WO2013186386A1 - Constructions super-dures et leurs procédés de fabrication - Google Patents

Constructions super-dures et leurs procédés de fabrication Download PDF

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Publication number
WO2013186386A1
WO2013186386A1 PCT/EP2013/062440 EP2013062440W WO2013186386A1 WO 2013186386 A1 WO2013186386 A1 WO 2013186386A1 EP 2013062440 W EP2013062440 W EP 2013062440W WO 2013186386 A1 WO2013186386 A1 WO 2013186386A1
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Prior art keywords
superhard
fraction
grains
grain size
diamond
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PCT/EP2013/062440
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English (en)
Inventor
Nedret Can
Humphrey Samkelo Lungisani Sithebe
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Element Six Abrasives SA
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Element Six Abrasives SA
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Priority to CN201380041312.0A priority Critical patent/CN104520253B/zh
Priority to US14/407,957 priority patent/US20150165590A1/en
Publication of WO2013186386A1 publication Critical patent/WO2013186386A1/fr
Anticipated expiration legal-status Critical
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/06—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • C04B35/5831—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride based on cubic boron nitrides or Wurtzitic boron nitrides, including crystal structure transformation of powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B10/00—Drill bits
    • E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B10/00—Drill bits
    • E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
    • E21B10/56—Button-type inserts
    • E21B10/567—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3804—Borides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/427—Diamond

Definitions

  • This disclosure relates to superhard constructions and methods of making such constructions, particularly but not exclusively to constructions comprising polycrystalline diamond (PCD) structures attached to a substrate and for use as cutter inserts or elements for drill bits for boring into the earth.
  • PCD polycrystalline diamond
  • Polycrystalline superhard materials such as polycrystalline diamond (PCD) and polycrystalline cubic boron nitride (PCBN) may be used in a wide variety of tools for cutting, machining, drilling or degrading hard or abrasive materials such as rock, metal, ceramics, composites and wood-containing materials.
  • tool inserts in the form of cutting elements comprising PCD material are widely used in drill bits for boring into the earth to extract oil or gas.
  • the working life of superhard tool inserts may be limited by fracture of the superhard material, including by spalling and chipping, or by wear of the tool insert.
  • Cutting elements such as those for use in rock drill bits or other cutting tools typically have a body in the form of a substrate which has an interface end/surface and an ultra hard material which forms a cutting layer bonded to the interface surface of the substrate by, for example, a sintering process.
  • the substrate is generally formed of a tungsten carbide-cobalt alloy, sometimes referred to as cemented tungsten carbide and the ultra hard material layer is typically polycrystalline diamond (PCD), polycrystalline cubic boron nitride (PCBN) or a thermally stable product TSP material such as thermally stable polycrystalline diamond.
  • PCD polycrystalline diamond
  • PCBN polycrystalline cubic boron nitride
  • TSP material such as thermally stable polycrystalline diamond
  • PCD Polycrystalline diamond
  • PCD material is an example of a superhard material (also called a superabrasive material) comprising a mass of substantially inter- grown diamond grains, forming a skeletal mass defining interstices between the diamond grains.
  • PCD material typically comprises at least about 80 volume % of diamond and is conventionally made by subjecting an aggregated mass of diamond grains to an ultra-high pressure of greater than about 5 GPa, and temperature of at least about 1 ,200°C, for example.
  • a material wholly or partly filling the interstices may be referred to as filler or binder material.
  • PCD is typically formed in the presence of a sintering aid such as cobalt, which promotes the inter-growth of diamond grains.
  • a sintering aid such as cobalt
  • Suitable sintering aids for PCD are also commonly referred to as a solvent-catalyst material for diamond, owing to their function of dissolving, to some extent, the diamond and catalysing its re-precipitation.
  • a solvent-catalyst for diamond is understood be a material that is capable of promoting the growth of diamond or the direct diamond-to-diamond inter-growth between diamond grains at a pressure and temperature condition at which diamond is thermodynamically stable. Consequently the interstices within the sintered PCD product may be wholly or partially filled with residual solvent-catalyst material.
  • PCD is often formed on a cobalt-cemented tungsten carbide substrate, which provides a source of cobalt solvent-catalyst for the PCD.
  • Materials that do not promote substantial coherent intergrowth between the diamond grains may themselves form strong bonds with diamond grains, but are not suitable solvent -catalysts for PCD sintering.
