CN101263083A - Sintered polycrystalline diamond material with extremely fine microstructures - Google Patents
Sintered polycrystalline diamond material with extremely fine microstructures Download PDFInfo
- Publication number
- CN101263083A CN101263083A CNA200680033795XA CN200680033795A CN101263083A CN 101263083 A CN101263083 A CN 101263083A CN A200680033795X A CNA200680033795X A CN A200680033795XA CN 200680033795 A CN200680033795 A CN 200680033795A CN 101263083 A CN101263083 A CN 101263083A
- Authority
- CN
- China
- Prior art keywords
- diamond
- pcd
- particle size
- metal
- size
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 120
- 239000010432 diamond Substances 0.000 title claims abstract description 120
- 239000000463 material Substances 0.000 title abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 53
- 239000002184 metal Substances 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims description 73
- 239000000203 mixture Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000010941 cobalt Substances 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 238000012935 Averaging Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000005245 sintering Methods 0.000 abstract description 27
- 238000012545 processing Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 150000004767 nitrides Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 3
- 229910001573 adamantine Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- SKYGTJFKXUWZMD-UHFFFAOYSA-N ac1l2n4h Chemical compound [Co].[Co] SKYGTJFKXUWZMD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Images
Landscapes
- Cutting Tools, Boring Holders, And Turrets (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A sintered polycrystalline diamond material (PCD) of extremely fine grain size is manufactured by sintering a diamond powder with pre-blended catalyst metal under high pressure/high temperature (HP/HT) processing. The PCD material has an average sintered diamond grain structure of less than 1.0 mum.
Description
The cross reference of related application: the application requires to submit on September 15th, 2005, title is " Sintered; Polycrystalline Diamond Compact with Extremely Fine Microstructure (the polycrystalline diamond briquetting with extremely fine microstructures) ", the U.S. Provisional Application No.60/717 of pending trial together, 227 right of priority, above-mentioned application is included in herein by reference fully.
Statement about federal funding research: inapplicable.
The title of the each side of joint study agreement: inapplicable.
Sequence table: inapplicable.
Background
1. technical field
Disclosed embodiment generally relates to the field of sintered diamond cutting and forming tool, and more specifically, relate to such diamond tool with superfine (extremely fine) microstructure (microstructure), be that described extremely fine microstructures is given improved tool performance, workability, and the ability of giving improved surface smoothness (surfacefinish) for workpiece material.
2. description of Related Art
Polycrystalline diamond (PCD) is widely used in comprising in the industrial application of metal cutting, wire drawing, drilling, and is used as wear parts.As herein defined, PCD is a kind of two-phase polycrystalline diamond product, and wherein diamond crystal is sintered to together to form the successive diamond lattice.This lattice, i.e. principal phase (majority phase) comprises diamond between particle-to-diamond in conjunction with (bond), and does not have between two parties non-diamond in conjunction with phase.A large amount of remainder catalyst metals, promptly second phase (minor phase) can be set in the space between the diamond crystal.
The PCD production method is at first open the sixties in 20th century, and has a detailed description in patent documentation.U.S. Patent No. 3,831,428, No.4,063,909, No.5,488,268 have described and have produced high pressure/high temperature (HP/HT) method that parting tool, wortle and ground auger with wear-resistant grinding abrasion and anti-chemical abrasion creep into cutter, and above-mentioned patent is incorporated herein by reference.Because PCD presents (uniform) mechanical property more consistent than single crystal diamond, and can obtain the size bigger than single crystal diamond, so PCD provides and has been better than natural or the adamantine substantive design advantage of synthetic single crystal.Yet the current PCD that produces does not provide cutting, the drawing of dead smooth or the workpiece surface that otherwise forms.Although the single crystal diamond is expensive, have anisotropy and size-constrained, still is the preferred kit material that is used for the single-point turning of optical material or has the drawing of great surface quality filament.Come from limited intensity and shock resistance and the mechanical fault of the PCD instrument that causes also is general.
(" sintered state (as-sintered) ") had the part (parts) of 1 μ m to the bortz size (grain size) of 100 μ m after obtainable PCD assembly (component) was included in the HP/HT sintering.Verified, thinner, consistent sintered state bortz size, for example about 0.1 μ m has proposed challenge to about 1.0 μ m (being called as " submicron ") to using PCD manufacturing process described above to carry out commercial production.The diamond particles of submicron (particle) is difficult to produce, and it is verified, because the high surface area (surface area) of the diamond particles of submicron attracts and retain the ability (described pollutant effect sintering process and product performance) of pollutent, the diamond particles of described submicron is difficult to handle between blend and mixing period.
