WO2012089565A1 - Matériau super-dur polycristallin de haute densité - Google Patents
Matériau super-dur polycristallin de haute densité Download PDFInfo
- Publication number
- WO2012089565A1 WO2012089565A1 PCT/EP2011/073463 EP2011073463W WO2012089565A1 WO 2012089565 A1 WO2012089565 A1 WO 2012089565A1 EP 2011073463 W EP2011073463 W EP 2011073463W WO 2012089565 A1 WO2012089565 A1 WO 2012089565A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- diamond
- polycrystalline superhard
- superhard material
- bonding
- grains
- Prior art date
Links
- 239000000463 material Substances 0.000 title claims abstract description 120
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 104
- 239000010432 diamond Substances 0.000 claims abstract description 104
- 239000002245 particle Substances 0.000 claims abstract description 47
- 229910052582 BN Inorganic materials 0.000 claims abstract description 34
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 10
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052733 gallium Inorganic materials 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 150000004767 nitrides Chemical class 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 229910052790 beryllium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims description 3
- 229910052762 osmium Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 40
- 239000002775 capsule Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001534 heteroepitaxy Methods 0.000 description 3
- 238000001657 homoepitaxy Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003863 metallic catalyst Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910033181 TiB2 Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 229910021387 carbon allotrope Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- -1 for example Co Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000004943 liquid phase epitaxy Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005334 plasma enhanced chemical vapour deposition Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000000348 solid-phase epitaxy Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
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- 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
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- C04B35/522—Graphite
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- 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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- C04B35/6316—Binders based on silicon compounds
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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
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Definitions
- This disclosure relates to a high density polycrystalline superhard material, a method of making high density polycrystalline superhard material, and to a wear element comprising a high density polycrystalline superhard material.
- Cutter inserts for machine and other tools may comprise a layer of polycrystalline diamond (PCD) or polycrystalline cubic boron nitride (PCBN) bonded to a cemented carbide substrate.
- PCD and PCBN are examples of superhard materials, also called superabrasive materials, which have a hardness value substantially greater than that of cemented tungsten carbide.
- PCD comprises a mass of substantially inter-grown diamond grains forming a skeletal mass, which defines 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, also 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 within PCD material may at least partly be filled with the catalyst material.
- PCD 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 grains 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.
- GB 2 453 023 discloses an ultra-hard composite construction comprising an ultra-hard body having a plurality of diamond crystals bonded to one another by a carbide reaction product.
- the carbide reaction product is formed from a carbide former selected from silicon, boron, titanium, molybdenum or vanadium with diamond at HPHT conditions.
- the ultra-hard body resulting from the HPHT process comprises in the range of from about 40 to 90 percent by volume diamond.
- the body may include a further diamond region positioned along a surface portion of the body and that is substantially exclusively diamond, having a diamond content of 95 to 99 percent or more.
- a polycrystalline superhard material comprising a mass of diamond, graphite or cubic boron nitride particles or grains bonded together by one or more ultrathin inter-granular bonding layers, the inter-granular bonding layers having an average thickness of greater than about 0.3 nm and less than about 100 nm.
- ultrathin bonding layer(s) may improve toughness.
- the average thickness of the inter-granular bonding layers is less than about 20 nm, or less than about 10 nm, or less than about 5 nm.
- the average particle size of the diamond or cubic boron nitride particles or grains is from about 50 nanometres to about 50 microns.
- the diamond content of the polycrystalline diamond material may, in some embodiments, be at least about 90 percent, at least about 95 percent, or at least about 99 percent of the volume of the polycrystalline superhard material. In some embodiments, the content of the inter-granular bonding material is at most about 10 volume percent, at most about 5 volume percent, or at most about 1 volume percent of the polycrystalline superhard material.