  • Cemented tungsten carbide which may be used to form a suitable substrate is formed from carbide particles being dispersed in a cobalt matrix by mixing tungsten carbide particles/grains and cobalt together then heating to solidify.
  • an ultra hard material layer such as PCD or
  • PCBN diamond particles or grains or CBN grains are placed adjacent the cemented tungsten carbide body in a refractory metal enclosure such as a niobium enclosure and are subjected to high pressure and high temperature so that inter-grain bonding between the diamond grains or CBN grains occurs, forming a polycrystalline ultra hard diamond or polycrystalline CBN layer.
  • the substrate may be fully cured prior to attachment to the ultra hard material layer whereas in other cases, the substrate may be green, that is, not fully cured. In the latter case, the substrate may fully cure during the HTHP sintering process.
  • the substrate may be in powder form and may solidify during the sintering process used to sinter the ultra hard material layer.
  • PCD polycrystalline diamond
  • a superhard polycrystalline construction comprising a body of polycrystalline superhard material formed of: a mass of superhard grains exhibiting inter-granular bonding and defining a plurality of interstitial regions therebetween, the superhard grains having an associated mean free path; a non-superhard phase at least partially filling a plurality of the interstitial regions and having an associated mean free path; wherein: the median of the mean free path associated with the non-superhard phase divided by (Q3-Q1 ) for the non-superhard phase is greater than or equal to 0.83, where Q1 is the first quartile and Q3 is the third quartile; and the median of the mean free path associated with the superhard grains divided by (Q3-Q1 ) for the superhard grains is less than 0.47.
  • the superhard grains comprise natural and/or synthetic diamond grains, the superhard polycrystalline construction forming a polycrystalline diamond construction.
  • the non-superhard phase comprises a binder phase.
  • the binder phase may comprise, for example, cobalt, and/or one or more other iron group elements, such as iron or nickel, or an alloy thereof, and/or one or more carbides, nitrides, borides, and oxides of the metals of Groups IV-VI in the periodic table.
  • the polycrystalline superhard construction further comprises a cemented carbide substrate bonded to the body of polycrystalline material along an interface.
  • the cemented carbide substrate may, for example, comprise tungsten carbide particles bonded together by a binder material, the binder material comprising an alloy of Co, Ni and Cr.
  • the tungsten carbide particles form at least 70 weight percent and at most 95 weight percent of the substrate; the binder material comprising between about 10 to 50 wt.% Ni, between about 0.1 to 10 wt.% Cr, and the remainder weight percent comprising Co; and wherein the size distribution of the tungsten carbide particles in the cemented carbide substrate has the following characteristics:
  • tungsten carbide particles have a grain size of between about 0.3 to 0.5 microns;
  • tungsten carbide particles have a grain size of between about 0.5 to 1 microns;
  • the mean grain size of the tungsten carbide particles is about 0.6+0.2 microns.
  • the binder in the substrate may additionally comprise between about 2 to 20 wt.% tungsten and between about 0.1 to 2 wt.% carbon.
  • a method of forming a superhard polycrystalline construction comprising: providing a mass of grains of superhard material comprising a first fraction having a first average size and a second fraction having a second average size,
  • the step of providing a mass of grains of superhard material comprises providing a mass of diamond grains having a first fraction having a first average size and a second fraction having a second average size, the first fraction having an average grain size ranging from about 10 to 60 microns, and the second fraction having an average grain size less than the size of the coarse fraction.
  • the second fraction may, for example, have an average grain size between around 1/10 to 6/10 of the size of the first fraction.
  • the average grain size of the first fraction is between around 10 to 60 microns, and the average grain size of the second fraction is between about 0.1 to 20 microns.
  • the weight ratio of the first fraction to the second fraction ranges from about 50% to about 97%, the weight ratio of the second fraction ranging from about 3% to about 50 weight%.
  • the ratio by weight percent of the first fraction to the second fraction is around 60:40, or around 70:30, or around 90:10, or around 80:20.
  • the step of providing a mass of grains of superhard material may comprises, for example, providing a mass of grains in which the grain size distributions of the first and second fractions do not overlap.
  • the step of providing a mass of grains of superhard material may, in some embodiments, comprise providing three or more grain size modes to form a multimodal mass of grains comprising a blend of grain sizes having associated average grain sizes.
  • the average grain sizes of the fractions is separated by an order of magnitude.
