanning electron microscope image (SEM image) magnified 300 times).
  • the starting powder was subjected to deformation grinding in a vertical agitated ball mill (Netzsch Feinmahltechik; PR 1S type), so the originally spherical particles assumed flake-like forms.
  • the following parameters were used in particular:
  • FIG. 2 is a SEM image magnified 300 times of the flakes produced in the deformation step.
  • the high degree of material deformation, which was caused by the specific grinding treatment, compared with the starting powder may be seen. Damage to the structure of the material (crack formation) may also clearly be seen.
  • FIG. 3 is a SEM image magnified 1,000 times of the product obtained.
  • the cauliflower-like structure of the agglomerate (secondary particle) may be seen, the primary particles having particle diameters of much less than 25 ⁇ m.
  • a sample of the primary particles or superfine particle agglomerates was subjected in a third method step to deagglomeration by ultrasound treatment in isopropanol in an ultrasonic device TG 400 (Sonic Ultraschallanlagenbau GmbH) lasting 10 minutes at 50% maximum power to obtain separated primary particles.
  • TG 400 Sonic Ultraschallanlagenbau GmbH
  • the particle size distribution of the deagglomerated sample was determined using a Microtrac® X 100 (manufacturer: Honeywell, U.S.A.) to ASTM C 1070-01.
  • FIG. 4 shows the particle size distribution thus obtained.
  • the D50 value of the starting powder was 40 ⁇ m and was reduced to approx 15 ⁇ m by the treatment according to the invention.
  • the remaining quantity of primary particles from comminution grinding were subjected in an alternative third method step to deagglomeration by treatment in a gas contrajet mill and subsequent ultrasound treatment in isopropanol in an ultrasonic device TG 400 (Sonic Ultaschallanagenbau GmbH) at 50% of the maximum power.
  • the particle size was again determined using a Microtrac® X 100.
  • FIG. 5 shows the particle size distribution obtained.
  • the D50 value was then only 8.4 ⁇ m. This proves the possibility of further increasing the fine fraction in the powder produced according to the invention by high-energy post-treatment.
  • FIG. 6 shows a SEM image ( ⁇ 600 magnification) of the powder after treatment in the gas contrajet mill.
  • the introduced grinding aid paraffin may be removed during powder metallurgical further processing of the alloy powder by thermal decomposition and/or evaporation and may be used as a compression aid.
  • Comminution grinding was then carried out in an eccentric vibration grinding mill, as described in Example 1.
  • the composition of the grinding aid used is summarised in Table 1.
  • a mixture containing 65% by weight Fe, 24% by weight Cr, 10% by weight Al and 1% by weight Y was obtained.
  • the chemical composition of the starting powder is accordingly not altered by the choice of given alloy contents.
  • a specific distribution of the components used (starting powder, grinding aid) is present in the composite powder obtained as a result of production according to the invention, so the composite powder undergoes a metallurgical change during further processing, for example by sintering or another thermal process.
  • a composite powder with a mean particle diameter D50 of 15 ⁇ m was obtained after comminution grinding and deagglomeration in an ultrasonic field. It was possible to obtain an alloy in the metallurgical sense from a composite powder of this type by thermal post-treatment.
  • Example 2 In contrast to Example 2, a change in the chemical composition was desired or allowed during the grinding operation.
  • An atonised alloy of composition Fe25,6Cr10,67Al with a mean particle diameter D50 of 40 ⁇ m was subjected to a deformation step under the conditions described in Example 1. Flake-like particles with a mean particle diameter D50 of 70 ⁇ m were obtained, of which the appearance did not significantly differ from that in Example 1.