The submicron diamond particles has low packing density (packing density), and this causes problem during loading shield cap (shieldingenclosure) and HP/HT processing.Be difficult to as one man infiltrate the very thin hole that is between initial diamond particles material (mass) Central Asia micron diamond grain, cause incomplete combination and sintering between the diamond particles with catalyst metal.The high surface area of almost often observing the submicron diamond powder causes diamond solution redeposition process to take place in incomparable inconsistent mode.This causes the growth of deleterious nonuniformity bortz, and makes infeasible other complicated factors of production of big parts when attempting final bortz size less than 1 micron.
The trial of production submicron monoblock type (monolithic) PCD now is the conforming product of output with any essence not also, no matter be, free-standing main body (body) whole, still (ii) attach to the PCD (being called as (supported) PCD that is with supporter) of substrate as (i).Use here, PCD refers to by successive diamond body (matrix), diamond-to-diamond combination, has or do not have catalyst metal and the sintering PCD body that constitutes.In general, PCD is a kind of two phase materials (diamond and catalyzer), and does not comprise the third phase (for example carbide of associativity, nitride or boride) between the bortz of occuping of any significant quantity.
At least the non-PCD diamond product that comprises some submicron bortzs is known.U.S. Patent No. 4,505,746 disclose use 3 μ m and submicron diamond particles, catalyst metal, and extra carbide, carbonitride, nitride and boride make more tough and tensile wear-resistant sintered diamond briquetting body mutually, and this patent is incorporated herein by reference.The U.S. Patent No. 4,303,422 of authorizing people such as Hara has been described the method that sintering is used for the diamond of parting tool or silk mould, and wherein adamantine particle size is less than 1 μ m, and this patent is incorporated herein by reference.People such as Hara have discussed the sub-micrometer grain structure high dimensional accuracy on the workpiece and the advantage aspect the fabulous surface smoothness are being provided.For people such as Hara, in order to produce useful sintered diamond tool, must add the 3rd combination phase and iron group catalyst metal to the submicron diamond particles, the described the 3rd in conjunction with carbide, nitride and the boride of planting IVB, VB, group vib metal (being called international pure and the 4th family of applied chemistry federation (IUPAC), the 5th family and the 6th family's element respectively in addition) mutually for one or more.In addition, people such as Hara has instructed the difficulty that generates submicron PCD.People's such as Hara embodiment 1 is presented to have during the HP/HT sintering and is less than the grain growth that the 5% submicron diamond powder experience one in conjunction with additive surpasses 300 μ m.These incomparable inconsistent materials are not enough firmly to be used as parting tool.None has described the generation of submicron PCD diamond body patent listed above.Two kinds of sintered products have all comprised except that the diamond of real PCD and the third phase the catalyzer.
U.S. Patent No. 6,319,460 have described the sintered diamond tool with improved overall flexibility, and described improved overall flexibility is to realize by the particle size that reduces diamond particles, and this patent is incorporated herein by reference.In this case, diamond particles is surrounded by the successive metallic matrix; Do not form the combination of intergranular diamond.This product is not PCD, but has the mixture of the bortz that is not narrower than 1 μ m.The resistance to abrasion of this product, intensity and thermostability will substantially be worse than real PCD.
The U.S. Patent Application Publication 2005/0019114 that Sung submitted has been described the generation of nanocrystalline (nanocrystalline) diamond, those nanocrystalline diamond materials have the particle size less than 0.1 μ m, and this patent application is incorporated herein by reference.This application has been instructed the nanocrystalline diamond of sintering costliness, especially gets rid of submicron (0.1 μ m is to 1 μ m) diamond particles and gets rid of the replaceable method of using liquid metal catalyst.Owing to do not exist catalyst metal, this application not to describe real PCD product; This product will have significant defective, and owing to the intrinsic problem of handling fine powder is difficult to produce.
Prior art fails to reach the particle size of submicron.U.S. Patent No. 5,855,996 and No.5,468,268 have described the influence of the particle size distribution (PSD) of PCD briquetting to its performance characteristics, and above-mentioned patent is incorporated herein by reference.In this case, as a kind of mode that increases diamond concentration in the sintering PCD product, submicron particles is used as the part of diamond particles material.15 volume percent are maximum submicron diamond shares possible in the prior art.U.S. Patent No. 5,855, the Photomicrograph in 996 shows the submicron diamond that in fact exists far fewer than 15 volume percent.