  • the mass of superhard grains comprises a first fraction having an average grain size of around 20 microns, a second fraction having an average grain size of around 2 microns, a third fraction having an average grain size of around 200nm and a fourth fraction having an average grain size of around 20nm.
  • a tool comprising the superhard polycrystalline construction defined above, the tool being for cutting, milling, grinding, drilling, earth boring, rock drilling or other abrasive applications.
  • the tool may comprise, for example, a drill bit for earth boring or rock drilling, a rotary fixed-cutter bit for use in the oil and gas drilling industry, or a rolling cone drill bit, a hole opening tool, an expandable tool, a reamer or other earth boring tools.
  • a drill bit or a cutter or a component therefor comprising the superhard polycrystalline construction defined above.
  • Figure 1 is a polycrystalline diamond (PCD) structures attached to a substrate;
  • Figure 2 is a plot showing wear scar depth for two embodiments.
  • Figure 3 is a plot of wear scar area against cutting length in a vertical borer test for an embodiment.
  • a "superhard material” is a material having a Vickers hardness of at least about 28 GPa. Diamond and cubic boron nitride (cBN) material are examples of superhard materials.
  • a "superhard construction” means a construction comprising a body of polycrystalline superhard material. In such a construction, a substrate may be attached thereto or alternatively the body of polycrystalline material may be free-standing and unbacked.
  • polycrystalline diamond is a type of polycrystalline superhard (PCS) material comprising a mass of diamond grains, a substantial portion of which are directly inter-bonded with each other and in which the content of diamond is at least about 80 volume percent of the material.
  • interstices between the diamond grains may be at least partly filled with a binder material comprising a catalyst for diamond.
  • interstices or "interstitial regions” are regions between the diamond grains of PCD material.
  • interstices or interstitial regions may be substantially or partially filled with a material other than diamond, or they may be substantially empty.
  • PCD material may comprise at least a region from which catalyst material has been removed from the interstices, leaving interstitial voids between the diamond grains.
  • PCBN polycrystalline cubic boron nitride
  • cBN cubic boron nitride
  • PCBN is an example of a superhard material.
  • a "catalyst material" for a superhard material is capable of promoting the growth or sintering of the superhard material.
  • substrate means any substrate over which the ultra hard material layer is formed.
  • a “substrate” as used herein may be a transition layer formed over another substrate.
  • the terms “radial” and “circumferential” and like terms are not meant to limit the feature being described to a perfect circle.
  • the superhard construction 1 shown in the Figure 1 may be suitable, for example, for use as a cutter insert for a drill bit for boring into the earth.
  • a cutting element 1 includes a substrate 10 with a layer of ultra-hard material 12 formed on the substrate 10.
  • the substrate may be formed of a hard material such as cemented tungsten carbide.
  • the ultra-hard material may be, for example, polycrystalline diamond (PCD), polycrystalline cubic boron nitride (PCBN), or a thermally stable product such as thermally stable PCD (TSP).
  • the cutting element 1 may be mounted into a bit body such as a drag bit body (not shown).
  • the exposed top surface of the ultra-hard material opposite the substrate forms the cutting face 14, which is the surface which, along with its edge 16, performs the cutting in use.
  • the substrate 10 is generally cylindrical and has a peripheral surface 20 and a peripheral top edge 22.
  • the grains of superhard material, such as diamond grains or particles in the starting mixture prior to sintering may be, for example, bimodal, that is, the feed comprises a mixture of a coarse fraction of diamond grains and a fine fraction of diamond grains.
  • the coarse fraction may have, for example, an average particle/grain size ranging from about 10 to 60 microns.
  • average particle or grain size it is meant that the individual particles/grains have a range of sizes with the mean particle/grain size representing the "average”.
  • the average particle/grain size of the fine fraction is less than the size of the coarse fraction, for example between around 1/10 to 6/10 of the size of the coarse fraction, and may, in some embodiments, range for example between about 0.1 to 20 microns.
  • the weight ratio of the coarse diamond fraction to the fine diamond fraction ranges from about 50% to about 97% coarse diamond and the weight ratio of the fine diamond fraction may be from about 3% to about 50%. In other embodiments, the weight ratio of the coarse fraction to the fine fraction will range from about 70:30 to about 90:10.
  • the weight ratio of the coarse fraction to the fine fraction may range for example from about 60:40 to about 80:20.
  • the particle size distributions of the coarse and fine fractions do not overlap and in some embodiments the different size components of the compact are separated by an order of magnitude between the separate size fractions making up the multimodal distribution.
  • the embodiments consists of at least a wide bi-modal size distribution between the coarse and fine fractions of superhard material, but some embodiments may include three or even four or more size modes which may, for example, be separated in size by an order of magnitude, for example, a blend of particle sizes whose average particle size is 20 microns, 2 microns, 200nm and 20nm.
  • Sizing of diamond particles/grains into fine fraction, coarse fraction, or other sizes in between, may be through known processes such as jet-milling of larger diamond grains and the like.
  • the diamond grains used to form the polycrystalline diamond material may be natural or synthetic.
  • the binder catalyst/solvent may comprise cobalt or some other iron group elements, such as iron or nickel, or an alloy thereof. Carbides, nitrides, borides, and oxides of the metals of Groups IV-VI in the periodic table are other examples of non-diamond material that might be added to the sinter mix.
  • the binder/catalyst/sintering aid may be Co.
  • the cemented metal carbide substrate may be conventional in composition and, thus, may be include any of the Group IVB, VB, or VIB metals, which are pressed and sintered in the presence of a binder of cobalt, nickel or iron, or alloys thereof.
  • the metal carbide is tungsten carbide.
  • both the bodies of, for example, diamond and carbide material plus sintering aid/binder/catalyst are applied as powders and sintered simultaneously in a single UHP/HT process.
  • the mixture of diamond grains and mass of carbide are placed in an HP/HT reaction cell assembly and subjected to HP/HT processing.
  • the HP/HT processing conditions selected are sufficient to effect intercrystalline bonding between adjacent grains of abrasive particles and, optionally, the joining of sintered particles to the cemented metal carbide support.
  • the processing conditions generally involve the imposition for about 3 to 120 minutes of a temperature of at least about 1200 degrees C and an ultra-high pressure of greater than about 5 GPa.
  • the substrate may be pre-sintered in a separate process before being bonded together in the HP/HT press during sintering of the ultrahard polycrystalline material.
  • both the substrate and a body of polycrystalline superhard material are pre-formed.
  • the bimodal feed of ultrahard grains/particles with optional carbonate binder-catalyst also in powdered form are mixed together, and the mixture is packed into an appropriately shaped canister and is then subjected to extremely high pressure and temperature in a press.
  • the pressure is at least 5 GPa and the temperature is at least around 1200 degrees C.
  • the preformed body of polycrystalline superhard material is then placed in the appropriate position on the upper surface of the preform carbide substrate (incorporating a binder catalyst), and the assembly is located in a suitably shaped canister.
  • the assembly is then subjected to high temperature and pressure in a press, the order of temperature and pressure being again, at least around 1200 degrees C and 5 GPa respectively.
  • the solvent/catalyst migrates from the substrate into the body of superhard material and acts as a binder-catalyst to effect intergrowth in the layer and also serves to bond the layer of polycrystalline superhard material to the substrate.
  • the sintering process also serves to bond the body of superhard polycrystalline material to the substrate.
  • An embodiment of a superhard construction may be made by a method including providing a cemented carbide substrate, contacting an aggregated, substantially unbonded mass of diamond particles against a surface of the substrate to form an pre-sinter assembly, encapsulating the pre-sinter assembly in a capsule for an ultra-high pressure furnace and subjecting the pre-sinter assembly to a pressure of at least about 5.5 GPa and a temperature of at least about 1 ,250 degrees centigrade, and sintering the diamond particles to form a PCD composite compact element comprising a PCD structure integrally formed on and joined to the cemented carbide substrate.
  • the pre-sinter assembly may be subjected to a pressure of at least about 6 GPa, at least about 6.5 GPa, at least about 7 GPa or even at least about 7.5 GPa.
  • the hardness of cemented tungsten carbide substrate may be enhanced by subjecting the substrate to an ultra-high pressure and high temperature, particularly at a pressure and temperature at which diamond is thermodynamically stable.
  • the magnitude of the enhancement of the hardness may depend on the pressure and temperature conditions.
  • the hardness enhancement may increase the higher the pressure. Whilst not wishing to be bound by a particular theory, this is considered to be related to the Co drift from the substrate into the PCD during press sintering, as the extent of the hardness increase is directly dependent on the decrease of Co content in the substrate.
  • solvent / catalyst material may be included or introduced into the aggregated mass of diamond grains from a source of the material other than the cemented carbide substrate.
  • the solvent / catalyst material may comprise cobalt that infiltrates from the substrate in to the aggregated mass of diamond grains just prior to and during the sintering step at an ultra-high pressure.
  • Solvent / catalyst for diamond may be introduced into the aggregated mass of diamond grains by various methods, including blending solvent / catalyst material in powder form with the diamond grains, depositing solvent / catalyst material onto surfaces of the diamond grains, or infiltrating solvent / catalyst material into the aggregated mass from a source of the material other than the substrate, either prior to the sintering step or as part of the sintering step.
  • CVD chemical vapour deposition
  • PVD physical vapour deposition
  • ALD atomic layer deposition
  • cobalt may be deposited onto surfaces of the diamond grains by first depositing a pre-cursor material and then converting the precursor material to a material that comprises elemental metallic cobalt.
  • cobalt carbonate may be deposited on the diamond grain surfaces using the following reaction:
  • the deposition of the carbonate or other precursor for cobalt or other solvent / catalyst for diamond may be achieved by means of a method described in PCT patent publication number WO/2006/032982.
  • the cobalt carbonate may then be converted into cobalt and water, for example, by means of pyrolysis reactions such as the following:
  • cobalt powder or precursor to cobalt such as cobalt carbonate
  • diamond grains may be blended with the diamond grains.
  • a precursor to a solvent / catalyst such as cobalt
  • the cemented carbide substrate may be formed of tungsten carbide particles bonded together by the binder material, the binder material comprising an alloy of Co, Ni and Cr.
  • the tungsten carbide particles may form at least 70 weight percent and at most 95 weight percent of the substrate;.
  • the binder material may comprise between about 10 to 50 wt.% Ni, between about 0.1 to 10 wt.% Cr, and the remainder weight percent comprises Co.
  • the size distribution of the tungsten carbide particles in the cemented carbide substrate ion some embodiments has the following characteristics:
  • the binder additionally comprises between about 2 to 20 wt.% tungsten and between about 0.1 to 2 wt.% carbon
  • a layer of the substrate adjacent to the interface with the body of polycrystalline diamond material may have a thickness of, for example, around 100 microns and may comprise tungsten carbide grains, and a binder phase.
  • This layer may be characterised by the following elemental composition measured by means of Energy-Dispersive X-Ray Microanalysis (EDX):
  • the elemental composition includes between about 0.5 to 2.0 wt% cobalt, between about 0.05 to 0.5 wt.% nickel and between about 0.05 to 0.2 wt.% chromium, the remainder is tungsten and carbon.
  • the layer of substrate may further comprise free carbon.
  • the magnetic properties of the cemented carbide material may be related to important structural and compositional characteristics.
  • the most common technique for measuring the carbon content in cemented carbides is indirectly, by measuring the concentration of tungsten dissolved in the binder to which it is indirectly proportional: the higher the content of carbon dissolved in the binder the lower the concentration of tungsten dissolved in the binder.
  • the following formula may be used to relate magnetic saturation, Ms, to the concentrations of W and C in the binder:
  • the binder cobalt content within a cemented carbide material may be measured by various methods well known in the art, including indirect methods such as such as the magnetic properties of the cemented carbide material or more directly by means of energy-dispersive X-ray spectroscopy (EDX), or a method based on chemical leaching of Co.
  • indirect methods such as such as the magnetic properties of the cemented carbide material or more directly by means of energy-dispersive X-ray spectroscopy (EDX), or a method based on chemical leaching of Co.
  • the mean grain size of carbide grains may be determined by examination of micrographs obtained using a scanning electron microscope (SEM) or light microscopy images of metallurgically prepared cross-sections of a cemented carbide material body, applying the mean linear intercept technique, for example.
  • the mean size of the WC grains may be estimated indirectly by measuring the magnetic coercivity of the cemented carbide material, which indicates the mean free path of Co intermediate the grains, from which the WC grain size may be calculated using a simple formula well known in the art. This formula quantifies the inverse relationship between magnetic coercivity of a Co- cemented WC cemented carbide material and the Co mean free path, and consequently the mean WC grain size. Magnetic coercivity has an inverse relationship with MFP.
  • the "mean free path" (MFP) of a composite material such as cemented carbide is a measure of the mean distance between the aggregate carbide grains cemented within the binder material.
  • the mean free path characteristic of a cemented carbide material may be measured using a micrograph of a polished section of the material. For example, the micrograph may have a magnification of about 1000x.
  • the MFP may be determined by measuring the distance between each intersection of a line and a grain boundary on a uniform grid.
  • the matrix line segments, Lm are summed and the grain line segments, Lg, are summed.
  • the mean matrix segment length using both axes is the "mean free path". Mixtures of multiple distributions of tungsten carbide particle sizes may result in a wide distribution of MFP values for the same matrix content. This is explained in more detail below.
  • the concentration of W in the Co binder depends on the C content. For example, the W concentration at low C contents is significantly higher.
  • the W concentration and the C content within the Co binder of a Co-cemented WC (WC-Co) material may be determined from the value of the magnetic saturation.
  • the magnetic saturation 4 ⁇ or magnetic moment ⁇ of a hard metal, of which cemented tungsten carbide is an example, is defined as the magnetic moment or magnetic saturation per unit weight.
  • the magnetic moment, ⁇ , of pure Co is 16.1 micro-Tesla times cubic metre per kilogram ⁇ T.m 3 /kg), and the induction of saturation, also referred to as the magnetic saturation, 4 ⁇ , of pure Co is 201.9 ⁇ . ⁇ 3 / ⁇ 3 ⁇ 4.
  • the cemented carbide substrate may have a mean magnetic coercivity of at least about 100 Oe and at most about 145 Oe, and a magnetic moment of specific magnetic saturation with respect to that of pure Co of at least about 89 percent to at most about 97 percent.
  • a desired MFP characteristic in the substrate may be accomplished several ways known in the art. For example, a lower MFP value may be achieved by using a lower metal binder content. A practical lower limit of about 3 weight percent cobalt applies for cemented carbide and conventional liquid phase sintering. In an embodiment where the cemented carbide substrate is subjected to an ultra-high pressure, for example a pressure greater than about 5 GPa and a high temperature (greater than about 1,400°C for example), lower contents of metal binder, such as cobalt, may be achieved.
  • the MFP would be about 0.1 micron, and where the mean size of the WC grains is about 2 microns, the MFP would be about 0.35 microns, and where the mean size of the WC grains is about 3 microns, the MFP would be about 0.7 microns.
  • These mean grain sizes correspond to a single powder class obtained by natural comminution processes that generate a log normal distribution of particles. Higher matrix (binder) contents would result in higher MFP values.
  • the substrate comprises Co, Ni and Cr.
  • the binder material for the substrate may include at least about 0.1 weight percent to at most about 5 weight percent one or more of V, Ta, Ti, Mo, Zr, Nb and Hf in solid solution.
  • the polycrystalline diamond (PCD) composite compact element may include at least about 0.01 weight percent and at most about 2 weight percent of one or more of Re, Ru, Rh, Pd, Re, Os, Ir and Pt.
  • a polycrystalline construction according to some embodiments may have a specific weight loss in an erosion test in a recirculating rig generating an impinging jet of liquid-solid slurry below 2x10 "3 g/cm 3 at the following testing conditions: a temperature of 50°C, an impingement angle of 45°, a slurry velocity of 20 m/s, a pH of 8.02, a duration of 3 hours, and a slurry composition in 1 cubic meter water of: 40 kg Bentonite; 2 kg Na2CO3; 3 kg carboxymethyl cellulose, 5 litres
  • a cemented carbide body may be formed by providing tungsten carbide powder having a mean equivalent circle diameter (ECD) size in the range from about 0.2 microns to about 0.6 microns, the ECD size distribution having the further characteristic that fewer than 45 percent of the carbide particles have a mean size of less than 0.3 microns; 30 to 40 percent of the carbide particles have a mean size of at least 0.3 microns and at most 0.5 microns; 18 to 25 percent of the carbide particles have a mean size of greater than 0.5 microns and at most 1 micron; fewer than 3 percent of the carbide particles have a mean size of greater than 1 micron.
  • ECD mean equivalent circle diameter
  • the tungsten carbide powder is milled with binder material comprising Co, Ni and Cr or chromium carbides, the equivalent total carbon comprised in the blended powder being, for example, about 6 percent with respect to the tungsten carbide.
  • binder material comprising Co, Ni and Cr or chromium carbides, the equivalent total carbon comprised in the blended powder being, for example, about 6 percent with respect to the tungsten carbide.
  • the blended powder is then compacted to form a green body and the green body is sintered to produce the cemented carbide body.
  • the sintering the green body may take place at a temperature of, for example, at least 1 ,400 degrees centigrade and at most 1 ,440 degrees centigrade for a period of at least 65 minutes and at most 85 minutes.