  • Comminution grinding was then carried out.
  • the procedure corresponded to that in Example 1 but 10 g of a Fe16Y powder with a mean particle diameter D50 of 40 ⁇ m were used as the grinding aid and the grinding lasted 2 hours.
  • Table 2 gives the composition and quantity of flake-like starting alloy and the grinding aid added for comminution grinding. TABLE 2 Composition of the flake-like starting alloy and mechanical grinding aid used Component Quantity [g] Fe [g] Cr [g] Al [g] Y [g] Fe25,6Cr10,67Al 150 95.6 38.4 16.0 0 Fe16Y 10 8.4 0 0 1.6 Total 160 104 38.4 16.0 1.6
  • the composite powder obtained had the composition Fe24Cr10Al1Y.
  • the composite powder was subjected to an ultrasound treatment after which a composite powder with a mean particle diameter D50 of 13 ⁇ m was obtained.
  • Example 3 The procedure was as in Example 3, a mixture of a plurality of brittle materials and pure iron powder being used as the grinding aid.
  • Table 3 contains the composition and original weighed in quantities of the starting powder and grinding aid.
  • the brittle grinding aids Fe60Al, Fe70Cr and Y2, 2H were brought to a mean particle diameter D50 of 40 ⁇ m before use in a separate grinding step.
  • the Fe powder used had a mean particle diameter D50 of 10 ⁇ m.
  • the composite powder obtained had the composition Fe24Cr10Al1Y.
  • the composite powder was subjected to an ultrasound treatment after which a composite powder with a mean particle diameter D50 of 15 ⁇ m was obtained.
  • the particularly brittle Fe16Y alloy was used as the only grinding aid during subsequent comminution grinding, which alloy had previously been comminuted to a mean particle diameter D50 of approx. 40 ⁇ m.
  • the procedure was as in Example 1, grinding lasting 2.5 hours.
  • Table 4 contains the composition and original weighed in quantities of the two flake-like FeCrAl starting alloys and of the brittle grinding aid (Fe16Y). TABLE 4 Composition of the flake-like starting alloys and the mechanical grinding aid used Component Quantity [g] Fe [g] Cr [g] Al [g] Y [g] Fe19,9Cr24,8Al 43 23.8 8.6 10.5 0 Fe27,9Cr5Al 107 71.8 29.8 5.5 0 Fe16Y 10 8.4 0 0 1.6 Total 160 104 38.4 16 1.6
  • the composite powder obtained had the composition Fe24Cr10Al1Y.
  • the composite powder was subjected to an ultrasound treatment after which a composite powder with a mean particle diameter D50 of 12 ⁇ m was obtained.
  • Ni15Co10Cr5,5Al4,8Ti3Mo1V alloy which is commercially available under the model name IN 100®, was subjected, as described in Example 1, to a deformation step under an inert atmosphere.
  • the chemical composition of the resultant superfine powder differed only slightly from that of the starting powder.
  • the hydrogen content rose to ⁇ 1,000 ppm.
  • the hydrogen content fell to below approx. 50 ppm again as a result of sintering under vacuum.
  • Spherical atomised Ni38Cr8,7Al1,09Hf with a mean particle diameter D50 of 40 ⁇ m was subjected, as described in Example 1, to a deformation step.
  • Spherical atomised Ni38Cr8,7Al1,09Hf with a mean particle diameter D50 of 40 ⁇ m was subjected, as described in Example 7 by using an attritor (agitated ball mill), to a deformation step.
  • an alloy powder with a mean particle diameter D50 of 13 ⁇ m, measured by Microtrac® X 100 was obtained.
  • the silicon used in this case was desirable or necessary in terms of alloy engineering in order to adjust the end composition Ni38Cr8,7Al1,09Hf and in terms of process engineering for attaining the desired grinding effect.
  • tat may be considered silicon is best suited as the grinding aid owing to its brittleness. This grinding process led to an increase in the oxygen content in the powder. At the conclusion of the grinding process the oxygen content was 0.4% by weight.
