WO2010100630A1 - Polycrystalline diamond element - Google Patents
Polycrystalline diamond element Download PDFInfo
- Publication number
- WO2010100630A1 WO2010100630A1 PCT/IB2010/050977 IB2010050977W WO2010100630A1 WO 2010100630 A1 WO2010100630 A1 WO 2010100630A1 IB 2010050977 W IB2010050977 W IB 2010050977W WO 2010100630 A1 WO2010100630 A1 WO 2010100630A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- melting point
- pcd
- low melting
- polycrystalline diamond
- metallic material
- Prior art date
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 85
- 239000010432 diamond Substances 0.000 title claims abstract description 85
- 230000008018 melting Effects 0.000 claims abstract description 88
- 238000002844 melting Methods 0.000 claims abstract description 88
- 239000000463 material Substances 0.000 claims abstract description 61
- 239000007769 metal material Substances 0.000 claims abstract description 44
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims description 29
- 229910052802 copper Inorganic materials 0.000 claims description 24
- 229910052709 silver Inorganic materials 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 16
- 239000000956 alloy Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 description 26
- 239000010941 cobalt Substances 0.000 description 26
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 26
- 239000010949 copper Substances 0.000 description 22
- 229910052751 metal Inorganic materials 0.000 description 22
- 239000002184 metal Substances 0.000 description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 19
- 239000004332 silver Substances 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 238000005553 drilling Methods 0.000 description 9
- 239000010439 graphite Substances 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000011435 rock Substances 0.000 description 8
- 238000001764 infiltration Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005755 formation reaction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 150000001247 metal acetylides Chemical class 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000003870 refractory metal Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000010438 granite Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000866 electrolytic etching Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 oxides Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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
- B24D3/10—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 for porous or cellular structure, e.g. for use with diamonds as abrasives
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
-
- 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
- E21B10/56—Button-type inserts
- E21B10/567—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts
- E21B10/5671—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts with chip breaking arrangements
-
- 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
- E21B10/5676—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts having a cutting face with different segments, e.g. mosaic-type 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
- E21B10/573—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts characterised by support details, e.g. the substrate construction or the interface between the substrate and the cutting element
- E21B10/5735—Interface between the substrate and the cutting element
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- PCD polycrystalline diamond
- Cutter inserts for drill bits for use in boring into the earth may comprise a layer of polycrystalline diamond (PCD) bonded to a cemented carbide substrate.
- PCD polycrystalline diamond
- Such cutter inserts may be referred to as polycrystalline diamond compacts (PDC).
- PCD is an example of a superhard, also called superabrasive, material comprising a mass of substantially inter-grown diamond grains, forming a skeletal mass defining interstices between the diamond grains.
- PCD material comprises at least about 80 volume % of diamond and may be 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 degrees centigrade in the presence of a sintering aid.
- Suitable sintering aids for PCD may also be referred to as a catalyst material for diamond.
- Catalyst material for diamond is understood to be material that is capable of promoting direct inter-growth of diamond grains at a pressure and temperature condition at which diamond is thermodynamically more stable than graphite. Some catalyst materials for diamond may promote the conversion of diamond to graphite at ambient pressure, particularly at elevated temperatures. Examples of catalyst materials for diamond are cobalt, iron, nickel and certain alloys including any of these.
- PCD may be formed on a cobalt-cemented tungsten carbide substrate, which may provide a source of cobalt catalyst material for the PCD.
- the interstices with PCD may at least partly be filled with a material, which may be referred to as a binder or a filler material. In particular the interstices may be wholly or partially filled with catalyst material for diamond.
- PCD bodies are commonly used as cutter inserts on drill bits used for boring into the earth in the oil and gas drilling industry.
- PCD bodies are also used for machining and milling metal-containing bodies, such as may be used in the auto manufacturing industry. In many of these applications the temperature of the PCD material becomes elevated as it engages a rock formation, workpiece or body with high energy.
- PCD is extremely hard and abrasion resistant, which is the reason it is the preferred tool material in some of the most extreme machining and drilling conditions, and where high productivity is required.
- a disadvantage of PCD containing certain catalyst materials for diamond as a filler material may be its relatively poor thermal stability above about 400 degrees centigrade.
- the catalyst material may promote the degradation of the PCD at elevated temperature, particularly at temperatures greater than about 750 degrees centigrade, as may be experienced in manufacture and use of PCD compacts.
- thermally stable diamond-bonded compacts that include a diamond-bonded body comprising a thermally stable region that extends a distance below a diamond-bonded body surface.
- the thermally stable region has a material microstructure comprising a matrix first phase of bonded together diamond crystals, and a second phase interposed within the matrix first phase.
- the second phase comprises one or more reaction products formed between one or more infiltrant material and the diamond crystals at high pressure / high temperature (HPHT) conditions.
- the infiltrant or replacement material may include one or more of the following elements: Si, Cu, Sn, Zn, Ag, Au, Ti, Cd, Al, Mg, Ga, Ge, which may also be used in compounds containing conventional solvent-catalyst materials (transition metals) where the solvent catalyst is rendered inactive by reaction with another material.
- United States patent application publication number 2008/0230280 discloses a PCD construction comprising a first region positioned remote from a surface and that includes a replacement material.
- the replacement material may be a noncatalyzing material that is disposed within interstitial regions between the diamond crystals in the first region.
- the noncatalyzing material can have a melting temperature of less than about 1 ,200 degrees centigrade and can be selected from low melting point metallic materials and/or alloys including elements, which can include those from Group IB of the Periodic table, such as copper. It is additionally desired that the replacement material display negligible or no solubility for carbon.
- PCD polycrystalline diamond
- a purpose of the invention is to provide a (PCD) element having enhanced thermal stability.
- a first aspect of the invention provides a polycrystalline diamond (PCD) element having internal diamond surfaces, the internal diamond surfaces defining interstices between them, the PCD element comprising a working surface, a low melting point region adjacent the working surface and in which the interstices are at least partially filled with a low melting point metallic material having a melting point of less than about 1 ,300 degrees centigrade at atmospheric pressure, or less than about 1 ,200 degrees centigrade at atmospheric pressure; and an intermediate region extending a distance of between about 5 microns and about 600 microns from a boundary defined by the low melting point region, the interstices of the intermediate region being at least partially filled with a catalyst material for diamond.
- PCD polycrystalline diamond
- the PCD element is bonded to a substrate at an interface and the intermediate region of the PCD element extends from the boundary defined by the low melting point region and the interface.
- the intermediate region extends a distance from the boundary of at most about 400 microns, at most about 200 microns, at most about 100 microns, at most about 50 microns, at most about 10 microns or even at most about 5 microns.
- the intermediate region extends a distance from the boundary of at least about 5 microns, at least about 10 microns, at least about 50 microns, at least about 100 microns, or even at least about 200 microns.
- the interstices of the intermediate region are at least 50% filled with a sintering aid or catalyst material for diamond, such as cobalt.
- the low melting point region extends a depth into the PCD element from the working surface, the depth being at most about 1 ,000 microns, at most about 500 microns or at most about 100 microns. In some embodiments, the low melting point region extends a depth into the PCD element from a working surface, the depth being at least about 5 microns, at least about 10 microns, at least about 50 microns, at least about 100 microns, or even at least about 200 microns.
- the low melting point region is in the form of a stratum or layer. In some embodiments, the low melting point region is in the form of a layer or stratum that extends to a depth of at least about 40 microns, at least about 100 microns or even at least about 200 microns from a working surface.
- the interstices within the low melting point region are at least 50 percent, at least about 70 percent, at least about 80 percent or at least about 90 percent filled with the low melting point metallic material.
- the low melting point metallic material has a melting point lower than 1 ,100 degrees centigrade at atmospheric pressure.
- the low melting point metallic material has a melting point greater than about 600 degrees centigrade or greater than about 700 degrees centigrade at atmospheric pressure.
- Embodiments of the invention have the advantage that the low melting point metallic material does not substantially melt when the PCD element, is brazed onto a tool carrier at temperatures of several hundred degrees centigrade.
- the low melting point metallic material is not capable of reacting to form a stable carbide at less than about 1 ,000 degrees centigrade at atmospheric pressure.
- Embodiments of the invention have the advantage that the low melting point metallic material does not react with the diamond to form carbides.
- the formation of carbide grains may retard the rate of infiltration of the low melting point metallic material in manufacture and may create undesirable stresses within the interstices due to volume changes occurring with the formation of new phases and compounds.
- the formation of carbides as a reaction product of a reaction between the low melting point metallic material and the diamond of the PCD would necessarily require some of the surrounding diamond to be sacrificed to the reaction, which may compromise the integrity of the microstructure.
- the low melting point metallic material is Ag, Mg, Cu or Pb in elemental form or an alloy including any of these elements, and in some embodiments the low melting point metallic material is Ag or Cu in elemental form or an alloy including either of these elements. In one embodiment, the low melting point metallic material has the characteristic that it is substantially resistant to oxidation.
- Embodiments of the invention have the advantage of having enhanced thermal stability without substantially compromising strength.
- the PCD element is bonded at an interface to a cemented carbide substrate, such as a cobalt-cemented tungsten carbide substrate, and in one embodiment, the PCD element is bonded to a hard-metal substrate via a bonding layer having a coefficient of thermal expansion intermediate that of the PCD and the hard-metal.
- the bonding layer comprises diamond grains and metal carbide, wherein the diamond grains are not substantially bonded to each other.
- the PCD element comprises an intermediate region that is remote from the working surface, in which the interstices are at least 50% filled with a catalyst material for diamond, the intermediate region being adjacent the interface and the low melting point region is remote from the interface.
- a second aspect of the invention provides an insert for a tool, the insert comprising an embodiment of a PCD element according to the invention.
- a third aspect of the invention provides a tool comprising an embodiment of an insert according to the invention.
- the tool is suitable for machining, drilling, boring, cutting or otherwise forming or degrading a hard or abrasive workpiece or other body, such as rock, concrete, asphalt, metal or hard composite materials.
- the tool is a drill bit for use in earth boring, rock drilling or rock degradation, as may be used in the oil and gas drilling and mining industries, and in one embodiment, the tool is a rotary drag bit for use in earth-boring and rock drilling in the oil and gas industry.
- a fourth aspect of the invention provides a method for making a PCD element, the method including providing a PCD body comprising a sintering aid within interstices of the PCD body, removing at least some of the sintering aid from a portion of the polycrystalline diamond element to form a porous region adjacent a working surface, and infiltrating or permeating at least a portion of the porous region with low melting point metallic material having a melting point of less than about 1,300 degrees centigrade at atmospheric pressure, or less than about 1 ,200 degrees centigrade at atmospheric pressure.
- substantially all of the sintering aid is removed from the PCD element.
- One embodiment of the method of the invention includes preventing or avoiding filling the pores within a part of the porous region with the low melting point metallic material.
- One embodiment of the method of the invention includes infiltrating a material comprising a catalyst material for diamond, such as cobalt, into a part of the porous region not filled with the low melting point metallic material.
- a controlled temperature cycle is employed in such a manner as to allow sufficient or a certain amount of the low melting point metallic material to be introduced into the porous region prior to infiltration with the material comprising a catalyst material for diamond.
- FIG 1 shows a schematic longitudinal cross sectional view of an embodiment of a PCD element.
- FIG 2 shows a schematic expanded cross sectional view of a region of the embodiment shown in FIG 1.
- FIG 3A shows schematic perspective views of components used in an embodiment of a method for manufacturing PCD compacts or inserts.
- FIG 3B shows a schematic perspective view of an embodiment of a PCD compact or insert.
- a "working surface" of an insert or element is any part of the insert or element which may in use contact a workpiece or body being worked. It is understood that any portion of a working surface is also a working surface.
- low melting point metallic material means metal in elemental or alloy form, which possesses the characteristic properties of a metal, including high electrical conductivity, thermal conductivity and fracture toughness.
- a catalyst material for diamond is a material that is capable of promoting the precipitation, growth and / or sintering-together of grains of diamond under a condition of pressure and temperature at which diamond is more thermodynamically stable than graphite.
- catalyst materials for diamond are iron, nickel, cobalt, manganese and certain alloys including any of these elements.
- Some catalyst materials for diamond are capable of promoting the conversion of diamond into graphite at ambient pressure, particularly at elevated temperatures.
- an embodiment of a PCD insert 200 comprises an embodiment of a PCD element 100 joined to a cemented carbide substrate 220 at an interface 116.
- the embodiment of the PCD element 100 has internal diamond surfaces 102, the internal diamond surfaces 102 defining interstices 104 between them.
- the PCD element 100 further comprises a working surface 114 and a low melting point region 111 adjacent the working surface 114 and in which the interstices 104 are at least partially filled with a low melting point metallic material having a melting point of less than about 1 ,300 degrees centigrade at atmospheric pressure, or less than about 1,200 degrees centigrade at atmospheric pressure.
- An intermediate region 112 extends a distance of between about 5 microns and about 600 microns from a boundary 116, the interstices 104 of the intermediate region 112 being at least partially filled with a catalyst material for diamond.
- the boundary is the interface (both indicated by reference number 116).
- PCD inserts of a wide range of shapes and sizes can be made, depending on the type of application.
- the inserts are particularly advantageous when used in applications where the insert may be subjected to high temperatures, and therefore where high thermal stability is important.
- An especially favoured application is as inserts for rotary drill bits used for rock drilling and earth boring in the oil and gas industry.
- an embodiment of a method for making a PCD element includes providing a PCD insert 300 that has been manufactured using an ultra-high pressure and high temperature (HPHT) method well- known in the art.
- the insert 300 comprises a PCD element 310 integrally bonded to a cemented carbide hard-metal substrate 320.
- the microscopic interstices (not shown) of the PCD element 310 are substantially filled with cobalt catalyst material.
- At least a part of PCD element 310 is detached from the insert 300 to produce a PCD body 311.
- One way of detaching the PCD element 310 is to grind away the substrate 320.
- the PCD body 311 is treated to remove catalyst material from the interstices to produce a porous and thermally stable PCD element 312.
- the porous PCD element 312 is then contacted on one side with a second cemented carbide substrate 340 and on the opposite side with a source 330 of low melting point metallic material.
- the source 330 may be in the form of a thin foil or disc, or powder.
- the substrate 340 includes tungsten carbide grains and a cobalt metal binder, the metal binder being capable of acting as a catalyst material to promote the growth and sintering of diamond grains.
- the porous PCD element 312, thus "sandwiched" between the substrate 340 and the foil or disc 330 is treated at an ultra-high pressure in excess of about 5GPa at temperatures sufficiently high to melt the low melting point metallic material and to melt the cobalt metal binder of the substrate 340, resulting in some of it infiltrating into the porous PCD element 312.
- the temperature cycle may be controlled in such a manner as to allow sufficient or a certain amount of the low melting point metallic material to be introduced into the porous PCD element 312 prior to the cobalt metal binder material melting and infiltrating into the porous PCD element 312.
- the resulting insert is removed and processed to final dimensions and tolerances to produce an embodiment of a finished PCD insert 200 shown in FIG 3B, comprising a PCD element 100 joined to a cemented carbide substrate 220.
- the PCD body has a thickness between a pair of opposite surfaces of at least about 1.5mm or at least about 1.8mm, one of the pair contacted with a source of low melting point metallic material and the other of the pair contacted with a source of catalyst material for diamond.
- One embodiment of the method of the invention includes heating a source of low melting point metallic material to a temperature within the range between the melting point of the low melting point metallic material and the melting point of the catalyst material, maintaining the temperature within this range for a period of time sufficient for the infiltration or permeation of the low melting point metallic material to be completed. In one embodiment, the temperature is then increased to greater than the melting point of the catalyst material for a period of time for the introduction of the catalyst material to be completed.
- One embodiment of the method includes contacting one surface of a porous PCD body with a source of silver, contacting another surface of the PCD body with a source of cobalt to form an assembly, subjecting the assembly to a pressure of at least about 5.5GPa, heating the assembly to a temperature in the range above the melting point of silver at the pressure and below the melting point of cobalt at the pressure, maintaining temperature within this range for a period of time of at least about 2 minutes or at least about 3 minutes, and then increasing the temperature to above the melting point of cobalt at the pressure.