- a method for making polycrystalline superhard material comprising providing a mass of diamond, graphite or cubic boron nitride particles or grains, depositing ultrathin layers of a bonding material on respective diamond, graphite or cubic boron nitride particles or grains, the bonding material being selected so as to be capable of forming bonds with the diamond, graphite or cubic boron nitride particles or grains, the average thickness of the deposited layers of bonding material being greater than about 0.5 nm and less than about 200 nm, consolidating the diamond, graphite or cubic boron nitride particles or grains and bonding material to form a green body, and subjecting the green body to a temperature and pressure at which the diamond, graphite or cubic boron nitride is thermodynamically stable, sintering and forming polycrystalline superhard material.
- the diamond particles or grains, prior to deposition of the bonding material may have, for example, an average particle or grain size of from about 50 nanometres to about 50 microns.
- a multimodal mixture of diamond particles or grains of varying average particle or grain size may be provided.
- the polycrystalline superhard material may be a standalone compact or the polycrystalline superhard material may be attached to a substrate.
- Sintering may be carried out at pressures of, for example, about 2.5 GPa or more, or 5 GPa or more, or 6.8 GPa or more, or 7.7 GPa or more, for example between about 8GPa to about 18GPa and temperatures of about 450 degrees centigrade or more, or 1500 degrees centigrade or more, or 2250 degrees centigrade or more, or 2400 degrees centigrade or more, for sintering times of 10 seconds or more, or 3 minutes or more, or 30 minutes or more.
- a wear element comprising a polycrystalline superhard material as described herein.
- high density polycrystalline diamond material comprises a mass of diamond particles or grains, a substantial portion of which are bonded to one another and in which the content of diamond is at least about 90 volume percent of the material.
- high density polycrystalline cubic boron nitride material comprises a mass of cubic boron nitride grains, a substantial portion of which are bonded to one another and in which the content of cubic boron nitride is at least about 90 volume percent of the material.
- epitaxy in its broadest sense is understood to include, but not limited to, the deposition of a polycrystalline or a monocrystalline layer of bonding material.
- the epitaxy may be “heteroepitaxy”, which is understood to mean that the superhard material and deposited layers of bonding material contain different components, or “homoepitaxy”, which is understood to mean that the superhard material and deposited layers of bonding material contain the same components.
- a “multi-modal size distribution of a mass of grains” is understood to mean that the grains have a size distribution with more than one peak, each peak corresponding to a respective "mode”.
- Multimodal polycrystalline bodies are typically made by providing more than one source of a plurality of grains, each source comprising grains having a substantially different average size, and blending together the grains or particles from the sources. Measurement of the size distribution of the blended grains typically reveals distinct peaks corresponding to distinct modes. When the grains are sintered together to form the polycrystalline body, their size distribution is further altered as the grains are compacted against one another and fractured, resulting in the overall decrease in the sizes of the grains. Nevertheless, the multimodality of the grains is usually still clearly evident from image analysis of the sintered article.
- a "green body” is an article that is intended to be sintered or which has been partially sintered, but which has not yet been fully sintered to form an end product. It may generally be self-supporting and may have the general form of the intended finished article.
- a "superhard wear element” is an element comprising a superhard material and is for use in a wear application, such as degrading, boring into, cutting or machining a workpiece or body comprising a hard or abrasive material.
- a polycrystalline superhard material having a high density of diamond or cubic boron nitride in its polycrystalline structure.
- a high-purity PCD or PCD-like material with high diamond density, high degree of bonding, very little or no free elements or compounds present and high fracture toughness is provided.
- an analogous high density PCBN material is provided.
- a mass of diamond particles or grains is provided.
- a layer of very thin bonding material is deposited on respective diamond particles or grains using a suitable method such as sol-gel deposition.
- the bonding materials are carbon allotropes such as graphite, graphene or diamond-like carbon, for example, and to achieve heteroepitaxy the bonding materials are carbide-forming elements such as silicon or suitable metals or alloys, for example.
- the starting mass is sintered at elevated temperature and pressure conditions as needed for the sintered diamond to be more thermodynamically stable than graphite. Typically, sintering takes place at a pressure in excess of about 5 GPa and a temperature in excess of about 1400°C.
