US3650714A - A method of coating diamond particles with metal - Google Patents

A method of coating diamond particles with metal Download PDF

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Publication number
US3650714A
US3650714A US804144A US3650714DA US3650714A US 3650714 A US3650714 A US 3650714A US 804144 A US804144 A US 804144A US 3650714D A US3650714D A US 3650714DA US 3650714 A US3650714 A US 3650714A
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Prior art keywords
diamond
titanium
particles
metal
coated
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US804144A
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English (en)
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Peter Farkas
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Permattach Diamond Tool Corp
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Permattach Diamond Tool Corp
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    • 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
    • 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
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten 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
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
    • 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
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—Metals
    • 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
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1436—Composite particles, e.g. coated particles
    • C09K3/1445—Composite particles, e.g. coated particles the coating consisting exclusively of metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12181—Composite powder [e.g., coated, etc.]

Definitions

  • ABSTRACT Titanium (or zirconium) coated single diamonds have high cohesion bonding between coating and diamond and have external surfaces adhesion-receptive to subsequently applied less oxidizable metal, resin, and ceramic coatings which permit the double coated particles to be mounted at elevated temperatures in or on extraneous supports with or without application of pressure, without loosening the cohesion bonding and without resort to nonoxidizing atmospheres; or permitting them to be directly mounted in nonoxidizing atmospheres, in either case providing long life support for single or multiple diamond arrays as in cutting and abrading implements.
  • diamond particles are supported for cutting, abrading, and other uses by attaching them, singly or multiply, to the surface of a support or by embedding them, in single or multiple layers or other conglomerate configuration, partially or wholly in metallic, ceramic or organic matrices.
  • the diamond surface interface bond is usually created either in the act of attaching the diamond to the support or in the act of hardening or sintering the matrix.
  • conventional binder metals for example, copper and silver alloys provide little if anything more than mechanical bonds to diamonds due to the failure of such alloys to wet the diamond surface and to the absence of any chemical bonds providing anything more than very low energies of adhesion
  • the art looking for improved bonds, began to carry out the brazing or embedding operations in the presence of transition metals, particularly titanium or zirconium, either as such or as hydrides.
  • U.S. Pat. No. 2,570,248 suggested use of an admixture of titanium hydride and copper powders applied to the junction of two bodies to be brazed; and Hall U.S. Pat. No. 2,728,651 suggested applying a slurry of titanium hydride in an organic liquid to a diamond and then sprinkling these titanium hydride coated diamonds onto a solder alloy layer and heating and dissociating the hydride and melting the solder and dissolving the titanium.
  • diamond bonds of great strength are provided by creating the diamond surface interface bond prior to any operation of permanently attaching it to an ultimate extraneous support or seating it in a matrix, so that only diamond-reactive materials need be present when creating the diamond surface bond.
  • These materials, forming the diamond surface interface bond, because they are oxidizable, are then covered with a less oxidizable protective layer or layers so that subsequent attaching or embedding operations with non-oxidizable brazing alloys can be carried out in the air without oxidizing the titanium. Operation in a nonoxidizing atmosphere is thus required only during the creation of the diamond surface interface and is not thereafter needed.
  • this invention provides single diamond particles with bonded coatings of those transition metals which are most likely to react with diamond or carbon, namely, titanium or zirconium or mixtures thereof.
  • the coatings are in the form of thin continuous layers of substantially uniform thickness which are bonded throughout the entire interface between the film and the diamond exterior surface with high energies of adhesion commensurate with those created by chemical bonds such as are present in titanium or zirconium carbide structure.
  • One of the beauties of the present invention is that a whole batch of diamond particles having mechanical deposits contacting each other can have the deposits converted into heat bonded coatings all at one time without fusing adjacent particles together, since the heat treatment is at a far less temperature than that which would melt the titanium or zirconium deposits.
  • fusion takes place between the coated diamonds which therefore can no longer be recovered in individual, discrete, flowable condition but rather fuse into a solid mass.
  • Diamond chips weighing an aggregate of 200 carats, 200250 mesh size, and cleaned by conventional solvents to rid their surfaces of organic contaminants are placed in a mechanical tumbler along with approximately 6 grams of titanium or zirconium powder (at least some of which, 10 percent or more, is in the hydride form) having a mesh size of 600 and tumbled for a length of time under room temperature and atmospheric pressure conditions until each diamond particle bears over its entire exterior surface a clinging deposit of the powder.