Exist produce have consistence, sintered state, the bortz size is less than the needs of the monoblock type PCD material of 1 μ m.Shockingly, the applicant has been found that several advantages that realize submicron PCD and need not add extra in conjunction with mutually or need not be by means of the method for the nanocrystalline diamond of costliness.
The disclosure that is comprised has been described the trial that solves one or more the problems referred to above herein.
Summary of the invention
In exemplary, glomerocryst (PCD) body comprises the diamond crystal that has less than the arithmetical mean sintered state bortz size of 1 μ m.In another embodiment, described PCD body comprises greater than about 0.1 μ m and less than the particle size of about 1.0 μ m.In another embodiment again, the sintered state particle size of PCD body is consistent basically.In other embodiments, described PCD body is all-in-one-piece; In described PCD body, do not exist interpolation in conjunction with phase, for example carbide, nitride or boride.The embodiment of PCD body can have the oxygen level that is lower than about 0.05 weight percent.In another embodiment again of PCD body, nitrogen content is lower than about 0.01 weight percent.Here the PCD body of being implemented can comprise diamond crystal, and wherein at least 63% described crystal has the particle size less than 1.0 μ m.Another embodiment is the PCD body with the average sintered state particle size between about 0.1 μ m and about 1.0 μ m, and the body thickness that has is greater than about 0.5mm.
One embodiment comprises a kind of method have less than polycrystalline diamond (PCD) body of the average sintered state particle size of 1.0 μ m that generates by following steps: begin with the diamond particles with volume averaging (volumetric mean) particle size less than about 1.0 μ m; To have catalyst metal and described diamond particles blend, to form the diamond powder blend less than the average particle size particle size of described bortz size; And causing between the adjacent bortz on the intergranular bonded time being enough to, adopt pressure and temperature to handle described diamond powder blend.In the embodiment of this method, described catalyst metal can be the iron family metal.In another embodiment again, described metal catalyst can be a cobalt.Described metal catalyst can be described diamond powder blend about 0.5% to about 15% weight.One embodiment uses metal catalyst as nanocrystal, and other embodiments comprise the metal catalyst nanocrystal that is attached to described diamond particles.Described processing pressure can be between about 20 kilobars and 70 kilobars.Described treatment temp can be at least about 1000 ℃, and the described treatment time is between about 3 minutes to about 120 minutes.In the embodiment of described method, described processing also comprises the cemented metal carbide supporter is included in described diamond powder blend.Other embodiments are used cyclic metal sintering carbide supported body, and wherein said bortz powder art blend is set in the described support ring.
Another embodiment comprises polycrystalline diamond (PCD) wear-resistant components again, described assembly for example, but be not limited to, machinery tools, wear-resistant pad (wear pad), press tool or mould, described assembly comprises the PCD body, and described PCD body has at about 0.1 μ m to the average sintered state bortz size between about 1.0 μ m.In another embodiment of described instrument, described PCD body is all-in-one-piece.In another embodiment again of described instrument, described PCD body is incorporated into substrate, and described substrate can be a cemented metal carbide, and described cemented metal carbide (cementedmetal carbide) is such as but not limited to cemented tungsten carbide (cemented tungsten carbide).
Description of drawings
Fig. 1 is scanning electronic microscope (" the SEM ") image of exemplary cobalt-diamond powder blend.
Fig. 2 describes to make the technology of the PCD body with average submicron sintered state particle size.
Fig. 3 is a SEM image that uses the embodiment of 0.8 μ m diamond powder.
Fig. 4 is a SEM image that uses the embodiment of 0.5 μ m diamond powder.
Fig. 5 is the SEM image of the product of prior art.
Embodiment
Before describing present method, system and material, should be appreciated that the disclosure is not limited to described ad hoc approach, system and material, because they can change.Be also to be understood that employed term only is used to describe specific version or embodiment in this description, and do not plan limited field.For example, as here with appended claims in employed, unless otherwise clearly indication of context, otherwise singulative " " (" a ", " an ") and " described " (" the ") comprise plural reference.In addition, word " HP/HT " refers to the material processing at high pressure (promptly between 25 kilobars and 75 kilobars or higher) and high temperature (promptly about 1000 ℃ or higher).Unless otherwise definition, otherwise employed here all technology and scientific and technical terminology all have the generally identical connotation of understanding of those of ordinary skills institute.