  • the flake-like particles obtained were comminution ground in an eccentric vibration grinding mill in the presence of tungsten carbide as the grinding aid and under the following conditions:
  • the result of comminution grinding was an alloy hard material composite powder in which the alloy components had been comminuted to a mean particle diameter D50 of approx. 5 ⁇ m and the hard material component to a mean particle diameter D50 of approx. 1 ⁇ m.
  • the hard material particles were substantially homogenously distributed in the alloy powder volume.
  • the alloy hard material composite powder could be processed by conventional process steps to form a spray powder,
  • 797 g WC with a mean particle diameter D50 to ASTM B 330 (FSSS) of 1 ⁇ m, ethanol, PVA (polyvinyl alcohol) and suspension stabilisers were added to 163 g of the alloy hard material composite powder produced according to the invention for dispersing and generating a suspension.
  • a suspension was produced which consisted to 25 vol. % of the metallic binding phase and to 75 vol. % of the WC hard material phase.
  • This suspension was further processed by spray granulation and classification to form a green spray powder with a particle size of 20 to 63 ⁇ m.
  • the organic auxiliaries were firstly removed from this green spray powder by gas evolution at 100 to 400° C.
  • Titanium powder with a mean particle diameter D50 of 100 ⁇ m was processed according to the invention and analogously to Example 1 to form flakes.
  • the flakes were then further processed in a comminution step analogously to Example 1, 10 g TiH 2 being added as the grinding agent to the Ti flakes used (original weighed in quantity: 150 g). After comminution grinding there was a fine titanium powder with a mean particle diameter D50 of approx. 15 ⁇ m.
  • the titanium powder produced according to the invention could be further processed by conventional process steps to form mould parts.
  • the titanium powder produced according to the invention was stored in an organic solvent, for example n-hexane.
  • organic solvent for example n-hexane.
  • the paraffin was dissolved for example in n-hexane, added to the powder and the n-hexane was then evaporated with continuous circulating of the powder. A superficial seal against uncontrolled absorption of oxygen was obtained thereby and the improvement in compressibility achieved. This procedure allows the titanium powder to be processed in air.
  • the flakes had a particle diameter to particle thickness ratio of approx. 1,000:1 and a mean particle diameter D50 of 150 ⁇ m.
  • the contrajet mill was operated with inert gas.
  • Atomised spherical material, which had not been pre-treated, of the same alloy with a particle diameter between 100 and 63 ⁇ m was used as the grinding aid.
  • the grinding chamber (volume: approx. 51) was filled with 2.51 powder bulk volume (67% by weight grinding aid and 33% by weight flakes) and the grinding process initiated.
  • the fine fraction produced was separated at 10 ⁇ m by corresponding adjustments of a sifter connected downstream of the mill.
  • Hastelloy® An atomised Ni17Mo15Cr6Fe5W1Co alloy with a mean particle diameter of 100 to 63 ⁇ m, which is commercially available under the name Hastelloy®, was mechanically treated in a high energy mill (eccentric vibration mill) under the following conditions:
  • Flakes were produced which had a diameter to thickness ratio of 1:2 and a flake thickness of approx. 20 ⁇ m.
  • Comminution grinding then took place in a gas contrajet mill. During comminution particles which had a particle diameter of ⁇ 20 ⁇ m were removed by suitably adjusting a sifter connected downstream. A fine alloy powder which, after ultrasound treatment, had a mean particle diameter D50 of 12 ⁇ m and a D90 value of 20 ⁇ m, determined using a Microtrac® X 100, was thus produced.