- One embodiment of the method includes contacting one surface of a porous PCD body with a source of copper, contacting another surface of the PCD body with a source of cobalt to form an assembly, subjecting the assembly to a pressure of at least about 5.5GPa, heating the assembly to a temperature in the range above the melting point of copper at the pressure and below the melting point of cobalt at the pressure, maintaining temperature within this range for a period of time of at least about 1 minute or at least about 2 minutes, and then increasing the temperature to above the melting point of cobalt at the pressure.
- the period of time is at most about 15 minutes or even at most about 10 minutes.
- the sintered PCD body can be produced in an ultra-high pressure furnace by sintering together diamond grains in the presence of a catalyst material for diamond at a pressure of at least about 5.5GPa and a temperature of at least about 1 ,300 degrees centigrade.
- the catalyst material may comprise a conventional transition metal type diamond catalyst material, such as cobalt, iron or nickel, or certain alloys thereof.
- the sintered PCD body, as a whole or at least a region thereof, may then be rendered thermally stable, for example, through the removal of the majority of binder catalyst material from the PCD body or desired region using acid leaching or another similar process known in the art.
- the catalyst material present in the PCD body 311 may be removed by any of various methods known in the art, such as electrolytic etching, evaporation techniques, acid leaching (for example by immersion in a liquor containing hydrofluoric acid, nitric acid or mixtures thereof) or by means of chlorine gas, as disclosed in international patent publication number WO2007/042920, or by another method (e.g. as disclosed in South African patent number 2006/00378).
- a PCD insert similar to PCD insert 300 in FIG 3A is provided.
- a region adjacent the working surface of the PCD element is depleted substantially of catalyst material by means of method known in the art, resulting in the region being porous.
- a low melting point metallic material is introduced into the pores of the porous region. The parameters of the method of introduction may be controlled to retain porosity within part of the porous region.
- a catalyst material is then infiltrated into the remaining pores of the masked or passivated region.
- the pressure is at least about 5.5 GPa, at least about 6GPa or at least about 6.5GPa. In one embodiment, the pressure is about 6.8GPa.
- the low melting point metallic materials according to the invention are substantially inert with respect to diamond and do not substantially promote its dissolution or degradation at ambient pressures. They may function as a heat conducting filler within the PCD element. While wishing not to be bound by any particular hypothesis, low melting point metallic materials are believed not to degrade diamond at the high temperatures that may be experienced in use, i.e. up to about 1 ,100 degrees centigrade. At temperatures for which the low melting point metallic material is in the solid phase, its presence in the interstices may enhance the strength of the PCD. In addition, the high thermal conductivity of the low melting point metallic material may further enhance the thermal stability of the polycrystalline diamond element in comparison to leached PCD.
- the low melting point metallic material At temperatures for which the low melting point metallic material is in or close to the molten phase, stress may be prevented from building up within the PCD by virtue of the low melting point metallic material leaking from the interstices as it thermally expands or melts. Solid metals close to their melting points generally have greatly reduced yield strength, which reduces build up of micro-stresses that may arise from a mismatch in the thermal expansion coefficients. Melting or softening of the metal may have the additional benefit of lubricating the action of the polycrystalline diamond element at high temperatures.
- the low melting point of the low melting point metallic material means that relatively low temperatures are required to infiltrate it into a polycrystalline diamond element in manufacture. In some embodiments of the method of the invention, the rate and extent of infiltration may readily be controlled by controlling its viscosity by controlling the temperature, without need to use very high temperatures.
- a PCD insert having a diameter of about 16mm and for use in a rotary drag bit for oil and gas drilling was used as the starting component.
- the insert was substantially cylindrical in form and comprised a PCD layer integrally bonded to a Co-cemented WC hard-metal substrate.
- the PCD layer was about 2.3 mm thick and the diamond grain size distribution was of a multi-modal type, comprising sintered diamond grains with average grain size of less than about 20 microns, the interstices between the diamond grains being filled with Co, a catalyst metal sourced from the hard-metal substrate during the step of IS
- the porous PCD disc was then re-infiltrated with cobalt from one side and copper from an opposite side, and simultaneously re-bonded to a second Co- cemented WC substrate.
- This re-infiltration step was carried out at an ultrahigh pressure of greater than about 5GPa, at which diamond is thermodynamically stable, and a temperature of about 1 ,400 degrees centigrade at which Co is molten at the ultra-high pressure.
- a pre-form assembly was prepared, the pre-form assembly comprising the porous PCD disc placed onto a flat surface of a cylindrical substrate, and a thin film of copper placed on top of the porous PCD disc.
- the copper film was less than 0.5mm thick and had been ultrasonically cleaned in an acetone bath.
- the assembly comprising the PCD disc thus "sandwiched" between the copper foil and the substrate was placed within a refractory metal jacket, which was subsequently placed within a ceramic support and subsequently sealed within another metal casing, as is well known in the art.
- the pre-form assembly was assembled into a capsule for an ultra-high pressure furnace and subjected to the ultra-high pressure and temperature. The temperature was increased from ambient to the maximum level over a period of time once the target pressure had been achieved.
- the insert was removed from the ultra-high pressure apparatus and the casing and jacketing was removed.
- the insert was then sliced into two parts along an axial plane, producing two cross- sectional surfaces. One of these surfaces was polished and analysed by means of SEM (scanning electron microscopy), revealing that the PCD had bonded well with the substrate and that substantially all of the interstices within the PCD were filled with copper, cobalt, or a combination of copper and cobalt.
- the copper had infiltrated from the flat working surface to a depth of about 1.7mm, a region with a depth of about 1.3mm from the flat working surface being substantially free of cobalt.
- the PCD interstices within about 0.2mm from the substrate were filled principally with cobalt, although some copper was evident.
- a second test insert was made as above and subjected to a wear test, which involved using the insert, suitably prepared as would be appreciated by the skilled person, to machine a granite block mounted on a vertical turret milling apparatus.
- the PCD layer displayed excellent wear resistance and thermal stability.
- a re-infiltrated insert was made using the same process as in Example 1 , the only difference being that a silver foil was used instead of a copper foil.
- the insert was also analysed and tested as in Example 1.
- the silver had infiltrated more deeply into the PCD than had the copper, to a depth of about 2.2mm from the flat working surface. This is believed to be due to the lower melting point of silver and consequently the fact that it would have melted at an earlier stage than the copper, therefore having more time to infiltrate the porous PCD before the cobalt melted and began infiltrating from the opposing direction.
- a porous PCD disc can be prepared using the process described in Example 2, and the silver can be introduced into the pores prior to the treatment at ultra-high pressure. This can be done by placing the porous PCD disc into a graphite vessel, and disposing a silver film on top of it, the silver film having been ultra-sonically cleaned in an acetone bath. The vessel can then be placed in a furnace and its contents heated in a vacuum to above the melting point of the silver, i.e. to about 1 ,000 degrees centigrade, causing the silver foil to melt and infiltrate the PCD disc.
- a porous PCD disc can be prepared using the process described in Example 2 and silver can be introduced into the pores prior to the treatment at ultrahigh pressure by depositing a very thin film of silver onto a flat surface of the PCD disc by means of sputtering and then causing it to melt.
- the mass of the silver deposited can be calculated to be just sufficient for 10% of the pores to be filled with silver, and consequently to provide just enough silver to infiltrate the PCD to a depth of about 10% of its thickness, i.e. to a depth of about 230 microns from the flat surface, leaving the remaining pores substantially empty. This mass could be about 12.5 milligrams.
- the film thickness should be as uniform as possible across the PCD surface.
- the silver-coated PCD can then be placed into a graphite vessel, with the coated surface remote from the base of the graphite vessel (i.e. on the top surface), and the vessel placed into a furnace.
- the vessel and its contents can be heated in a vacuum to above the melting point of the silver, i.e. to i about 1 ,000 degrees centigrade, causing the silver coating to melt and infiltrate the PCD disc.