In embodiments, body is to be made by the submicron polycrystalline diamond (" PCD ") (being the catalytic sintered diamond product of liquid metal) with sintered state arithmetical mean (promptly average) the bortz size that is lower than 1 μ m and is higher than 0.1 μ m.Average sintering particle size is to use division lines method (line intercept method) definite.This method is based on the particle size determined of intersecting by the line drawn at random on the microstructure photo, and is familiar with to those skilled in the art.
Use has the diamond powder of the catalystic material (for example cobalt) of blend in advance, and a method embodiment can generate the high quality P CD with the average sintered state particle size from 0.1 μ m to 1.0 μ m.In another embodiment, in the PCD body, there is not wedding agent such as carbide, nitride or boride.Therefore, PCD body described herein only comprises diamond and catalyzer basically.As indicated in this area, existing P CD technology can not generate the sintered state monoblock type PCD with the particle size that is lower than 1.0 μ m with the amount (substantial amount) of essence.
The diamond powder blend:The raw material diamond particles can be natural or HP/HT synthetic (preferred amorphous/nano crystal " impact (shock) " diamond) single crystal particle, or the glomerocryst polymer with the sub-micron particle size between about 0.1 μ m and about 1.0 μ m.The starting material diamond particle size is the volume averaging particle size of measuring by such as grain size analysis instrument or any other suitable analyser of MacxKerodt thunder gram (Microtrac).In one embodiment, the average-volume particle size of diamond particles is 0.8 μ m.In another embodiment, this average-volume particle size is 0.5 μ m.In the 3rd embodiment, effectively sintering have a particle of 0.3 μ m average-volume particle size.This diamond powder blend also comprises the catalyst metal that one or more plant blend in advance, for example cobalt or other iron family metals.Preferably, this metal catalyst is a pure metal, perhaps only has small amount of impurities and is essentially pure.Specifically, described catalyzer is the form of the nano-crystalline granule that directly is attached to diamond particles, described nano-crystalline granule by those of ordinary skills present or known from now on any method make.In some embodiments, metal catalyst can have the average particle size particle size littler than described bortz.
Fig. 1 illustrates the scanning electron microscopy of the powder raw material 100 that can be used for an embodiment.In Fig. 1, the cobalt granule 120 that the diamond particles 110 of 0.8 μ m average-volume size has 100 nanometers (nm) mean sizes is attached to their surface.Can also use other iron family metals.In one embodiment, in raw material blend, comprise 5% to catalyst metal until 10% weight.Described catalyzer can be present in the blend with the amount that changes.In some embodiments, catalyzer can account for blend from about 1% to about 10% weight.In other embodiments, catalyzer can account for blend from about 0.5% to about 15% weight.In other embodiments, catalyzer can account for blend from about 5% to about 7% weight.
The technology that the submicron PCD body of band supporter is made in Fig. 2 A and 2B representative.Fig. 2 A refers to the system before HP/HT processing 200.Fig. 2 B refers to the submicron PCD body 250 of the band supporter of handling through HP/HT.In the embodiment of Fig. 2 A, diamond powder blend 210 (above-described diamond particles is together with metal catalyst) and cemented metal carbide supporter 220 can be set in the protective guard 230.The diamond particles 210 of blend and metallic carbide supporter 220 can be in single HP/HT process sintering simultaneously.In embodiments, metallic carbide supporter 220 only and with the layers of diamond particles reaction at 240 places, interface of metallic carbide supporter, be attached to supporter with PCD body with gained.The product 250 that generates is the sintering PCD bodies 260 that are attached to metallic carbide supporter 220.This PCD body 260 comprises diamond-to-diamond combination.Product 250 is moved out of from protective guard 230 subsequently.Should be appreciated that method as described herein can be used to make monoblock type (promptly not with supporter) structure.Under these circumstances, can use the method shown in Fig. 2 A and the 2B in the mode that need not supporter 220.
Selected HP/HT treatment condition are enough to provide the combination of the intergranular between the adjacent bortz, and the joint of sintered diamond particles to the cemented metal carbide supporter (joining) is provided alternatively.In one embodiment, described treatment condition generally comprise the pressure about 3 minutes to about 120 minutes of the temperature that imposes at least 1000 ℃ and at least 20 kilobars (Kbar).In another embodiment, can use about 50 and about 70 kilobars between pressure, and the temperature between about 1400 ℃ and about 1600 ℃.Other temperature and pressures are possible.Pressure, temperature and process lasting time are selected as making the bortz growth during the sintering to minimize, and can be that those skilled in the art are present or known from now on.Temperature and pressure described herein is an approximation.