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
US10/563,982 2003-07-11 2004-07-06 Method For The Production Of Fine Metal Powder, Alloy Powder And Composite Powder Abandoned US20070199410A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10331785A DE10331785B4 (de) 2003-07-11 2003-07-11 Verfahren zur Herstellung feiner Metall-, Legierungs-und Verbundpulver
DE10331785.6 2003-07-11
PCT/EP2004/007365 WO2005007327A2 (de) 2003-07-11 2004-07-06 Verfahren zur herstellung feiner metall-, legierungs- und verbundpulver

Publications (1)

Publication Number Publication Date
US20070199410A1 true US20070199410A1 (en) 2007-08-30

Family

ID=34071652

Family Applications (1)

Application Number Title Priority Date Filing Date
US10/563,982 Abandoned US20070199410A1 (en) 2003-07-11 2004-07-06 Method For The Production Of Fine Metal Powder, Alloy Powder And Composite Powder

Country Status (16)

Country Link
US (1) US20070199410A1 (ru)
EP (1) EP1646465A2 (ru)
JP (1) JP2007528936A (ru)
KR (1) KR20060026961A (ru)
CN (1) CN1863628A (ru)
AU (1) AU2004257411B2 (ru)
BR (1) BRPI0412509A (ru)
CA (1) CA2531683A1 (ru)
DE (1) DE10331785B4 (ru)
IL (1) IL173056A (ru)
MX (1) MXPA06000361A (ru)
NO (1) NO20060628L (ru)
RU (1) RU2367542C2 (ru)
SG (1) SG147433A1 (ru)
WO (1) WO2005007327A2 (ru)
ZA (1) ZA200600252B (ru)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090011252A1 (en) * 2007-04-13 2009-01-08 Gotz Matthaus Process for applying a multilayered coating to workpieces and/or materials
US20090252634A1 (en) * 2006-07-12 2009-10-08 Roland Scholl Metallic powder mixtures
US20090277301A1 (en) * 2006-07-12 2009-11-12 H.C. Starck Gmbh Metallic powder mixtures
US20100003157A1 (en) * 2006-07-12 2010-01-07 H.C. Starck Gmbh Metallic powder mixtures
US20100047622A1 (en) * 2006-09-22 2010-02-25 H.C. Starck Gmbh Metal powder
US20100107816A1 (en) * 2008-10-30 2010-05-06 Henning Zoz Method of making metal flakes
CN105506382A (zh) * 2015-12-21 2016-04-20 常熟市梅李合金材料有限公司 高电阻电热合金丝
CN106166616A (zh) * 2016-09-29 2016-11-30 柳州增程材料科技有限公司 一种3d打印用金属粉末的制备方法
CN106216698A (zh) * 2016-09-29 2016-12-14 柳州增程材料科技有限公司 一种3d打印用合金粉末的制备工艺
WO2019023123A1 (en) * 2017-07-24 2019-01-31 United States Of America, As Represented By The Secretary Of The Army ALUMINUM NANOGALVANIC COMPOSITIONS USEFUL FOR THE PRODUCTION OF HYDROGEN GASES AND THEIR TREATMENT AT LOW TEMPERATURE
CN113617493A (zh) * 2021-06-29 2021-11-09 南京信彩科技有限公司 一种彩色油墨制备用原料研磨方法
US11559837B2 (en) * 2018-04-04 2023-01-24 Metal Powder Works, LLC System and method for powder manufacturing