- a free-standing fully leached PCD disc was produced according to a similar process to that disclosed in Example 1.
- Diamond powder having a size distribution that can be resolved into at least two distinct peaks was placed against a cobalt cemented tungsten carbide substrate, and this assembly was encapsulated in a refractory metal jacket and subjected to an ultra-high pressure of at least about 5.5GPa and a temperature of at least about 1,500 degrees centigrade to sinter the diamond powder into a PCD layer bonded to the substrate.
- the PCD disc After sintering the PCD disc was separated from the substrate by lapping away the carbide base and substantially all of the cobalt was removed from the interstices of the PCD by means of leaching in an acid liquor, as is well known in the art, to form a porous PCD body having a generally disc form.
- a copper disc was placed against one end of the porous PCD body and a cobalt cemented tungsten carbide substrate was placed against the opposite end of the PCD body, and this assembly was encapsulated within a refractory metal jacket.
- the porous PCD body was thus sandwiched between the substrate and the copper disc.
- the copper disc had a thickness of about 0.25mm and diameter substantially the same as that of the PCD body.
- the mass of the copper discs was at around 420 mg, which equates to less than about 10 percent of the volume of the PCD body, and was at a level considered to be in excess of the volume required to fill the entire void created during the leaching process.
- the assembly was further encased in a manner known in the art for HPHT sintering and subjected to a second high pressure thermal cycle at a temperature of around 1,410 degrees centigrade and a pressure of around 5.2 GPa.
- the PCD insert comprising a PCD layer containing copper and cobalt, and joined to the substrate was recovered and machined to final specifications to form a PCD cutter insert.
- the PDC cutter insert was subjected to a milling test, which involved a high-
- a further material was made using the method disclosed in Example 5, but by substituting the copper disc with 520 mg of silver powder. Once again, the mass was chosen to correspond to around 10 vol % of the fully leached disc. The conditions selected for the second high pressure thermal cycle were identical to those used in Example 5. Performance results from this material showed an improvement in thermal stability above that of non-reinfiltrated PCD.
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Abstract
Description
Claims
Priority Applications (7)
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CN2010800163954A CN102395694A (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
CA2754150A CA2754150A1 (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
JP2011552569A JP2012519776A (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
EP10711264A EP2403969A1 (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
RU2011140403/02A RU2011140403A (en) | 2009-03-06 | 2010-03-08 | ELEMENT FROM POLYCRYSTALLINE DIAMOND |
US13/254,455 US20120061149A1 (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
US14/331,547 US20150174733A1 (en) | 2009-03-06 | 2014-07-15 | Polycrystalline diamond element |
Applications Claiming Priority (2)
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GBGB0903826.6A GB0903826D0 (en) | 2009-03-06 | 2009-03-06 | Polycrystalline diamond element |
GB0903826.6 | 2009-03-06 |
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US13/254,455 A-371-Of-International US20120061149A1 (en) | 2009-03-06 | 2010-03-08 | Polycrystalline diamond element |
US14/331,547 Continuation US20150174733A1 (en) | 2009-03-06 | 2014-07-15 | Polycrystalline diamond element |
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WO2010100630A1 true WO2010100630A1 (en) | 2010-09-10 |
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US (2) | US20120061149A1 (en) |
EP (1) | EP2403969A1 (en) |
JP (1) | JP2012519776A (en) |
KR (1) | KR20120006017A (en) |
CN (1) | CN102395694A (en) |
CA (1) | CA2754150A1 (en) |
GB (1) | GB0903826D0 (en) |
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WO (1) | WO2010100630A1 (en) |
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Also Published As
Publication number | Publication date |
---|---|
EP2403969A1 (en) | 2012-01-11 |
CN102395694A (en) | 2012-03-28 |
RU2011140403A (en) | 2013-04-20 |
GB0903826D0 (en) | 2009-04-22 |
US20120061149A1 (en) | 2012-03-15 |
US20150174733A1 (en) | 2015-06-25 |
KR20120006017A (en) | 2012-01-17 |
CA2754150A1 (en) | 2010-09-10 |
JP2012519776A (en) | 2012-08-30 |
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