In another embodiment again, diamond and catalyzer can be with HP/HT technology sintering under the situation that does not have the metallic carbide supporter.Can use follow-up HP/HT or soldering processes to come attached cemented metal carbide supporter.
In another embodiment again, described metallic carbide supporter can be a ring, and can be set in the described support ring with the material (diamond powder blend) of catalyzer diamond particles together.These can be sintered in HP/HT technology under the situation of adding or not adding extra catalyst metal together.
Here the disclosure that is comprised relates in machining and for example has improved intensity and flexible sintering PCD when non-ferrous metal, pottery and wood composite.In addition, this openly relates in the workability such as the raising during the manufacturing of the wear-resistant components of PCD machinery tools, wear-resistant pad, press tool or mould.At last, this openly relates to these instruments provide the surface smoothness of raising on the workpiece that for example comprises aluminium casting or steel wire ability.As described herein instrument can for example comprise all-in-one-piece sintering PCD, (for example a kind of cemented metal carbide that is attached to substrate, as cemented tungsten carbide or other materials) sintering PCD layer, and the sintering PCD within cemented metal carbide (for example cemented tungsten carbide, perhaps other are used in the stringy material) ring.
In a word, in the PCD commercial production, it is general making the product that reclaims from the reaction chamber of HP/HT device or base stand various precision work (finishing) operation, so that any covering metal that adheres to is removed from the outside surface of briquetting (compact), described finishing operations comprises the cutting of for example processing (electrode discharge machining) or carrying out with laser apparatus by electrode discharge, milling is especially milled.Extraly, can adopt these to operate briquetting is processed into the shape that satisfies about the product specification of diamond layer thickness and/or carbide supported body thickness.
In the PCD body that generates, can be by the average sintered state bortz size that division lines method records less than one micron.This size can also be greater than 0.1 μ m.In each embodiment, the averageparticle size can be less than 0.9 μ m, 0.8 μ m, 0.7 μ m, 0.6 μ m or 0.5 μ m.Described PCD body can be consistent basically.These can comprise 50%, 63%, 7%, 90%, 98% and 100% the bortz less than 1 μ m based on the embodiment that symmetrical normal state particle size distributes.Other embodiments can have other scopes.Described body can also have low oxygen level, for example is lower than 0.05%, is lower than 0.01% or the oxygen level between the Equipment Inspection limit and arbitrary above-mentioned numerical value.Here the PCD body that is comprised can have about 0.5 millimeter (mm) to about 1mm, up to about 1.5mm, greater than 1mm, up to about 2mm, perhaps the thickness of other sizes (being that upper surface arrives substrate interface).
Use here, the body intention with " consistent " particle size or " consistent basically " particle size comprises averageparticle size wherein less than 1 micron body, and meaning promptly surpasses 50% particle and is lower than 1 μ m behind sintering.
In addition, during manufacture, can use cobalt or other catalyst metal of various amounts.In some embodiments, some or all of catalyst metal can be retained in the finished product.Some or all of therein catalyst metal can be retained in the interior embodiment of material, and described catalyst metal is not to exist mutually as wedding agent.Described metal catalyst does not form chemical bond with diamond carbon, and only exists as amounts of residual contamination do.
EmbodimentHere embodiment is provided to illustrate each embodiment, and does not plan to limit the scope of the invention.
Embodiment 1Referring again to Fig. 2 A and 2B, this embodiment demonstrates the ability of making such PCD mixture, and in described PCD mixture, sintered diamond is integrally coupled to the cemented metal carbide substrate.Having the diamond of 7% weight cobalt-cobalt dust blend roughly is set between the dish of cobalt of tantalum (Ta) shield cap 230 and cemented tungsten carbide (WC)+13% weight, described blend distributes as shown in Figure 1, has roughly 0.8 μ m volume averaging raw material diamond size 210.Make this subassembly (assembly) stand HP/HT and handled about 20 minutes, to form submicron sintering PCD tool blank 260 in the about 1400 ℃ temperature of about 55 kilobars.Generating the thick diamond layer 260 of 1.5mm, and the total thickness of this base 250 is 3.2mm to this PCD tool blank 250 by precision work.Measure by the direct transversal that this microstructure carried out with field emission scanning electron microscope and to be evaluated, this average sintered state bortz is of a size of 0.87 μ m.Use different initial diamond powder size, diamond bed thickness and cobalt blending amount to carry out several variants of this process.These variants are summed up in table 1.