Families Citing this family (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2006062039A1 (ja) * 2004-12-06 2008-06-05 サンレックス工業株式会社 金属製品の製造方法および金属製品
DE102005001198A1 (de) * 2005-01-10 2006-07-20 H.C. Starck Gmbh Metallische Pulvermischungen
DE102006043498A1 (de) * 2006-09-12 2008-03-27 Artur Wiegand Dispergiermaschine und deren Verwendung für die Herstellung von Pulvermischungen
EP1980645A1 (de) * 2007-04-13 2008-10-15 Ralf Stein Verfahren zum Aufbringen einer mehrlagigen Beschichtung auf Werkstücke und/oder Werkstoffe
DE102007052198B3 (de) * 2007-10-26 2009-04-02 H.C. Starck Gmbh Metallpulvermischung und deren Verwendung
JP5266601B2 (ja) * 2008-09-15 2013-08-21 田森 亮 耐摩耗性コバルト基合金
DE102009057128A1 (de) 2009-12-08 2011-06-09 H.C. Starck Gmbh Verfahren zur Herstellung von sintermetallischen Hohlkörpern, damit erhältliche Produkte und deren Verwendung
DE102009057127A1 (de) 2009-12-08 2011-06-09 H.C. Starck Gmbh Teilchenfilter, Filterkörper, deren Herstellung und Verwendung
DE102009057257A1 (de) 2009-12-08 2011-06-09 H.C. Starck Gmbh Makroporöse Hohlkörper aus gesintertem Material, Verfahren zu deren Herstellung und Verwendung
JP5673971B2 (ja) 2010-08-18 2015-02-18 フウ、シンユ 粉末粒子の整形設備、整形方法、及び製造方法
DE102011113854A1 (de) * 2011-09-21 2013-03-21 Durum Verschleißschutz GmbH Hartstoffpulver und Verfahren zur Herstellung von Hartstoffpulver
DE102012020829B4 (de) 2012-10-16 2019-01-03 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung von Verbundbauteilen
CN102994913A (zh) * 2012-11-22 2013-03-27 宁波得利时泵业有限公司 一种均质混合泵的定子材料
KR101728936B1 (ko) 2014-07-28 2017-04-21 세종대학교산학협력단 우수한 강도 및 연성을 갖는 하이엔트로피 합금
CN105132802A (zh) * 2015-08-21 2015-12-09 苏州莱特复合材料有限公司 一种齿轮用粉末冶金材料及其制备方法
DE102016114533A1 (de) 2016-08-05 2018-02-08 Flowserve Flow Control Gmbh Eisenbasierte Legierung zur Herstellung thermisch gespritzter Verschleißschutzschichten
CN106399805A (zh) * 2016-09-29 2017-02-15 铜陵市超越电子有限公司 薄膜电容器端子专用合金组合物
EP3318534A1 (en) * 2016-11-07 2018-05-09 Höganäs AB (publ) Iron based media
CN106555119A (zh) * 2016-11-29 2017-04-05 张家港市鑫华易金属材料有限公司 一种隔热耐磨型复合金属材料
CN107236358B (zh) * 2017-07-28 2020-09-29 广东石油化工学院 一种应用于pvc印刷的低粘度水性油墨
CN107201079B (zh) * 2017-07-28 2020-09-29 广东石油化工学院 一种应用于pvc印刷的快干性水性油墨
CN107829039A (zh) * 2017-09-26 2018-03-23 宁国市恒铸新型材料科技有限公司 一种铝电解打壳锤头用合金材料及新型打壳锤头表面增材的成型工艺
EP3790692A4 (en) * 2018-05-11 2022-01-19 Equispheres Inc. POWDER FOR ADDITIONAL MANUFACTURING AND ADDITIONAL MANUFACTURING PART MANUFACTURED WITH IT
KR102214810B1 (ko) * 2018-10-17 2021-02-09 최경미 픽업롤러의 제조방법
CN109175389B (zh) * 2018-11-08 2021-04-09 宏力(天津)环保科技有限公司 一种稀土复合热材及制备方法
RU2748155C1 (ru) * 2020-10-28 2021-05-19 Федеральное государственное бюджетное учреждение науки Институт химии твердого тела и механохимии Сибирского отделения Российской академии наук (Ru) Способ получения активированного порошка металлического иридия
CN112522632A (zh) * 2020-12-09 2021-03-19 苏州莱特复合材料有限公司 一种粉末冶金耐磨定子及其生产工艺
CN113084150B (zh) * 2021-03-24 2023-08-25 河南东微电子材料有限公司 一种钌钴铼合金粉末的制备方法
CN114939663B (zh) * 2022-05-24 2023-03-10 中国工程物理研究院材料研究所 一种3d打印用钯粉及其制备方法和应用
CN114799187B (zh) * 2022-05-27 2024-04-16 鞍钢股份有限公司 一种提高真空气雾化制粉细粉率的方法