  • the equivalent total carbon (ETC) comprised in the cemented carbide material is about 6.12 percent with respect to the tungsten carbide.
  • the size distribution of the tungsten carbide powder may, in some embodiments, have the characteristic of a mean ECD of 0.4 microns and a standard deviation of 0.1 microns.
  • the catalysing material may removed from a region of the polycrystalline layer adjacent an exposed surface thereof. Generally, that surface will be on a side of the polycrystalline layer opposite to the substrate and will provide a working surface for the polycrystalline diamond layer. Removal of the catalysing material may be carried out using methods known in the art such as electrolytic etching, and acid leaching and evaporation techniques.
  • a quantity of sub-micron cobalt powder sufficient to obtain 2 mass% in the final diamond mixture was initially de-agglomerated in a methanol slurry in a ball mill with WC milling media for 1 hour.
  • a fine fraction of diamond powder with an average grain size of 2 ⁇ was then added to the slurry in an amount to obtain 10 mass % in the final mixture.
  • Additional milling media was introduced and further methanol was added to obtain suitable slurry; and this was milled for a further hour.
  • a coarse fraction of diamond, with an average grain size of approximately 20 ⁇ was then added in an amount to obtain 88 mass % in the final mixture.
  • the slurry was again supplemented with further methanol and milling media, and then milled for a further 2 hours. The slurry was removed from the ball mill and dried to obtain the diamond powder mixture.
  • the diamond powder mixture was then placed into a suitable HpHT vessel, adjacent to a tungsten carbide substrate and sintered at a pressure of around 6.8 GPa and a temperature of about 1500 °C.
  • Example 2
  • a quantity of sub-micron cobalt powder sufficient to obtain 2.4 mass% in the final diamond mixture was initially de-agglomerated in a methanol slurry in a ball mill with WC milling media for 1 hour.
  • a fine fraction of diamond powder with an average grain size of 2 ⁇ was then added to the slurry in an amount to obtain 29.3 mass % in the final mixture.
  • Additional milling media was introduced and further methanol was added to obtain a suitable slurry; and this was milled for a further hour.
  • a coarse fraction of diamond, with an average grain size of approximately 20 ⁇ was then added in an amount to obtain 68.3 mass % in the final mixture.
  • the slurry was again supplemented with further methanol and milling media, and then milled for a further 2 hours.
  • the slurry was removed from the ball mill and dried to obtain the diamond powder mixture.
  • the diamond powder mixture was then placed into a suitable HpHT vessel, adjacent to a tungsten carbide substrate and sintered at a pressure of around 6.8 GPa and a temperature of about 1500 °C.
  • the diamond content of the sintered diamond structure is greater than 90 vol% and the coarsest fraction of the distribution is greater than 60 weight % and preferably greater than weight 70%.
  • the PCD compact formed according to Example 2 was then compared in a vertical boring mill test with commercially available polycrystalline diamond cutter elements.
  • the wear flat area was measured as a function of the number of passes of the cutter element boring into the workpiece.
  • the results obtained are illustrated graphically by Figure 3.
  • the results provide an indication of the total wear scar area plotted against cutting length. It will be seen that the PCD compact formed according to example 2 was able to achieve a greater cutting length and smaller wear scar area than that occurring in a conventional PCD compacts which were subjected to the same test for comparison.
  • the conventional PCD compacts in this test comprised Ref 1 which was sintered at a pressure of 6.8GPa and had an average diamond grain size of around 1 1 .3 microns and Ref 2 which was sintered at a pressure of 6.8GPa and had a grain size of around 9.5 microns.
  • individual diamond particles/grains are, to a large extent, bonded to adjacent particles/grains through diamond bridges or necks.
  • the individual diamond particles/grains retain their identity, or generally have different orientations.
  • the average grain/particle size of these individual diamond grains/particles may be determined using image analysis techniques. Images are collected on a scanning electron microscope and are analysed using standard image analysis techniques. From these images, it is possible to extract a representative diamond particle/grain size distribution.
  • the body of polycrystalline diamond material will be produced and bonded to the cemented carbide substrate in a HPHT process.
  • the binder phase and diamond particles it is advantageous for the binder phase and diamond particles to be arranged such that the binder phase is distributed homogeneously and is of a fine scale.
  • the homogeneity or uniformity of the sintered structure is defined by conducting a statistical evaluation of a large number of collected images.