The average sintered state particle size and the body thickness of table 1 submicron PCD embodiment described herein.
| Averageparticle size (μ m) | The amount of cobalt in the powder blend (% weight) | The mean thickness of PCD body (millimeter) |
| 0.5 | 7 | 0.5 |
| 0.4 | 7 | 0.5 |
| 0.25 | 7 | 0.5 |
| 0.8 | 1 | 0.5 |
| 0.8 | 2 | 0.5 |
| 0.8 | 5 | 0.5 |
| 0.8 | 7 | 0.5 |
| 0.8 | 7 | 1.0 |
| 0.8 | 7 | 1.5 |
| 0.8 | 7 | 2 |
| 0.8 | 10 | 1.5 |
Sintering PCD body among the embodiment 1 that used following technical Analysis: scanning electronic microscope (SEM), oxygen and nitrogen determination.As a comparison, also analyzed the PCD body made from prior art and commercially available material.Table 2 highlights more viewed differences.
Table 2 has the cobalt blend and does not have the sample comparison of cobalt blend.
| Analytical technology | New PCD material | Prior art |
| LECO-nitrogen | 0.009％ | 0.0165％ |
| LECO-oxygen | 0.046％ | 0.087％ |
Table 2 illustrates, and compares with prior art PCD material, and the PCD material of the embodiment here has low nitrogen and oxygen concn.Embodiment described herein can have the nitrogen content that is lower than about 0.01% (w/w).Embodiment described herein can have the nitrogen content that is lower than about 0.05% (w/w).
SEM image among Fig. 3 illustrates the sub-micrometer grain size of PCD body embodiment that use as described herein has the diamond powder preparation of 0.8 μ m volume averaging size.Fig. 4 illustrates the sub-micrometer grain size of PCD body embodiment that use as described herein has the diamond powder preparation of 0.5 μ m volume averaging size.Fig. 5 illustrates the particle size of commercially available product Sumitomo Grade DA2200 (Sumitomo DA2200 level) PCD body.
Table 3 illustrates the observed value of the sintered diamond microstructure of using three kinds of identical among division lines method pair and Fig. 5-7 materials.This method is based on the particle size determined of intersecting by the line drawn at random on the microstructure photo.
The particle size that table 3 uses division lines method to record compares (size is in micron)
| Product | Averageparticle size (μ m) | Standard deviation |
| 0.8 the initial powder of μ m | 0.87 | 0.41 |
| 0.5 the initial powder of μ m | 0.88 | 0.24 |
| Sumitomo DA2200 | 1.46 | 0.79 |
These assessments show that new PCD material as described herein has lower oxygen and nitrogen content, have much thin particle size, and reach the averageparticle size that is lower than 1 μ m, and it is much thin that this particle size can obtain product than the thinnest commerce.
Embodiment 2With reference to Fig. 8, this embodiment illustrates the ability of silk mould (wire die) base 800 of making band carbide supporter.These are such materials, and promptly wherein diamond part 810 is sintered in the carbide ring 820, and described sintering operation is to use independent source metal as catalyzer rather than use the cobalt binder from the carbide substrate to carry out sintering mutually.In this embodiment, used the diamond powder 810 that has 0.5 μ m volume averaging particle size, also comprises the thin dispersive cobalt (being similar to embodiment 1) of 7% weight.The powder blend 810 of diamond and cobalt has been loaded onto the center of carbide cylinder 820, and described carbide cylinder 820 is installed in tantalum (Ta) cover 830.Cobalt (Co) sheet 840 (illustrating with decomposition view) are placed in the powder top, and described powder is afterwards followed by Ta shield cap 850 (also illustrating with decomposition view).Several such subassemblies are loaded in the HP/HT reaction chamber, and the pressure that the temperature between about 1300 ℃ and about 1500 ℃ stands about 55 kilobars reaches 15 minutes to form sintering PCD silk mould.This PCD silk mould is recovered from reaction chamber and precision work, thereby the diameter of whole PCD sintering volume is about 7mm, the thick 6mm that is about.Comprise that the silk mould overall diameter that surrounds adamantine carbide ring is about 14mm.
Should be appreciated that top disclosed and other various features and function or during its alternative can be combined to a lot of other different systems and use by expectation.Should also be appreciated that those skilled in the art can make replacement, modification, variation or the improvement of various current not predictions or expection from now on, described replacement, modification, variation or improvement are also planned to be included in the appended claims.