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3941584A (en) * 1972-09-29 1976-03-02 The International Nickel Company, Inc. Production of reflective metal flake pigments
US4115107A (en) * 1976-12-14 1978-09-19 Aluminum Company Of America Method of producing metal flake
US4482374A (en) * 1982-06-07 1984-11-13 Mpd Technology Corporation Production of electrically conductive metal flake
US4724162A (en) * 1986-04-19 1988-02-09 Fuji Photo Film Co., Ltd. Process for producing magnetic recording medium
US4787561A (en) * 1986-08-13 1988-11-29 Gte Products Corporation Fine granular metallic powder particles and process for producing same
US4884754A (en) * 1989-01-03 1989-12-05 Gte Products Corporation Process for producing fine copper flakes
US5246897A (en) * 1991-08-09 1993-09-21 Asahi Glass Company Ltd. Powder mixture for monolithic refractories containing graphite and a method of making thereof
US6277169B1 (en) * 1997-02-24 2001-08-21 Superior Micropowders Llc Method for making silver-containing particles
US20030008131A1 (en) * 2001-07-03 2003-01-09 Steward, Inc. Method for making radiation absorbing material (RAM) and devices including same
US6892954B2 (en) * 2003-06-04 2005-05-17 Siemens Westinghouse Power Corporation Method for controlling a spray process
US7611615B2 (en) * 2001-06-14 2009-11-03 Cerel (Ceramics Technologies) Ltd. Process for manufacturing a metal electrode

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1123816A (en) * 1978-02-06 1982-05-18 Harold M. Simons Granulating and activating metal to form metal hydride
JPS60251203A (ja) * 1984-05-25 1985-12-11 Hitachi Metals Ltd 粉末冶金用粉末の製造方法
JP2583905B2 (ja) * 1987-09-30 1997-02-19 東西化学株式会社 チタンフレークの製造方法
US4940490A (en) * 1987-11-30 1990-07-10 Cabot Corporation Tantalum powder
DE3832472A1 (de) * 1988-09-23 1990-03-29 Siemens Ag Verfahren zur herstellung eines werkstoffes mit einer hartmagnetischen phase aus pulverfoermigen ausgangskomponenten
JPH0598301A (ja) * 1991-10-07 1993-04-20 Hitachi Metals Ltd 扁平状金属微粉末およびその製造方法
JPH07118701A (ja) * 1993-10-22 1995-05-09 Katayama Tokushu Kogyo Kk フレーク状金属粉末、金属多孔体およびフレーク状金属粉末の製造方法
DE4418600C2 (de) * 1994-05-27 1997-03-20 Fraunhofer Ges Forschung Verfahren zur Herstellung von dispersionsverstärkten metallischen Werkstoffen, insbesondere Kupfer und Silber
DE4418598C2 (de) * 1994-05-27 1998-05-20 Fraunhofer Ges Forschung Verfahren zur Herstellung einer hochdispersen Pulvermischung insbesondere zur Herstellung von Bauteilen aus schwer sinterbaren Werkstoffen mit intermetallischen Phasen
JP2002266005A (ja) * 2001-03-07 2002-09-18 Fukuda Metal Foil & Powder Co Ltd 扁平状金属粉末の製造方法およびそれにより得られた粉末
JP2002285208A (ja) * 2001-03-27 2002-10-03 Sumitomo Special Metals Co Ltd 希土類合金粉末材料の調製方法およびそれを用いた希土類合金焼結体の製造方法
DE10126377B4 (de) * 2001-04-05 2004-12-23 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verbundpulver sowie Verfahren und Vorrichtung zu seiner Herstellung

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3941584A (en) * 1972-09-29 1976-03-02 The International Nickel Company, Inc. Production of reflective metal flake pigments
US4115107A (en) * 1976-12-14 1978-09-19 Aluminum Company Of America Method of producing metal flake
US4482374A (en) * 1982-06-07 1984-11-13 Mpd Technology Corporation Production of electrically conductive metal flake
US4724162A (en) * 1986-04-19 1988-02-09 Fuji Photo Film Co., Ltd. Process for producing magnetic recording medium
US4787561A (en) * 1986-08-13 1988-11-29 Gte Products Corporation Fine granular metallic powder particles and process for producing same
US4884754A (en) * 1989-01-03 1989-12-05 Gte Products Corporation Process for producing fine copper flakes
US5246897A (en) * 1991-08-09 1993-09-21 Asahi Glass Company Ltd. Powder mixture for monolithic refractories containing graphite and a method of making thereof
US6277169B1 (en) * 1997-02-24 2001-08-21 Superior Micropowders Llc Method for making silver-containing particles
US7611615B2 (en) * 2001-06-14 2009-11-03 Cerel (Ceramics Technologies) Ltd. Process for manufacturing a metal electrode
US20030008131A1 (en) * 2001-07-03 2003-01-09 Steward, Inc. Method for making radiation absorbing material (RAM) and devices including same
US6892954B2 (en) * 2003-06-04 2005-05-17 Siemens Westinghouse Power Corporation Method for controlling a spray process