- suitable conditions from low pressure (for instance about 2.5 GPa) to about 10 GPa or more (even up to 25 GPa) and modest temperature (for instance about 450°C) to about 2400°C or more in the diamond-stable region can be used to convert the nano-sized carbon allotrope to diamond or to cause reaction of the diamond grains with the carbide-former to form inter-granular bonded layers of from a few to about 100 atoms thick.
- the pressure conditions are from about 8 GPa to about 10 GPa or, in other embodiments about 8GPa to about 18GPa.
- Excellent bonding in the sintered mass may be achieved by means of very thin bonded layers of bonding material that form between the diamond particles or grains, these inter-granular layers ranging from a few atoms to tens of atoms in thickness.
- the resultant material may be highly thermally- stable and tough.
- reaction bonding as defined above, may result in a reduction in pressure requirement compared with direct diamond to diamond conversion which would have significant implications for commercialisation as cost increases very rapidly and achievable product size decreases significantly as the pressure requirement is increased.
- the very thin layers of bonding material may be arranged on the diamond grains using methods such as, but not limited to, sol-gel, physical vapour deposition, chemical vapour deposition, atomic layer deposition, liquid-phase epitaxy, solid-phase epitaxy, molecular-beam epitaxy or magnetron sputtering.
- the layers may partially or completely cover the diamond grains.
- the average size of the starting diamond particles or grains may range from about 50 nm to about 50 microns.
- the average thickness of the starting graphitic, other carbon or carbide-forming very thin bonding material layers may range from, for example, about 0.5 nm to about 200 nm.
- the carbon binder source may be graphite, or glassy carbon, or graphene, or any type of fullerene, or diamond-like carbon.
- the carbide forming bonding elements may be chosen from, for example, Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, B, Al, Ga, C, Si and Ge.
- the bonding material may be silicon or silicon carbide.
- Combinations of two or more of the carbon binder sources or two or more of the carbide-forming elements or two or more of the carbides may be used.
- the purity of the starting materials is selected to assist in the production of PCD with very small flaw sizes thereby not only improving strength but leading to the option of transparent PCD material.
- the average thickness of the newly grown inter- granular bonded layers may vary from less than 1 nm, typically from about 0.3 nm, to less than about 100 nm, or less than about 20 nm, or less than about 10 nm, or less than about 5 nm.
- the bonded layer material may be diamond, or a carbide constrained by neighbouring diamond grains to have a crystal structure closer to that of diamond than to that of the free carbide, and small amounts of the carbide-forming elements or alloys may be present.
- a low degree of misorientation between the diamond grain and the newly formed layer is expected due to the layer being very thin, i.e. a misfit angle of less than approximately 1 1 degrees is expected.
- the carbides have higher coefficient of thermal expansion than diamond, so the diamond grains in the final product should be under compressive stress, hence the carbide neck should be in tension favouring intergranular crack propagation. This should act as a toughening mechanism. Toughness is further enhanced by the nanosized nature of the bonded inter- layer material. Greater fracture toughness will assist in the manufacture of higher precision cutting tools that display less edge chipping of the tool, giving a cleaner and more accurate cut and more impact resistance. Improved thermal stability is expected in all cases enabling increased cutting speeds and longer lifetime in drilling applications.
- the superhard material is cBN powder used to synthesise PCBN.
- the bonding material may be a boride and/or nitride former in the case of heteroepitaxy or it may be hBN in the case of homoepitaxy.
- the superhard starting material is cBN powder
- very thin bonding material layers of nitride and/or boride formers are arranged on the primary cBN crystals.
- the bonding materials may be chosen from Be, Mg, Ca, Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, B, Al, Ga, In, C, Si, Ge, Sn, Pb, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb or compounds / alloys of these.
- the very thin bonding material layer may be hBN arranged on the cBN primary crystals and directly converted to PCBN under appropriate pressure and temperature conditions.
- carbide, nitride, boride and carbonitride binder compounds that can be used in some embodiments are TiC, TiB 2 , TiC x Ni -x and TiN.
