US20190381569A1 - Superhard constructions & methods of making same - Google Patents

Superhard constructions & methods of making same Download PDF

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Publication number
US20190381569A1
US20190381569A1 US16/474,117 US201716474117A US2019381569A1 US 20190381569 A1 US20190381569 A1 US 20190381569A1 US 201716474117 A US201716474117 A US 201716474117A US 2019381569 A1 US2019381569 A1 US 2019381569A1
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Prior art keywords
super hard
grains
construction
diamond
fraction
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Maweja Kasonde
Teresa Rodriguez Suarez
Amanda Lynne Mckie
Edwin Stewart Eardley
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Elment Six Uk Ltd
Element Six UK Ltd
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Element Six UK Ltd
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Assigned to ELMENT SIX (UK) LIMITED reassignment ELMENT SIX (UK) LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: EARDLEY, Edwin Stewart, KASONDE, MAWEJA, MCKIE, Amanda Lynne, RODRIGUEZ SUAREZ, TERESA
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    • 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
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
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    • 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
    • C04B35/528—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 obtained from carbonaceous particles with or without other non-organic components
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C04B35/6264—Mixing media, e.g. organic solvents
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
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    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62685—Treating the starting powders individually or as mixtures characterised by the order of addition of constituents or additives
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/02—Local etching
    • 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
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00—Processes utilising sub- or super atmospheric pressure
    • B01J2203/06—High pressure synthesis
    • B01J2203/0605—Composition of the material to be processed
    • B01J2203/062—Diamond
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/241—Chemical after-treatment on the surface
    • B22F2003/244—Leaching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • 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
    • 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
    • B22F2207/00—Aspects of the compositions, gradients
    • B22F2207/01—Composition gradients
    • B22F2207/03—Composition gradients of the metallic binder phase in cermets
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/405—Iron group metals
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    • 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
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    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/528—Spheres
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Definitions

  • This disclosure relates to super hard constructions and methods of making such constructions, particularly but not exclusively to constructions comprising polycrystalline diamond (PCD) structures attached to a substrate, and tools comprising the same, particularly but not exclusively for use in rock degradation or drilling, or for boring into the earth.
  • PCD polycrystalline diamond
  • Polycrystalline super hard 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 super hard tool inserts may be limited by fracture of the super hard 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 a super 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 super 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 thermally stable product
  • PCD Polycrystalline diamond
  • PCD material is an example of a super hard material (also called a superabrasive material or ultra hard 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.
  • PCD polycrystalline diamond
  • a super hard polycrystalline construction comprising:
  • a method of forming a super hard polycrystalline construction comprising:
  • 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.
  • FIG. 1 is a perspective view of an example of a PCD cutter element or construction for a drill bit for boring into the earth;
  • FIG. 2 is a schematic cross-section of a conventional portion of a PCD microstructure with interstices between the inter-bonded diamond grains filled with a non-diamond phase material;
  • FIG. 3 is a cross-section through a first example of a super hard construction showing the microstructure of the construction
  • FIG. 4 is a plot showing the results of a vertical borer test comparing three example cutters with two conventional PCD cutter elements
  • FIG. 5 is a plot showing the results of a vertical borer test for two example cutters with four conventional PCD elements.
  • FIG. 6 is a plot showing the results of a vertical borer test for an example cutter with five conventional PCD elements.
  • a “super hard material” is a material having a Vickers hardness of at least about 28 GPa. Diamond and cubic boron nitride (cBN) material are examples of super hard materials.
  • a “super hard construction” means a construction comprising a body of polycrystalline super hard material. In such a construction, a substrate may be attached thereto.
  • polycrystalline diamond is a type of polycrystalline super hard (PCS) material comprising a mass of diamond grains, a substantial portion of which are directly inter-bonded (intergrown) with each other and in which the content of diamond is at least about 80 volume percent of the material.
  • PCS polycrystalline super hard
  • 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.
  • a “catalyst material” for a super hard material is capable of promoting the growth or sintering of the super hard material.
  • substrate as used herein means any substrate over which the super hard material layer is formed.
  • a “substrate” as used herein may be a transition layer formed over another substrate.
  • integrally formed means regions or parts are produced contiguous with each other and are not separated by a different kind of material.
  • FIG. 1 is a schematic view of an example of a conventional PCD super hard construction such as a cutting element 1 which includes a substrate 3 with a layer of super hard material 2 formed on the substrate 3 .
  • the substrate 3 may be formed of a hard material such as cemented tungsten carbide.
  • the super hard material 2 may be, for example, high density polycrystalline diamond (PCD) comprising at least 80 vol % of interbonded (intergrown) diamond grains.
  • the cutting element 1 may be mounted into a bit body such as a drag bit body (not shown) and may be suitable, for example, for use as a cutter insert for a drill bit for boring into the earth.
  • the exposed top surface of the super hard material opposite the substrate forms the cutting face 4 , also known as the working surface, which is the surface which, along with its edge 6 , performs the cutting in use.
  • the substrate 3 is generally cylindrical and has a peripheral surface 10 and a peripheral top edge 12 .
  • the working surface or “rake face” 4 of the polycrystalline composite construction 1 is the surface or surfaces over which the chips of material being cut flow when the cutter is used to cut material from a body, the rake face 4 directing the flow of newly formed chips.
  • This face 4 is commonly also referred to as the top face or working surface of the cutting element as the working surface 4 is the surface which, along with its edge 6 , is intended to perform the cutting of a body in use.
  • cutting edge refers to the actual cutting edge, defined functionally as above, at any particular stage or at more than one stage of the cutter wear progression up to failure of the cutter, including but not limited to the cutter in a substantially unworn or unused state.
  • chips are the pieces of a body removed from the work surface of the body being cut by the polycrystalline composite construction 1 in use.
  • a “wear scar” is a surface of a cutter formed in use by the removal of a volume of cutter material due to wear of the cutter.
  • a flank face may comprise a wear scar.
  • material may progressively be removed from proximate the cutting edge, thereby continually redefining the position and shape of the cutting edge, rake face and flank as the wear scar forms.
  • the substrate 3 is typically formed of a hard material such as a cemented carbide material, for example, cemented tungsten carbide.
  • the interstices 24 between the inter-bonded grains 22 of super hard material such as diamond grains in the case of PCD may be at least partly filled with a non-super hard phase material.
  • This non-super hard phase material also known as a filler material may comprise residual catalyst/binder material, for example cobalt.
  • the polycrystalline super hard material of examples comprises a matrix of fine grains (for example having a mean grain size of about 10 micrometres) with additional large grains embedded therein (for example having a mean particle size of about 30 micrometres) sintered using cobalt metal catalyst in an HPHT vehicle.
  • the super hard material of the various examples used to form the layer or region of super hard material may be, for example, polycrystalline diamond (PCD) and/or polycrystalline cubic boron nitride (PCBN) and/or lonsdalite and the super hard particles or grains may be of natural and/or synthetic origin.
  • PCD polycrystalline diamond
  • PCBN polycrystalline cubic boron nitride
  • lonsdalite and the super hard particles or grains may be of natural and/or synthetic origin.
  • the substrate of the examples may be formed of a hard material such as a cemented carbide material and may include, for example, cemented tungsten carbide, cemented tantalum carbide, cemented titanium carbide, cemented molybdenum carbide or mixtures thereof.
  • the binder metal for such carbides suitable for forming the substrate may be, for example, nickel, cobalt, iron or an alloy containing one or more of these metals and may include additional elements or compounds of other materials such as chromium, or vanadium. This binder may, for example, be present in an amount of 10 to 20 mass %, but this may be as low as 6 mass % or less.
  • the layer or region of super hard material may comprise PCBN.
  • Components comprising PCBN are used principally for machining metals.
  • PCBN material comprises a sintered mass of cubic boron nitride (cBN) grains.
  • the cBN content of PCBN materials may be at least about 40 volume %. When the cBN content in the PCBN is at least about 70 volume % there may be substantial direct contact among the cBN grains. When the cBN content is in the range from about 40 volume % to about 60 volume % of the compact, then the extent of direct contact among the cBN grains is limited.
  • PCBN may be made by subjecting a mass of cBN particles together with a powdered matrix phase, to a temperature and pressure at which the cBN is thermodynamically more stable than the hexagonal form of boron nitride, hBN.
  • PCBN is less wear resistant than PCD which may make it suitable for different applications to that of PCD.
  • a PCD or PCBN grade is a PCD or PCBN material characterised in terms of the volume content and size of diamond grains in the case of PCD or cBN grains in the case of PCBN, the volume content of interstitial regions between the grains, and composition of material that may be present within the interstitial regions.
  • a grade of super hard material may be made by a process including providing an aggregate mass of super hard grains having a size distribution suitable for the grade, optionally introducing catalyst material or additive material into the aggregate mass, and subjecting the aggregated mass in the presence of a source of catalyst material for the super hard material to a pressure and temperature at which the super hard grains are more thermodynamically stable than graphite (in the case of diamond) or hBN (in the case of CBN), and at which the catalyst material is molten. Under these conditions, molten catalyst material may infiltrate from the source into the aggregated mass and is likely to promote direct intergrowth between the diamond grains in a process of sintering, to form a polycrystalline super hard structure.
  • the aggregate mass may comprise loose super hard grains or super hard grains held together by a binder material. In the context of diamond, the diamond grains may be natural or synthesised diamond grains.
  • the grains of super hard material may be, for example, diamond grains or particles.
  • 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.
  • the coarse fraction may have an average grain size of at least 1.5 the size of the fine fraction, and may, in some examples, be at least 2 times the size of the fine fraction or up to around 10 times the size of the fine fraction, for example around 7 times the size.
  • the volume ratio of the coarse diamond fraction to the fine diamond fraction may range from about 5% to about 30% coarse diamond and the volume ratio of the fine diamond fraction may be from about 70% to about 95%.
  • Some examples consist of a wide bi-modal size distribution between the coarse and fine fractions of super hard material, but some examples may include three or even four or more size modes.
  • 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 cemented metal carbide substrate may, for example, be conventional in composition and, thus, may include any of the Group IVB, VB, or VI B 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.
  • the substrate may be pre-formed for example by pressing the green body of grains of hard material such as tungsten carbide into the desired shape, including the interface features at one free end thereof, and sintering the green body to form the substrate element.
  • the substrate interface features may be machined from a sintered cylindrical body of hard material, to form the desired geometry for the interface features.
  • the substrate may, for example, comprise WC particles bonded with a catalyst material such as cobalt, nickel, or iron, or mixtures thereof.
  • a green body for the superhard construction which comprises the pre-formed substrate, and the particles of superhard material such as diamond particles or cubic boron nitride particles, may be placed onto the substrate, to form a pre-sinter assembly which may be encapsulated in a capsule for an ultra-high pressure furnace, as is known in the art.
  • the superabrasive particles for example in powder form, are placed inside a metal cup formed, for example, of niobium, tantalum, or titanium.
  • the pre-formed substrate are placed inside the cup and hydrostatically pressed into the superhard powder such that the requisite powder mass is pressed around the interface features of the preformed carbide substrate to form the pre-composite.
  • the pre-composite is then outgassed at about 1050 degrees C.
  • the pre-composite is closed by placing a second cup at the other end and the pre-composite is sealed by cold isostatic pressing or EB welding.
  • the pre-composite is then sintered to form the sintered body.
  • the superhard grains may be diamond grains and the substrate may be cobalt-cemented tungsten carbide.
  • the pre-sinter assembly may comprise an additional source of catalyst material such as a disc or surrounding cup containing catalyst material such as cobalt which may be placed adjacent to and/or around the diamond grains in the pre-composite assembly.
  • the method may include loading the capsule comprising a pre-sinter assembly into a press and subjecting the green body to an ultra-high pressure and a temperature at which the superhard material is thermodynamically stable to sinter the superhard grains.
  • the green body may comprise diamond grains and the pressure to which the assembly is subjected is at least about 5 GPa and the temperature is at least about 1,300 degrees centigrade. In some examples, the pressure to which the assembly may be subjected is around 5.5-6 GPa, but in some examples it may be around 7.7 GPa or greater. Also, in some examples, the temperature used in the sintering process may be in the range of around 1400 to around 1500 degrees C.
  • the polycrystalline super hard constructions may be ground to size and may include, if desired, a 45° chamfer of approximately 0.4 mm height on the body of polycrystalline super hard material so produced.
  • 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.
  • Methods of depositing solvent/catalyst for diamond, such as cobalt, onto surfaces of diamond grains are well known in the art, and include chemical vapour deposition (CVD), physical vapour deposition (PVD), sputter coating, electrochemical methods, electroless coating methods and atomic layer deposition (ALD). It will be appreciated that the advantages and disadvantages of each depend on the nature of the sintering aid material and coating structure to be deposited, and on characteristics of the grain.
  • the binder/catalyst such as 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 WO2006/032982.
  • 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 cobalt powder or precursor to cobalt, such as cobalt carbonate.
  • 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 sintered cutter construction may be subjected to a leaching treatment process to remove accessible residual catalyst binder material from that layer or region, for example a boiling HCl acid leaching treatment.
  • the starting powders are prepared by milling 1 gram of spherical particle cobalt powder of particle size of about 2 micrometres in a Retsch planetary ball mill in 10 grams of liquid methanol with 125 grams of WC balls at 90 rpm for 10 minutes. Then 84 grams of the fine grain diamond material, in this case having an average particle size of 10 micrometres is added to the milled mixture together with 20 grams of methanol and 125 grams of WC balls. The mixture is milled for a further 20 minutes at 120 rpm.
  • the slurry is then dried in a rotovapor at 70 C to remove the solvent (methanol) and form a dry powder which is then sieved under 106 micrometres.
  • the precomposite To prepare the precomposite, about two grams of the dry powder is placed in a niobium cup. A WC substrate is introduced in the cup and pressed on the powder.
  • the precomposite can be compacted by a manual or hydraulic press or by vibration compaction.
  • the precomposite is then outgassed under vacuum at about 1100 C for 5 hours.
  • the outgassed precomposite is then sealed by electron beam welding to form a precomposite assembly.
  • the assembly is then subjected to an HPHT (high pressure and high temperature) sintering process at a temperature above 1450 C and a pressure above around 6 GPa to sinter the composite.
  • HPHT high pressure and high temperature
  • Example 1 Mean particle size of fine Mean particle size of course diamond diamond 4 m 10 m 15 m diamond diamond (vol. diamond (vol. 30 m diamond (vol. %) %) (vol. %) Example 1 85 15 Example 2 90 10 Example 3 85 15 Example 4 85 15 Example 5 70 15 15 Example 6 80 20 Example 7 70 30
  • the slurry was dried in a rotovapor at 70 C to remove the solvent (methanol) and the dry powder was sieved under 106 micrometres.
  • To prepare the precomposite about two grams of the dry powder was placed in a niobium cup. A WC substrate was introduced into the cup and pressed on the powder.
  • the precomposite may be compacted by a manual or hydraulic press or by vibration compaction.
  • the precomposite was then outgassed under vacuum at about 1100 C for 5 hours.
  • the outgassed precomposite was then sealed by electron beam welding to form a precomposite assembly which was then subjected to an HPHT treatment in an HPHT vehicle at a temperature above 1450 C and pressure above 6 GPa.
  • the cutter constructions prepared according to the above examples were recovered after sintering and fully processed.
  • the samples were also analysed using SEM imaging techniques which showed that the size ratios and sizes of the sintered grains were retained in the sintering process so corresponded to original sizes in the starting materials.
  • the constructions were treated to remove some or all accessible residual catalyst binder material in the interstitial spaces between the interbonded diamond grains of the sintered construction. This may be achieved by, for example, subjecting the cutter construction to a boiling HCl acid leaching treatment to remove all accessible catalysing material from the PCD structure, but other conventional techniques for leaching may be used.
  • the wear flat area was measured as a function of the number of passes of the cutter element boring into the workpiece.
  • the results provide an indication of the total wear scar area plotted against cutting length.
  • the example cutters denoted by reference numerals 102 , 104 and 106 were able to achieve a longer resistance to spalling indicated by the longer working life than the conventional cutters denoted by reference numerals 100 and 108 .
  • FIG. 5 which shows the results of a vertical borer test for two example cutters (denoted by reference numerals 208 and 210 ) compared to four conventional PCD cutters (reference numerals 200 , 202 , 204 , 206 , 212 and 214 ) the example cutters were able to achieve a longer resistance to spalling indicated by the longer working life than the conventional cutters.
  • FIG. 6 shows the results of a vertical borer test for an example cutter (reference numeral 310 ) with five conventional PCD cutters ( 300 , 302 , 304 , 306 , 308 ) which further confirms the example cutters were able to achieve a longer resistance to spalling indicated by the longer working life than the conventional cutters.
  • the super hard constructions of the examples may be finished by, for example, grinding, to provide a super hard element which is substantially cylindrical and having a substantially planar working surface, or a generally domed, pointed, rounded conical or frusto-conical working surface.
  • the super hard element may be suitable for use in, for example, a rotary shear (or drag) bit for boring into the earth, for a percussion drill bit or for a pick for mining or asphalt degradation.
  • the examples described have a single layer of super hard material, in other examples, only a portion of the cutting volume may be composed of the super hard material of the examples and the remainder of the cutting volume may be composed of a different material such as conventional PCD or a composition having a different diamond grade or grades or a ceramic material.
  • the coarse fraction particles may be, for example, single crystal particles or polycrystalline agglomerates of diamond grit, CVD crushed particles, diamond obtained by PVD methods, and/or natural or synthesised diamond.
  • ratio of particle sizes may be with reference to the equivalent diameter of coarse particles to the equivalent diameter of the fine particles in the matrix, it will be understood that the ratio of particle size may also be the ratio of volume fraction of the large particles divided by the volume fraction of the fine particles comprising the main matrix in the super hard region of the construction.

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US20230015853A1 (en) * 2019-12-31 2023-01-19 Element Six (Uk) Limited Sensor elements for a cutting tool and methods of making and using same

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CN113860301A (zh) * 2021-10-29 2021-12-31 河南联合精密材料股份有限公司 一种表面具有裂纹的类多晶钻石粉及其制备方法

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