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090252634A1 (en) * 2006-07-12 2009-10-08 Roland Scholl Metallic powder mixtures
US20090277301A1 (en) * 2006-07-12 2009-11-12 H.C. Starck Gmbh Metallic powder mixtures
US20100003157A1 (en) * 2006-07-12 2010-01-07 H.C. Starck Gmbh Metallic powder mixtures
US9856546B2 (en) 2006-09-22 2018-01-02 H. C. Starck Gmbh Metal powder
US20100047622A1 (en) * 2006-09-22 2010-02-25 H.C. Starck Gmbh Metal powder
US20100297440A1 (en) * 2007-04-13 2010-11-25 Noell Oliver Method for the Application of a High-Strength-Coating to Workpieces and/or Materials
US20090011252A1 (en) * 2007-04-13 2009-01-08 Gotz Matthaus Process for applying a multilayered coating to workpieces and/or materials
US20100107816A1 (en) * 2008-10-30 2010-05-06 Henning Zoz Method of making metal flakes
CN105506382A (zh) * 2015-12-21 2016-04-20 常熟市梅李合金材料有限公司 高电阻电热合金丝
CN106166616A (zh) * 2016-09-29 2016-11-30 柳州增程材料科技有限公司 一种3d打印用金属粉末的制备方法
CN106216698A (zh) * 2016-09-29 2016-12-14 柳州增程材料科技有限公司 一种3d打印用合金粉末的制备工艺
WO2019023123A1 (en) * 2017-07-24 2019-01-31 United States Of America, As Represented By The Secretary Of The Army ALUMINUM NANOGALVANIC COMPOSITIONS USEFUL FOR THE PRODUCTION OF HYDROGEN GASES AND THEIR TREATMENT AT LOW TEMPERATURE
US11198923B2 (en) 2017-07-24 2021-12-14 The United States Of America As Represented By The Secretary Of The Army Aluminum based nanogalvanic compositions useful for generating hydrogen gas and low temperature processing thereof
US11559837B2 (en) * 2018-04-04 2023-01-24 Metal Powder Works, LLC System and method for powder manufacturing
US20230118560A1 (en) * 2018-04-04 2023-04-20 Metal Powder Works, LLC System and Method for Powder Manufacturing
CN113617493A (zh) * 2021-06-29 2021-11-09 南京信彩科技有限公司 一种彩色油墨制备用原料研磨方法

Also Published As

Publication number Publication date
AU2004257411B2 (en) 2009-10-29
JP2007528936A (ja) 2007-10-18
KR20060026961A (ko) 2006-03-24
RU2006103980A (ru) 2006-08-10
BRPI0412509A (pt) 2006-09-05
AU2004257411A1 (en) 2005-01-27
SG147433A1 (en) 2008-11-28
IL173056A (en) 2010-06-16
RU2367542C2 (ru) 2009-09-20
CA2531683A1 (en) 2005-01-27
IL173056A0 (en) 2006-06-11
CN1863628A (zh) 2006-11-15
NO20060628L (no) 2006-04-07
WO2005007327A3 (de) 2006-07-06
DE10331785B4 (de) 2007-08-23
WO2005007327A2 (de) 2005-01-27
MXPA06000361A (es) 2006-03-30
DE10331785A1 (de) 2005-03-03
ZA200600252B (en) 2007-03-28
EP1646465A2 (de) 2006-04-19