Claims (21)
1. a polycrystalline diamond (PCD) body comprises the diamond crystal that has less than the arithmetical mean sintered state bortz size of 1 μ m.
2. PCD body as claimed in claim 1, wherein said particle size is greater than 0.1 μ m.
3. PCD body as claimed in claim 1, wherein said body has the oxygen level that is lower than about 0.05 weight percent.
4. PCD body as claimed in claim 1, wherein said body has the nitrogen content that is lower than about 0.01 weight percent.
5. polycrystalline diamond as claimed in claim 1 (PCD) body comprises diamond crystal, and wherein at least 63% described crystal has the particle size less than 1.0 μ m.
6. polycrystalline diamond as claimed in claim 1 (PCD) body, the thickness of wherein said sintered diamond body is greater than about 0.5mm.
7. PCD body as claimed in claim 1 also comprises the cemented metal carbide supporter.
8. a generation has the method less than poly-product diamond (PCD) body of the arithmetical mean sintered state bortz size of 1 μ m, comprising:
Provide and have less than about 1.0 μ m and greater than the diamond particles of the volume averaging particle size of about 0.1 μ m;
To have catalyst metal and described diamond particles blend, to form the diamond powder blend less than the average particle size particle size of described bortz size; And
Causing between the adjacent bortz on the intergranular bonded time being enough to, adopting pressure and temperature to handle described diamond powder blend.
9. method as claimed in claim 8, wherein said catalyst metal comprises the iron family metal.
10. method as claimed in claim 8, wherein said metal catalyst comprises cobalt.
11. method as claimed in claim 8, wherein said metal catalyst comprise described diamond powder blend about 0.5% to about 15% weight.
12. method as claimed in claim 8, wherein said metal catalyst comprises nano-crystalline granule.
13. method as claimed in claim 12, wherein said nano-crystalline granule directly is attached to described diamond particles.
14. method as claimed in claim 8, wherein said pressure are between about 20 kilobars and 70 kilobars, and wherein said temperature is at least about 1000 ℃, and the wherein said time is between about 3 minutes to about 120 minutes.
15. method as claimed in claim 8 also comprises with the cemented metal carbide supporter and handles described diamond powder blend.
16. method as claimed in claim 8, wherein said metallic carbide supporter comprises support ring, and described diamond powder blend is set in the described support ring.
17. a polycrystalline diamond (PCD) wear-resistant components comprises the PCD body, described PCD body comprises having the diamond crystal to the arithmetical mean sintered state bortz size between about 1.0 μ m at about 0.1 μ m.
18. assembly as claimed in claim 17, wherein said PCD body is all-in-one-piece.
19. assembly as claimed in claim 17, wherein said PCD body is incorporated into substrate.
20. assembly as claimed in claim 17, wherein said substrate comprises cemented metal carbide.
21. assembly as claimed in claim 17, wherein said cemented metal carbide comprises cemented tungsten carbide.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US71722705P | 2005-09-15 | 2005-09-15 | |
| US60/717,227 | 2005-09-15 | ||
| US11/531,389 | 2006-09-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101263083A true CN101263083A (en) | 2008-09-10 |
Family
ID=39962946
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200680033795XA Pending CN101263083A (en) | 2005-09-15 | 2006-09-14 | Sintered polycrystalline diamond material with extremely fine microstructures |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101263083A (en) |
| ZA (1) | ZA200802380B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103703208A (en) * | 2011-06-22 | 2014-04-02 | 贝克休斯公司 | Coated particles and related methods |
| CN104114722A (en) * | 2011-12-21 | 2014-10-22 | 六号元素磨料股份有限公司 | Methods of forming a superhard structure or body comprising a body of polycrystalline diamond containing material |
| CN104178653A (en) * | 2014-09-10 | 2014-12-03 | 刘秀珠 | Sintering method of polycrystalline diamond (PCD) material |
| CN105925863A (en) * | 2016-06-16 | 2016-09-07 | 河南黄河旋风股份有限公司 | Manufacturing method for polycrystalline diamond compacts applicable to wire cutting |
| CN106552555A (en) * | 2015-09-29 | 2017-04-05 | 六号元素(英国)有限公司 | Diamond crystalses with facet |
| US9670065B2 (en) | 2010-10-29 | 2017-06-06 | Baker Hughes Incorporated | Methods of forming graphene-coated diamond particles and polycrystalline compacts |
-
2006
- 2006-09-14 CN CNA200680033795XA patent/CN101263083A/en active Pending
-
2008
- 2008-03-13 ZA ZA200802380A patent/ZA200802380B/en unknown
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9670065B2 (en) | 2010-10-29 | 2017-06-06 | Baker Hughes Incorporated | Methods of forming graphene-coated diamond particles and polycrystalline compacts |
| US10538432B2 (en) | 2010-10-29 | 2020-01-21 | Baker Hughes, A Ge Company, Llc | Methods of forming graphene-coated diamond particles and polycrystalline compacts |
| CN103703208A (en) * | 2011-06-22 | 2014-04-02 | 贝克休斯公司 | Coated particles and related methods |
| CN103703208B (en) * | 2011-06-22 | 2016-10-26 | 贝克休斯公司 | The granule of coating and correlation technique |
| US9611699B2 (en) | 2011-06-22 | 2017-04-04 | Baker Hughes Incorporated | Coated particles and related methods |
| US10323463B2 (en) | 2011-06-22 | 2019-06-18 | Baker Hughes Incorporated | Methods of making diamond tables, cutting elements, and earth-boring tools |
| CN104114722A (en) * | 2011-12-21 | 2014-10-22 | 六号元素磨料股份有限公司 | Methods of forming a superhard structure or body comprising a body of polycrystalline diamond containing material |
| CN104178653A (en) * | 2014-09-10 | 2014-12-03 | 刘秀珠 | Sintering method of polycrystalline diamond (PCD) material |
| CN106552555A (en) * | 2015-09-29 | 2017-04-05 | 六号元素(英国)有限公司 | Diamond crystalses with facet |
| CN106552555B (en) * | 2015-09-29 | 2019-12-31 | 六号元素(英国)有限公司 | Faceted diamond grains |
| CN105925863A (en) * | 2016-06-16 | 2016-09-07 | 河南黄河旋风股份有限公司 | Manufacturing method for polycrystalline diamond compacts applicable to wire cutting |
Also Published As
| Publication number | Publication date |
|---|---|
| ZA200802380B (en) | 2009-01-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5289957B2 (en) | Sintered polycrystalline diamond material with ultrafine structure | |
| CN101228095B (en) | High-hardness polycrystalline diamond and process for producing the same | |
| US8404010B2 (en) | Abrasive compact with improved machinability | |
| JP5574566B2 (en) | Cubic boron nitride compact | |
| CN105916615B (en) | The manufacture method of diamond conjugant, the instrument comprising the diamond conjugant and the diamond conjugant | |
| US20110253459A1 (en) | Polycrystalline diamond composite compact element, tools incorporating same and method for making same | |
| CN101263083A (en) | Sintered polycrystalline diamond material with extremely fine microstructures | |
| EP3266756B1 (en) | Polycrystalline diamond body, cutting tool, wear-resistant tool, and grinding tool | |
| CN102459667A (en) | Composite cemented carbide rotary cutting tools and rotary cutting tool blanks | |
| JP5140606B2 (en) | Wire drawing dies | |
| CN110219042B (en) | Polycrystalline diamond body, cutting tool, wear-resistant tool, grinding tool, and method for manufacturing polycrystalline diamond body | |
| SE457537B (en) | DIAMOND PRESSURE BODY FOR A TOOL AND WAY TO MANUFACTURE IT | |
| CN101583450A (en) | Cutting tool | |
| KR100642841B1 (en) | Heat-resistant composite diamond sintered product and method for production thereof | |
| CN111233476A (en) | Binder-free polycrystalline diamond material and preparation method thereof | |
| US20140154509A1 (en) | Providing a catlyst free diamond layer on drilling cutters | |
| CN104837546A (en) | Providing a catalyst free diamond layer on drilling cutters | |
| JP6253140B2 (en) | Method for producing hexagonal tungsten nitride sintered body | |
| EP1033414A2 (en) | Corrosion resistant polycrystalline abrasive compacts | |
| JP5087776B2 (en) | Method for producing a composite diamond body | |
| SE442962B (en) | SINTRAD DIAMOND BODY AND PROCEDURE FOR ITS MANUFACTURING | |
| KR830001730B1 (en) | Manufacturing method of diamond sintered body | |
| Gorla | Impact resistance and energies of intermetallic bonded diamond composites and polycrystalline diamond compacts and their comparison | |
| JPS6011278A (en) | Manufacture of diamond sintered composite body | |
| EP0037714A1 (en) | High pressure, high temperature die assembly |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20080910 |