  • the diamonds with the deposits thereon are then placed together in a graphite crucible and brought down to a vacuum ofabout 10' mm. of mercury and to a minimum of about 10" and subjected to a temperature of 850900" C. for a period of at least 10-15 minutes.
  • the particles in the crucible are allowed to cool in the vacuum and then are removed from the vacuum chamber.
  • each particle is discrete and unattached to other particles except by occasional frangible attachment, which can be readily broken without damage to the surface.
  • each particle Under the microscope, each particle is seen to have acquired a very thin smooth even external metallic film of substantially uniform thickness which may be for example about percent by weight of the combined weight of the film and the enclosed diamond.
  • the diamond core is shown at 1
  • the diamond surface interface with the surrounding titanium film is at 2
  • 3 is the titanium film.
  • the coating is not loosened as is the case with nickel-clad diamonds.
  • the bonds of this invention do withstand de-bonding forces imparted as a result of difference in the coefficients of expansion of the diamond and the coating.
  • the initial layer formed on the diamond particles is thus viewed as being a non-homogeneous layer progressing outwardly from titanium carbide content at and near the interface towards all or entirely all uncarbided titanium content on and near the external surface rendering the coated particle adhesion-receptive to metallic as well as nonmetallic bonding materials.
  • the coated particle has the high cohesion characteristics of metal-carbide structure at the interface, yet permits further application to the external surface of the coated particle of protective layers by conventional techniques with the resulting outer adhesions being greater than would be provided were the external surface of the initial layer constituted of titanium carbide.
  • This dual function characteristic of the single applied titanium layer is achieved by omitting from the coating the metal alloys or brazing materials which were heretofore used but produced only low diamond adhesions, not far removed from those of solely mechanical bonds, and by limiting the depth of carbide formation.
  • the uncarbided surface may be subsequently carburized as by heating in a pack of carbon or methane where such carburizing is desired, as to reduce oxidation or create a harder surface and is not incompatible with good adhesion to subsequent bonding materials.
  • a minimum temperature is about 350 C., i.e., sufficient to dissociate the hydride and the maximum is that temperature at which graphitization of the diamond under the prevailing conditions would occur, say l,250 C.
  • temperature conditions should be always such as to minimize formation of any significant amounts of carbide on the external surface of the coated particles. Because of this dual function of the single applied layer, one does not include, as has been done previously in initial titanium coatings, any other alloy or brazing material, producing far lower adhesions more commensurate with solely mechanical bonds.
  • EXAMPLE la The same procedure is followed except the deposit is an admixture of 1 part of titanium and 1 part zirconium by weight (again each partially in the form of hydrides).
  • a further layer of copper or nickel is plated onto the entire FIG. 1 particle to a thickness of 0.002 0.005 inch.
  • conventional vacuum deposit techniques including sputtering, may be utilized.
  • the coated particles are then embedded in a metallic matrix by the following procedure to produce the product shown (again greatly magnified) in FIG. 2 wherein 1 is the diamond particle; 2 is the interface; 3 is the titanium layer; 4 is the copper or nickel layer; and 5 is a fragment of the metallic matrix:
  • the particles are mixed with copper powder and subjected to a hot press in a graphite mold or a cold press and subsequently sintered or infiltrated with brazing material by usual techniques.
  • a resin powder with or without metallic or other filler may be used.
  • vitrifying techniques may be used.
  • the copper or nickel layer 4 may be constituted of successive layers of copper and nickel.
  • the copper coated, the nickel coated, or the double copper, nickel coated particle may be sintered or fused in situ at the sintering or fusing temperatures of the less-oxidizable metal or metals in a nonoxidizing atmosphere producing metallurgical cohesion bonding between the transition metal and the overlying less-oxidizable metal.
  • a protective layer or layers such as 4 is essential only in those cases where further operations are to be done without the benefit of nonoxidizing atmospheres.
  • a metal layer or layers is helpful wherever press techniques are to be utilized since the softer metal will not damage the surface of the mold.
  • the coated diamond particles 1, 2, 3, 4 can be used themselves as powdered metals with conventional powdered metallurgical techniques such as cold pressing, sintering, or infiltration for manufacturing diamond impregnated bodies.