Similar Documents

Publication Publication Date Title
AU2004257411B2 (en) Method for the production of fine metal powder, alloy powder and composite powder
US10676805B2 (en) Atomized picoscale composition aluminum alloy and method thereof
US20090123690A1 (en) Metallic Powder Mixtures
US20100003157A1 (en) Metallic powder mixtures
EP2325342B1 (en) Hot compaction and extrusion of L12 aluminum alloys
US11872631B2 (en) Additive manufacturing of composite powders
US20090277301A1 (en) Metallic powder mixtures
EP2325343B1 (en) Forging deformation of L12 aluminum alloys
JPH0261521B2 (ru)
US20090252634A1 (en) Metallic powder mixtures
Enayati Formation of nanoscale layered structures and subsequent transformations during mechanical alloying of Ni60Nb40 powder mixture in a low energy ball mill
US11085109B2 (en) Method of manufacturing a crystalline aluminum-iron-silicon alloy
Radu Miniaturisation and Nanotechnology in PM: Combined Mechanical Disordering-Reactive Synthesis, Possible Method of Bulk Nanocrystalline Intermetallics Obtaining

Legal Events

Date Code Title Description
AS Assignment

Owner name: H.C. STARCK GMBH, GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:SCHOLL, ROLAND;FISTER, DIETMAR;SPIEKER, CHRISTIAN;AND OTHERS;REEL/FRAME:017687/0521;SIGNING DATES FROM 20060131 TO 20060209

AS Assignment

Owner name: H.C. STARCK GMBH & CO. KG, GERMANY

Free format text: CHANGE OF NAME;ASSIGNOR:H.C. STARCK GMBH;REEL/FRAME:018766/0488

Effective date: 20060926

Owner name: H.C. STARCK GMBH & CO. KG,GERMANY

Free format text: CHANGE OF NAME;ASSIGNOR:H.C. STARCK GMBH;REEL/FRAME:018766/0488

Effective date: 20060926

AS Assignment

Owner name: H. C. STARCK GMBH & CO. KG, GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH;REEL/FRAME:019197/0734

Effective date: 20070321

Owner name: H. C. STARCK GMBH & CO. KG,GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH;REEL/FRAME:019197/0734

Effective date: 20070321

AS Assignment

Owner name: BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH, GERMANY

Free format text: CORRECTIVE ASSIGNMENT TO CORRECT THE THE ASSIGNEE NEED TO BE CHANGED TO BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH PREVIOUSLY RECORDED ON REEL 018766 FRAME 0488;ASSIGNOR:H.C. STARK GMBH;REEL/FRAME:019604/0833

Effective date: 20060926

Owner name: BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH,GERMANY

Free format text: CORRECTIVE ASSIGNMENT TO CORRECT THE THE ASSIGNEE NEED TO BE CHANGED TO BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH PREVIOUSLY RECORDED ON REEL 018766 FRAME 0488. ASSIGNOR(S) HEREBY CONFIRMS THE CHANGE OF NAME;ASSIGNOR:H.C. STARK GMBH;REEL/FRAME:019604/0833

Effective date: 20060926

Owner name: BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH, GERMANY

Free format text: CORRECTIVE ASSIGNMENT TO CORRECT THE THE ASSIGNEE NEED TO BE CHANGED TO BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH PREVIOUSLY RECORDED ON REEL 018766 FRAME 0488. ASSIGNOR(S) HEREBY CONFIRMS THE CHANGE OF NAME;ASSIGNOR:H.C. STARK GMBH;REEL/FRAME:019604/0833

Effective date: 20060926

AS Assignment

Owner name: H.C. STARCK GMBH, GERMANY

Free format text: MERGER;ASSIGNOR:H.C. STARCK GMBH & CO. KG;REEL/FRAME:019681/0705

Effective date: 20070604

Owner name: H.C. STARCK GMBH,GERMANY

Free format text: MERGER;ASSIGNOR:H.C. STARCK GMBH & CO. KG;REEL/FRAME:019681/0705

Effective date: 20070604

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION