WO2002057029A1 - Procede de preparation de poudres enrobees de metal - Google Patents

Procede de preparation de poudres enrobees de metal Download PDF

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Publication number
WO2002057029A1
WO2002057029A1 PCT/US2001/032560 US0132560W WO02057029A1 WO 2002057029 A1 WO2002057029 A1 WO 2002057029A1 US 0132560 W US0132560 W US 0132560W WO 02057029 A1 WO02057029 A1 WO 02057029A1
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WO
WIPO (PCT)
Prior art keywords
metal
coated
powder
precursor
glycolic
Prior art date
Application number
PCT/US2001/032560
Other languages
English (en)
Inventor
Lynn K. Kurihara
Richard Everett
Original Assignee
The Government Of The United States Of America, As Represented By The Secretary Of The Navy
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 The Government Of The United States Of America, As Represented By The Secretary Of The Navy filed Critical The Government Of The United States Of America, As Represented By The Secretary Of The Navy
Publication of WO2002057029A1 publication Critical patent/WO2002057029A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
    • 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
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F1/18—Non-metallic particles coated with metal
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4584—Coating or impregnating of particulate or fibrous ceramic material
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • 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 method for making bulk quantities of metal-coated powders at low temperatures.
  • Metal-coated powders can range in size from nanometers to microns and may be used in a number of processes, including: catalysis reactions, electromagnetic shielding, ferro-fluids, magnetic recording, composite precursors and advanced-engineered materials. Aero-propulsion and aero-structural applications with materials requirements that specify a high degree of microstructural control could benefit from metal-coated particle composites. For example, the development of a high toughness, high strength aluminum-based material would be an enabling technology for advanced reusable rocket propulsion, specifically in cryogenic pump rotor housings and impeller rotors.
  • Metal-coated powders can be prepared by physical vapor deposition, mechanical blending and mixing, and chemical routes. Vapor methods are not cost effective and can only be used to make small amounts of material. Mechanical blending often introduces impurities into the final product. Fluidized beds have been used to coat powders with metals. However, as with vapor methods, the initial fluidized bed equipment is expensive and it is difficult to coat the powders evenly and to process powders of different sizes.
  • Figlarz et al. in U.S. Patent No. 4,539,041, discloses producing metallic powders by reducing a solid oxide, hydroxide, or salt of a metal in a liquid phase. The solid compound is suspended in a polyol and the resultant metallic precipitate is isolated.
  • U.S. Patent No. 4,539,041 discloses producing metallic powders by reducing a solid oxide, hydroxide, or salt of a metal in a liquid phase. The solid compound is suspended in a polyol and the resultant metallic precipitate is isolated.
  • 5,698,483 discloses a method of preparing nano sized powders that comprises mixing an aqueous continuous phase containing at least one metal cation salt with a hydrophilic organic polymeric disperse phase, thereby forming a metal cation salt/polymer gel, then heat treating the gel at a temperature sufficient to drive off water and organics within the gel, leaving as residue a nanometer particle-size powder.
  • Hidaka et al., 5,250,101 discloses a process for producing a fine powder with a primary particle diameter of not more than 0.5 microns by heating an organic acid metal salt in the presence of palladium, which lowers the thermal decomposition temperature of the salt, which then thermally decomposes the organic acid metal salt in the presence of the palladium.
  • Viau et al. in U.S. Patent No. 5,925, 166, discloses a process for obtaining iron or iron-based powders by organic liquid phase precipitation. Metal precursors are introduced into a basic polyol or, optionally, into a simple alcohol solution, heating the reaction medium to obtain a metal precipitate, and recovering and treating the precipitate to obtain the desired powder.
  • Klapdor et al. in U.S. Patent No. 5,951,739, discloses a process for preparing nanocrystalline metal powders by reacting halides of metals with alkali metal hydrides or alkaline earth metal hydrides in an organic solvent with continual milling.
  • Chow et al. in U.S. Patent No. 5,759,230, describes producing nanostructured metal powders and films using an alcoholic solvent. A mixture of a metal precursor is heated in an alcoholic solvent to reduce the metal precursor to a metal precipitate, which can then be isolated, e.g., by filtration.
  • metal coated powders are produced at a relatively low temperatures by suspending a precursor metal salt and the powder to be coated in a glycol. As the mixture is heated, the metal is reduced and precipitates as a coating onto the powders. Suspension of the powder may be accomplished by proper choice of glycol, powder size, combined with ultrasonification, mechanical agitation, or stirring, or using conventional foam bubbling. The mixture is heated to reflux with resultant reduction and precipitation. The growth of the metal films occurs in solution. The metal-coated powders are then removed from the solution, generally by filtration. Time, concentration of the metal precursor salt, and temperature of reflux can be used to control the coating thickness.