- Preferred reaction-bonded compounds in the PCD or PCBN very thin bonded layer region may include but are not limited to: SiC, S13N4, TiC, TiN, TaC, TaN, TiC x N 1 -x , TaC x N 1-x , WC, WN 2 , NbC, Nb 2 C, and TiB 2 . It is also noted that compounds may be formed on the diamond or cBN particle or grain surfaces before sintering. This is because reactions may occur during the arrangement of the bonding material due to the elevated temperatures used in some of these processes.
- a method for making polycrystalline superhard material comprises providing a mass of diamond or cubic boron nitride particles or grains, depositing ultrathin layers of a bonding material on respective diamond or cubic boron nitride particles or grains, the bonding material being selected so as to be capable of forming bonds with the diamond or cubic boron nitride particles or grains, and the average thickness of the deposited layers of bonding material being greater than about 0.5 nm and less than about 200 nm.
- the diamond or cubic boron nitride particles or grains and bonding material are consolidated into a green body, which green body is then subjected to a temperature and pressure at which the diamond or cubic boron nitride is more thermodynamically stable than graphite or hBN, respectively, in order to sinter it and form polycrystalline diamond or cubic boron nitride material.
- the diamond or cubic boron nitride particles Prior to deposition of the bonding material, may have, for example, an average particle size ranging from about 50 nanometres to about 50 microns.
- the green body, once formed is placed in a suitable container and introduced into a high pressure high temperature press.
- Pressure and heat are applied in order to sinter the diamond particles together, typically at pressures of 2.5 GPa or more, or of 5 GPa or more, or of 6.8 GPa or more, or of 7.7 Gpa or more, and up to about 10 GPa, and temperatures of 450°C or more, or 1500°C or more, or 2250°C or more, or 2400°C or more, but in some embodiments the pressures may be up to around 25GPa.
- Non-limiting examples of polycrystalline superhard materials will now be described.
- 10 g of crushed diamond of average particle size 0.75 micron may be cleaned by placing in a furnace and heating at 800 degrees centigrade for 1 hour in 10% hydrogen in an argon atmosphere.
- the diamond powder may then be transferred into a plasma reactor of the type typically used to deposit diamond-like carbon (DLC), and the diamond particles may be coated with a coating (not entirely uniform, but covering most of the surface of the diamond particles) of DLC of approximately 35 nm thickness.
- the coated diamond particles may be transferred to a capsule and subjected to approximately 8 GPa and 2000 degrees centigrade for approximately 30 seconds at dwell time.
- the sintered compact may be recovered from the capsule and high resolution scanning electron microscopy of a polished section is expected to show diamond grains connected by layers of diamond of approximately 4-12 nanometres thick. HRTEM analysis of the composite is expected to confirm that the layers have a diamond crystal structure.
- the diamond content of the sintered compact is expected to be close to 100% by volume.
- 20 g of diamond of average particle size 2 microns may be cleaned by placing in a furnace and heating at 800 degrees centigrade for 1 hour in 10% hydrogen in an argon atmosphere.
- the diamond may then be transferred to a radio frequency plasma-enhanced chemical vapour deposition (rf PECVD) reactor and subjected to standard conditions for silicon thin film deposition: the deposition temperature would typically be 200 degrees centigrade, and silane (SiH 4 ) and hydrogen (H 2 ) gases would be fed into the reactor to maintain a SiH 4 partial pressure of 0.9 Torr and a [H 2 ]:[SiH 4 ] ratio of 80.
- rf PECVD radio frequency plasma-enhanced chemical vapour deposition
- the rf power flux would be set at 70 mW/cm 2
- the gases would be purged from the reactor with argon, the reactor cooled and the diamond recovered.
- 2 g of the diamond, now coated with a silicon layer of approximately 50 nanometres thick may then be placed in a capsule in a glove box under argon atmosphere to prevent oxidation of the silicon layer.
- the capsule may be pressed in a high-pressure high- temperature press at 8 GPa and 1800 degrees centigrade for approximately 15 seconds dwell time at condition.
- the sintered compact may be recovered from the capsule and high resolution scanning electron microscopy of a polished section is expected to show diamond grains connected by layers of silicon carbide of approximately 4-15 nanometres thick. Analysis of the composite using X-ray diffraction and the Scherrer calculation is expected to indicate the silicon carbide layer consisting of crystallites of approximately 4- 15 nanometres.
- the diamond content of the sintered compact is expected to be approximately 99 % by volume.
- crushed cubic boron nitride (cBN) of average particle size 0.50 micron may be transferred into a chemical vapour deposition reactor that may be fed with a gas mixture containing BCl3-NH 3 -H 2 -Ar, at flow rates of approximately BCI3 : 0.2 ml/sec; NH 3 : 1 .0 ml/sec; H 2 : 0.5 ml/sec; Ar: 2 ml/sec.
- An opaque and semi-crystalline film of boron nitride is expected to form on the cBN particles after a dwell time of approximately 5 minutes at 950-1050 degrees centigrade.
- the coating is expected to be approximately 45 nm thick.
- the coated cBN particles may be transferred to a capsule and subjected to approximately 6 GPa and 1800-2100 degrees centigrade for approximately 30 seconds at dwell time.
- the sintered compact may be recovered from the capsule and high resolution scanning electron microscopy of a polished section is expected to show cBN grains connected by layers of cBN of approximately 4-12 nanometres thick. HRTEM analysis of the composite is expected to indicate that the layers have a cBN crystal structure.
- the cBN content of the sintered compact is expected to be approximately 95 % by volume.
- cBN crushed cubic boron nitride
- 50 g of crushed cubic boron nitride (cBN) of average particle size 0.1 -0.3 micron may be transferred into an atomic layer deposition reactor and coated with titanium metal using 10-30 cycles of approximately 3 seconds long each to achieve a 3-10 nanometre thick coating of titanium metal on the cBN particles.
- the coated cBN particles may be transferred to a capsule and subjected to approximately 6 GPa and 1800-2100 degrees centigrade for approximately 30 seconds at dwell time.
- the sintered compact may be recovered from the capsule and high resolution scanning electron microscopy of a polished section is expected to show cBN grains connected by layers of titanium boride and titanium nitride of approximately 2-3 nanometres thick.
- the cBN content of the sintered compact is expected to be approximately 95 % by volume.
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Abstract
L'invention concerne un matériau super-dur polycristallin comprenant une masse de particules ou de grains de diamant, de graphite ou de nitrure de bore cubique lié(e)s ensemble par des couches de liaison inter-granulaires ultraminces, les couches de liaison inter-granulaires présentant une épaisseur moyenne supérieure à environ 0,3 nm et inférieure à environ 100 nm. Le présent document divulgue également un procédé pour la fabrication d'un tel matériau super-dur polycristallin.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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US13/997,781 US20130337248A1 (en) | 2010-12-29 | 2011-12-20 | High density polycrystalline superhard material |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201061428054P | 2010-12-29 | 2010-12-29 | |
GBGB1022033.3A GB201022033D0 (en) | 2010-12-29 | 2010-12-29 | High density polycrystalline superhard material |
US61/428,054 | 2010-12-29 | ||