  • a coated product prepared as in Example 2 can be mounted on a tool by applying a conventional brazing material between the coated particle and a clean surface ofa steel shank and the brazing material then heated with a gas torch in air to melt the brazing material.
  • FIG. 3 The resulting product is shown in FIG. 3 wherein Z] is the diamond; 23 is the titanium layer; 24 is the copper or nickel layer; 25 is the brazing material and 26 is a portion of the steel shank,
  • Coated particles prepared in accordance with Example 2 are covered with a layer of sponge iron by the following procedure:
  • Brazing material is applied to the coated particles which are then mixed with sponge iron powder and placed in vacuum or hydrogen furnace to braze the iron particles to the surface of the coated diamond.
  • a batch of said products are then embedded in a resin matrix by conventional procedure.
  • FIG. 4 This produces the product shown in FIG. 4 wherein 31 is the diamond; 32 is the interface; 33 is the titanium layer; 34 is a metallic layer; 35 is a brazing material; 36 are sponge iron particles; and 37 is a portion of a resin matrix.
  • a coated product prepared in accordance with Example I is plated with a coating of copper or nickel to a thickness of about 0.002 0.005 inch.
  • minute whiskers, fibers or filaments, of ceramic, glass or aluminum oxide are placed in the metal plating solution and allowed to settle on the surface of the diamond during the course of approximately 25 minutes. Subsequent agitation of the diamonds in the plating solution results in further deposit of whiskers on the coated diamond particle surfaces during the plating operation.
  • whisker-covered particles are then embedded in a resin matrix by conventional techniques to provide a grinding wheel section as shown in FIG. 5, wherein 41 is a natural or synthetic diamond particle; 42 is the interface; 43 is the titanium layer; 44 is a copper or nickel coating; 45 are whiskers; and 46 is a portion of the resin matrix.
  • FIG. 6 shows a fragment of a wheel dressing tool having an unusually high diamond concentration which produces more cutting points and eliminates undercutting action by dressed abrasive particles.
  • a low carbon steel shank having'a cavity about 0.150 inch in diameter by 0.250 inch deep.
  • Diamond particles bearing the titanium coatings of this invention overlaid with a nickel or copper layer (or both) are hot pressed into the cavity with copper and silver brazing alloy powders at 750 C. in air.
  • the titanium may be over-coated directly with a ceramic or resin material as by applying them in powdered form and then vitrifying or hot pressing the applied powder in a conventional manner.
  • the coated diamond particles of this invention may be used in making a great variety of cutting or abrading products including dressing tools, dressing wheels, saw blades, grinding wheels, grinding wheel segments either single or multiple layer, saw blade segments or inserts, drilling bits, routing, boring, turning, countersinking, and single or multiple point tools, chamfering and edging tools and wire and other saws and all other kinds of honing, lapping, cutting and abrading devices; or may be used to manufacture optical lens generators or button inserts.
  • the protective metallic layer may be of any metal bonding material which can be electroplated, electroless plated, vacuum deposited or sputtered, for example, nickel, copper, iron, zinc, tin, silver, gold, cadmium or cobalt or their alloys or admixtures thereof.
  • Useful brazing or soldering bonding materials are copper, bronze, copper-silver alloy, copper-beryllium alloy, copperzinc alloy or any other metallurgical brazing material or solders which have adhesion to the protective layer or to the transition metal coating if the metallic protective layer is omitted.
  • a method of coating diamond particles comprising mixing a batch of individual discrete diamond particles with transition metal powder consisting essentially of powders selected from the class consisting of powders of titanium, zirconium, and their hydrides, and mixtures thereof, to form a dry deposit of said powder over the external surfacesof said diamond particles and then subjecting the particles with their deposits thereon in a single container to a temperature in the range of a minimum of about 350 and a maximum of l,000 C. in a nonoxidizing atmosphere to coat the entire surface of each particle with a thin continuous layer consisting essentially of said transition metal, cooling the particles and removing them from said atmosphere in the form of individual discrete, nonadherent, flowable transition metal coated particles, each containing a single diamond particle.
  • titanium carbide structure is formed at the interfaces between the metal coatings and the diamonds.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
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  • Polishing Bodies And Polishing Tools (AREA)
  • Carbon And Carbon Compounds (AREA)
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