  • the process of the present invention makes it possible to deposit more types of ferrous and non-ferrous metals and alloys than has previously been possible. It also allows for more control over coating thickness and coating uniformity. This improved control could make possible advantageous improvements to a composite material's microstructure: larger mean nearest neighbor distance (and reduced nearest neighbor distance standard deviation); and improved mechanical properties (higher proportional limit and yield stresses, and larger strains to failure). These generic improvements to the composite, which are independent of the matrix and particle composition, allow more widespread usage of composites in critical applications.
  • Any metal powders can be used in the present invention that is not soluble (at any temperature) in tire particular glycol used. This includes metal oxides, borides, carbides, nitrides, suicides, and the like. Any glycol or diol can be used, either alone or in combination with another alcohol.
  • the time for formation of the metal powder depends upon the coating thickness desired, and can range from a few minutes to a few hours.
  • a metal precursor is mixed with the powder to be coated and a glycol.
  • Glycols that can be used for this purpose include aliphatic glycols or corresponding glycol polyesters which are liquid at reaction temperatures.
  • the aliphatic glycols can be alkylene glycols having up to 6 carbon atoms in the main chain, or an ethanediol, a propanediol, a butanediol, a pentanediol, or a hexanediol, as well as polyalkylene glycols derived from these alkylene glycols.
  • Other glycols include ethyleneglycol, diethylene glycol, tri-ethylene glycol, dipropylene glycol, and polyetheylene glycols liquid at the reaction temperatures, or glycerol.
  • Particularly interesting polyols for use in the process of the present invention include: ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,2-propanediol, di-propylene glycol, 1,2-butanediol, 1,3- butanediol, 1,4-butanediol, and 2,3-butanediol.
  • These glycols are advantageous because of their significant reducing power, boiling temperatures between about 185° and 328°C, proper thermal stability, and low price. Furthermore, these glycols raise fewer potential toxicity problems.
  • the metal precursor or precursors are mixed with the powder to be coated and a glycol solvent.
  • the glycol solvent may be either heated or unheated.
  • the resulting mixture is reacted at temperatures sufficiently high to dissolve or allow the reaction of the metal precursor(s), thereby liberating the free metal to precipitate onto the powder.
  • the mixture is reacted at about 80-360°C, depending upon the reflux temperature of the glycol. The preferred temperature depends on the reaction system used.
  • the reaction mixture is cooled naturally in air or quenched. Because quenching provides greater control over the reaction time, it is generally preferred over natural ambient air cooling. However, for quenching to be useful in coating a powder, the powder substrate must be able to withstand rapid thermal changes. If the powder cannot withstand these rapid temperature changes, then natural air cooling should be used.
  • the method of the present invention may be used to form particles coated with pure metals, alloys, or composites thereof.
  • powders may be coated with the following: vanadium, chromium, magnesium, iron, cobalt, nickel, copper, niobium, molybdenum, ruthenium, rhenium, palladium, silver, indium, tin, tantalum, tungsten, osmium, indium, platinum, gold; or various alloys thereof; or meta-stable alloys containing these metals as primary constituents.
  • the precursor form of the metal depends upon the metal itself. Generally, the precursor may be any metal-containing compound that, under the reaction conditions, can be reduced to the elemental metal.
  • Typical precursors include: metal acetates and hydrates thereof; metal chlorides and hydrates thereof; metal nitrates; metal oxides; metal oxalates; metal hydroxides and acids, including the desired metal as part of an oxyanion (e.g., tungstic acid) and salts of such acids (e.g., sodium tungstate and potassium hexachloroplatinate); and metal organic or organometallic compounds.
  • oxyanion e.g., tungstic acid
  • salts of such acids e.g., sodium tungstate and potassium hexachloroplatinate
  • metal organic or organometallic compounds e.g., metal organic or organometallic compounds.
  • the powders that can be coated by the process of the present invention include metals, ceramic oxides, borides, nitrides, and carbides.
  • the particle size of the powders to be coated ranges from about 1 nanometer to about 1000 microns. Specific Examples or Modes
  • Cobalt coated powders can be used for magnetic, structural, electronic, and catalytic applications.
  • the following polyol process can achieve nanostructured cobalt films formed on boron carbide.
  • Example 3 Co-coated Powders in the Presence of a Magnetic Field
  • Example 2 was repeated except that two magnets were placed around the flask.
  • the choice of powder or film can be controlled by the selection of the proper synthesis conditions to favor either nucleation or growth, respectively.
  • the formation of monodispersed particles generally follows 3 stages: at phase I, nuclei form; at phase II or nucleation, particles form; and at phase III or growth, films form. Growth is a function of concentration of atoms in solution, time, and temperature.
  • Powders can be coated with refractory metals and their alloys such as tungsten, molybdenum, rhenium, and tantalum. If the oxides of these metals are chemically stable under the reaction conditions used, they cannot be reduced to form coatings on powders. Therefore, the precursors of these refractory metals should be chosen to avoid the formation of stable oxides or their stable intermediates. Generally, the precursors of refractory metals should be salts or acids, rather than oxides or hydroxides. Acids and salts including the oxyanion of the desired refractory metal or metals, however, may be preferred.
  • the present invention implicitly contains a nucleating agent, i.e., the powder which is to be coated.
  • the metal which is reduced is coated onto the powder to produce a powder-coated metal.
  • there is no requirement for a catalyst so that the resulting coated powders are free or essentially free of impurities that would deleteriously alter their properties.
  • surfactants and or dispersants may be added to the reaction mixture to avoid the agglomeration of nanoparticles. If a highly pure product is desired, these surfactants and dispersants should be essentially free of insoluble materials, or capable of having them burnt out of H e final product. Where a surfactant is used, the best choice of surfactant depends upon the desired metal. Because ionic surfactants may undesirably alter the pH of the reaction system during reduction of the metal precursor, steric stabilization using a nonionic surfactant (e.g., a high temperature polymeric surfactant) is preferred. If desired, however, a mixture of ionic and nonionic surfactants can be used.
  • a nonionic surfactant e.g., a high temperature polymeric surfactant
  • the pH may influence the method of the present invention. For example changing the pH during the reaction may be used to alter the solubility of the reaction product in the reaction mixture. If a constant pH is desired throughout the reaction, the reaction mixture may be modified to include a buffer.
  • the mixture may be stirred or otherwise agitated (e.g., by sonication). However, stirring or agitation is not required.
  • the effects of stirring during the reaction depend upon the metal coating to be produced and the energy added during stirring. Stirring during production of magnetically coated materials would most likely increase agglomeration, in which case the use of a surfactant would be beneficial.
  • a composite metal film includes at least one metal component and at least one other (second) component that is intentionally included in amounts that significantly enhance the desirable properties of the film or powder.
  • the second component is usually, but not necessarily, another metal.
  • the metal may be any metal, not just those metals that could be deposited as a pure coating according to the present invention.
  • the second component of the coating is a chemically stable ceramic
  • the present invention provides a powder coated with a metal/ceramic composite.
  • a metal/ceramic composite includes at least 50 percent (by volume) metal, in the form of a single phase material or an alloy.
  • composite includes alloys and metal/ceramic composites and applies to phase-separated mixtures of a metal with at a least one other component.
  • alloy applies to inter-metallic compounds and solid solutions of two or more metals.
  • At least one precursor for the metal component and at least one precursor for the other component(s) of the coating are combined in the reaction mixture before heating to reaction or re-fluxing temperature. Otherwise, the process proceeds as described above to make single metal coated powders.
  • the initial molar ratios of the components may not be reflected in the final product. Additionally, the ability of precursors to atomically mix in the reaction solution does not assure that the components will form a composite substance. For this reason, the correct starting ratios of the precursors of each compound for any composite substance must be determined empirically. The relative reduction potentials of each component can provide some guidance in making this empirical determination.
  • the process of the present invention makes it possible to produce larger quantities of metal coated powders than conventional techniques, while achieving better chemical homogeneity due to the mixing of constituents at the molecular or atomic level. Additionally, the chemical route employed in the present invention does not require expensive processing equipment and the production costs are relatively low. i addition, the solvent used in this process is recyclable and the coating thickness can be controlled by selecting the synthesis conditions to favor either nucleation or growth.
  • the process of the present invention can be used to deposit magnetic materials as well as non-magnetic materials. Additionally, the process can be used to deposit single elements, alloys, or multi-component elements.
  • the powder feedstock can be of any size and shape.
  • powders having a particle size ranging from about 0.01 micron to about 1000 microns can be advantageously prepared according to the present invention. These coated particles can be used to make particulate-reinforced composites.

Abstract

L'invention concerne des poudres enrobées de métal obtenues par suspension d'un sel métallique précurseur et de la poudre à enrober dans un glycol. Ce mélange est chauffé, le sel métallique est réduit et le métal est précipité, de manière à obtenir un enrobage sur la poudre.
PCT/US2001/032560 2001-01-19 2001-10-18 Procede de preparation de poudres enrobees de metal WO2002057029A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US09/764,161 US20040055419A1 (en) 2001-01-19 2001-01-19 Method for making metal coated powders
US09/764,161 2001-01-19

Publications (1)

Publication Number Publication Date
WO2002057029A1 true WO2002057029A1 (fr) 2002-07-25

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US (1) US20040055419A1 (fr)
WO (1) WO2002057029A1 (fr)

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EP2258502A1 (fr) * 2009-05-04 2010-12-08 Laird Technologies, Inc. Procédé pour le chargement uniforme et plus important d'agents de remplissage dans une matrice polymère utilisant un matériau hôte fortement poreux
US8663506B2 (en) 2009-05-04 2014-03-04 Laird Technologies, Inc. Process for uniform and higher loading of metallic fillers into a polymer matrix using a highly porous host material

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