GB1022033.3 | 2010-12-29 |
Publications (1)
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WO2012089565A1 true WO2012089565A1 (fr) | 2012-07-05 |
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Family Applications (1)
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PCT/EP2011/073463 WO2012089565A1 (fr) | 2010-12-29 | 2011-12-20 | Matériau super-dur polycristallin de haute densité |
Country Status (3)
Country | Link |
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US (1) | US20130337248A1 (fr) |
GB (2) | GB201022033D0 (fr) |
WO (1) | WO2012089565A1 (fr) |
Cited By (1)
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WO2013085979A1 (fr) * | 2011-12-05 | 2013-06-13 | Diamond Innovations, Inc. | Outil de découpe à base de nitrure de bord cubique fritté |
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CN102639268B (zh) * | 2010-09-07 | 2015-05-27 | 住友电工硬质合金株式会社 | 切削工具 |
US9382602B2 (en) * | 2011-09-01 | 2016-07-05 | Smith International, Inc. | High content PCBN compact including W-RE binder |
GB201412073D0 (en) * | 2014-07-07 | 2014-08-20 | Element Six Abrasives Sa | Super hard constructions & methods of making same |
GB201423405D0 (en) * | 2014-12-31 | 2015-02-11 | Element Six Abrasives Sa | Superhard construction & methods of making same |
GB201423409D0 (en) * | 2014-12-31 | 2015-02-11 | Element Six Abrasives Sa | Superhard constructions & methods of making same |
US10167675B2 (en) * | 2015-05-08 | 2019-01-01 | Diamond Innovations, Inc. | Polycrystalline diamond cutting elements having lead or lead alloy additions |
RU2611633C2 (ru) * | 2015-06-29 | 2017-02-28 | Открытое акционерное общество "Научно-исследовательский институт природных, синтетических алмазов и инструмента" - ОАО "ВНИИАЛМАЗ" | Способ изготовления алмазного инструмента |
RU2625693C2 (ru) * | 2015-06-29 | 2017-07-18 | Открытое акционерное общество "Научно-исследовательский институт природных, синтетических алмазов и инструмента" - ОАО "ВНИИАЛМАЗ" | Способ получения поликристаллических алмазных материалов |
US20170066110A1 (en) * | 2015-09-08 | 2017-03-09 | Baker Hughes Incorporated | Polycrystalline diamond, methods of forming same, cutting elements, and earth-boring tools |
CN105525345B (zh) * | 2016-02-18 | 2018-06-26 | 长春阿尔玛斯科技有限公司 | 金刚石多晶体合成超硬材料及其生产工艺 |
GB201622467D0 (en) * | 2016-12-31 | 2017-02-15 | Element Six Ltd | A method of making a polycrystalline super hard constructions |
CN108675813A (zh) * | 2018-07-07 | 2018-10-19 | 郑州万创智造科技有限公司 | 一种高强度聚晶立方氮化硼及其制造方法 |
CN109175388B (zh) * | 2018-10-31 | 2021-08-31 | 泉州市华兴超硬工具有限公司 | 一种金刚石锯片及其制备方法 |
CN112391547B (zh) * | 2019-08-14 | 2022-07-08 | 中南大学 | 一种聚晶材料的制备方法 |
US11767268B2 (en) * | 2019-12-16 | 2023-09-26 | Sumitomo Electric Industries, Ltd. | Cubic boron nitride sintered material |
CN111270120B (zh) * | 2020-03-25 | 2021-12-14 | 西安工程大学 | 一种切割石料用金刚石颗粒增强复合刀具材料的制备方法 |
CN112608153B (zh) * | 2020-12-10 | 2022-12-09 | 富耐克超硬材料股份有限公司 | 高导热高强度散热基板及其制备方法 |
CN112759395B (zh) * | 2021-01-22 | 2022-04-12 | 湖北天瓷电子材料有限公司 | 一种高q值微波介质陶瓷粉料的制备方法 |
CN113999009B (zh) * | 2021-12-29 | 2022-03-15 | 湖南大学 | 一种铌酸铋钙基压电陶瓷及其制备方法和应用 |
CN114573349B (zh) * | 2022-04-07 | 2023-06-27 | 南方科技大学 | 一种聚晶金刚石及其制备方法和用途 |
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- 2011-12-20 US US13/997,781 patent/US20130337248A1/en not_active Abandoned
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Also Published As
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GB2486973A (en) | 2012-07-04 |
US20130337248A1 (en) | 2013-12-19 |
GB201022033D0 (en) | 2011-02-02 |
GB2486973B (en) | 2015-07-08 |
GB201121905D0 (en) | 2012-02-01 |
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