  • the distribution of the binder phase which is easily distinguishable from that of the diamond phase using electron microscopy, can then be measured in a method similar to that disclosed in EP 0974566.
  • This method allows a statistical evaluation of the average thicknesses of the binder phase along several arbitrarily drawn lines through the microstructure.
  • This binder thickness measurement is also referred to as the "mean free path" by those skilled in the art.
  • the material which has the smaller average thickness will tend to be more homogenous, as this implies a "finer scale" distribution of the binder in the diamond phase.
  • the smaller the standard deviation of this measurement the more homogenous is the structure.
  • a large standard deviation implies that the binder thickness varies widely over the microstructure, i.e. that the structure is not even, but contains widely dissimilar structure types.
  • the binder and diamond mean free path measurements were obtained for various samples formed according to embodiments in the manner set out below.
  • dimensions of mean free path within the body of PCD material refer to the dimensions as measured on a surface of, or a section through, a body comprising PCD material and no stereographic correction has been applied.
  • the measurements are made by means of image analysis carried out on a polished surface, and a Saltykov correction has not been applied in the data stated herein.
  • samples are used to enhance the reliability and accuracy of the statistics.
  • the number of images used to measure a given quantity or parameter may be, for example between 10 to 30. If the analysed sample is uniform, which is the case for PCD, depending on magnification, 10 to 20 images may be considered to represent that sample sufficiently well.
  • the resolution of the images needs to be sufficiently high for the inter-grain and inter-phase boundaries to be clearly made out and, for the measurements stated herein an image area of 1280 by 960 pixels was used.
  • Images used for the image analysis were obtained by means of scanning electron micrographs (SEM) taken using a backscattered electron signal.
  • the back-scatter mode was chosen so as to provide high contrast based on different atomic numbers and to reduce sensitivity to surface damage (as compared with the secondary electron imaging mode). .
  • a sample piece of the PCD sintered body is cut using wire EDM and polished. At least 10 back scatter electron images of the surface of the sample are taken using a Scanning Electron Microscope at 1000 times magnifications.
  • the original image was converted to a greyscale image.
  • the image contrast level was set by ensuring the diamond peak intensity in the grey scale histogram image occurred between 10 and 20. .
  • An auto threshold feature was used to binarise the image and specifically to obtain clear resolution of the diamond and binder phases.
  • the software having the trade name analysis Pro from Soft Imaging System® GmbH (a trademark of Olympus Soft Imaging Solutions GmbH) was used and excluded from the analysis any particles which touched the boundaries of the image. This required appropriate choice of the image magnification:
  • Each particle was finally represented by the number of continuous pixels of which it is formed.
  • the Analysis software programme proceeded to detect and analyse each particle in the image. This was automatically repeated for several images.
  • Q1 is typically referred to as the first quartile (also called the lower quartile) and is the number below which lies the 25 percent of the bottom data.
  • Q3 is typically referred to as the third quartile (also called the upper quartile) has 75 percent of the data below it and the top 25 percent of the data above it.

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Abstract

L'invention concerne une construction polycristalline super-dure comprenant un corps en matériau polycristallin super-dur formé par une masse de grains super-durs présentant une liaison intergranulaire et définissant une pluralité de régions interstitielles entre eux, les grains super-durs ayant un libre parcours moyen associé, et une phase non super-dure remplissant au moins en partie une pluralité des régions interstitielles et ayant un libre parcours moyen associé. La médiane du libre parcours moyen associé avec la phase non super-dure divisée par (Q3-Q1) pour la phase non super-dure est supérieure ou égale à 0,83, Q1 étant le premier quartile et Q3 le troisième quartile ; et la médiane du libre parcours moyen associé avec les grains super-durs divisée par (Q3-Q1) pour les grains super-durs est inférieure à 0,47.
PCT/EP2013/062440 2012-06-15 2013-06-14 Constructions super-dures et leurs procédés de fabrication Ceased WO2013186386A1 (fr)

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GB201600001D0 (en) * 2016-01-01 2016-02-17 Element Six Uk Ltd Superhard constructions and methods of making same
US20190071932A1 (en) * 2017-09-06 2019-03-07 Varel International Ind., L.L.C. Superhard cutter having shielded substrate
GB201919480D0 (en) * 2019-12-31 2020-02-12 Element Six Uk Ltd Polycrystalline diamond constructions & methods of making same
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