CN103237776A - Polycrystalline diamond material containing nitrogen compound or halide - Google Patents
Polycrystalline diamond material containing nitrogen compound or halide Download PDFInfo
- Publication number
- CN103237776A CN103237776A CN2011800585024A CN201180058502A CN103237776A CN 103237776 A CN103237776 A CN 103237776A CN 2011800585024 A CN2011800585024 A CN 2011800585024A CN 201180058502 A CN201180058502 A CN 201180058502A CN 103237776 A CN103237776 A CN 103237776A
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- Prior art keywords
- chloride
- polycrystalline diamond
- diamond material
- adamantine
- diamond
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- 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
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- C23F1/02—Local etching
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Abstract
A polycrystalline diamond material comprising a mass of diamond particles or grains exhibiting inter-granular bonding and a binder material comprises a non-metallic catalyst material for diamond, the non-metallic catalyst material for diamond comprising at least one nitrogen compound derived from an ammonium compound and/or at least one halide.
Description
Technical field
The disclosure relates to the method for polycrystalline diamond (PCD) material and this material of preparation.
Background technology
The cutting insert that is used for lathe and other instrument can comprise polycrystalline diamond (PCD) layer that is bonded to sintered carbide (cemented carbide) base material.PCD is superhard material a kind of example of (being called super hard abrasive again), and it has significantly the hardness value greater than cemented tungsten carbide.
What the parts that comprise PCD were used in numerous types is used for cutting, machining, boring or broken hard or high-abrasive material for example rock, metal, pottery, matrix material and contain the instrument of the material of timber.PCD comprises the diamond crystals of a large amount of intergrowth basically (inter-grown) that forms skeletal substance, and it defines the gap in diamond crystals.The PCD material comprises at least about the diamond of 80 volume % and can stand by a large amount of diamond crystalses that will assemble in the presence of sintering aid (being called again for adamantine catalyst substance) to make greater than the ultra-high voltage of about 5GPa with at least about 1200 ℃ temperature.Be used for adamantine catalyst substance be understood to be to promote diamond crystals diamond than graphite the direct material of intergrowth under the more thermodynamically stable pressure and temperature condition.Some are used for adamantine catalyst substance may be under environmental stress, particularly promote diamond to the conversion of graphite at elevated temperatures.The example that is used for adamantine catalyst substance is cobalt, iron, nickel and some any alloy that comprises these.Can form PCD at the wolfram varbide base material of cobalt sintering, described base material can be provided for the source of the cobalt catalyst material of PCD.Gap in the PCD material can be filled with described catalyst substance at least in part.
Yet the known problem that such PCD material runs into is described for adamantine catalyst substance, in the residual existence in described gap PCD material performance is at high temperature produced harmful effect especially for adamantine metallic catalyst material, for example Co, Ni or Fe.During using, the heating of described PCD material and thermal destruction, this major part is owing to catalytic gold hard rock greying and also cause the existence of the described Metal catalyst materials of the stress in the PCD material, and this stress is because due to the huge difference of the thermal expansion between described Metal catalyst materials and the described diamond microstructure.
A kind of method that addresses this problem is typically to remove catalyst substance (being called catalyst/solvent in this area again) by leaching (leaching) from the PCD material.
US3,745,623 and US4,636,253 have instructed the acid mixture that uses through heating in leaching technology, wherein use HF, HCl and HNO respectively
3And HNO
3Mixture with HF.
US4,288,248 and US4,224,380 have described by comprising HNO
3-HF(nitric acid and hydrofluoric acid) thermal medium in leach the PCD table top and remove described catalyst/solvent, the aforementioned hot medium use separately or with comprise HCl-HNO
3Second thermal medium of (hydrochloric acid and nitric acid) is used in combination.
US2007/0169419 has described a kind of method of leaching part or all catalyst/solvent in the following way from the PCD table top: protect a part of PCD table top not leached and protected PCD table top is immersed the caustic soln so that described catalyst/solvent is dissolved in water and the chloroazotic acid.The described technology of leaching is accelerated by using ultrasonic energy, and this ultrasonic energy stirring interface between described PCD table top and described caustic soln is to accelerate the dissolution rate of described catalyst/solvent.
US4,572,722 disclose a kind of by before leaching technology or during be transmitted in by laser cutting or spark and form the technology of leaching that the hole obtains accelerating in the PCD table top.Then, by use conventional acidleach drop technology, electrolysis is leached extracts to leach described PCD table top with liquid zinc.
A replacement method that addresses this problem is to use for adamantine nonmetal character catalyst substance, and it produces more heat-staple PCD material.
JP2795738 (B2) has described at the mixture of the sintering temperature diamond powder of the pressure of 6-12GPa and 1700-2500 ℃ and metal carbonate and has produced the sintered polycrystalline material of being made up of the nonmetal character binding agent of the 0.1-15vol% that is positioned at the sintered diamond layer.
JP4114966 has described to use and has been added into the carbon dust of diamond powder and alkaline earth metal carbonate as sintering aid, thereby improves the sinterability of described nonmetal character system.
JP2003226578 has also solved the sinterability problem of difference, and it has been described and has used oxalic acid dihydrate as sintering aid in the nonmetal character solvent system of carbonate based.
JP2002187775 has described and has added other organic compound with the carbonate based nonmetal character PCD of acquisition sintering, and has described the interpolation of metallic carbide similarly in JP6009271.
Summary of the invention
Usually, the disclosure relates to and comprises the polycrystalline diamond material that has for adamantine nonmetal character catalyst substance.
From first aspect; provide to comprise a large amount of diamond particles or the crystal grain that demonstrates the intergranular keying action and the polycrystalline diamond material that contains the adhesive substance may that is useful on adamantine nonmetal character catalyst substance, be used for adamantine nonmetal character catalyst substance and comprise at least a nitrogen compound and/or at least a halogenide that is derived from ammonium compound.
Described ammonium compound can contain negatively charged ion, and this negatively charged ion is selected from carbonate, phosphate radical, hydroxide radical, oxide compound negatively charged ion, sulfate radical, borate, titanate radical, silicate, halogen ion and their combination.
Described halogenide can contain the positively charged ion that is selected from basic metal, alkaline-earth metal, transition metal, ammonium and their combination.
In some embodiments, describedly can comprise following one or more for adamantine nonmetal character catalyst substance: lithium chloride, sodium-chlor, Repone K, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, bariumchloride, Yttrium trichloride, zirconium chloride, zinc chloride, niobium chloride, their all oxidation state and their mixture.
In some embodiments, the average particle size particle size of described diamond particles or crystal grain can be for about 5 nanometers to about 50 microns or about 20 nanometers to about 20 microns or about 50 nanometers to about 10 microns.
In some embodiments, the diamond content of described polycrystalline diamond material can for the volume of described polycrystalline diamond material at least about 80%, at least about 88%, at least about 90%, at least about 92% or even at least about 96%.In one or more embodiments, the diamond content of described polycrystalline diamond material can be at the most about 98% of the volume of described polycrystalline diamond material.
The content that is used for adamantine nonmetal character catalyst substance can for example be about 20 volume % at the most of described PCD material, about 10 volume %, about 8 volume % or even about 4 volume % at the most at the most at the most.
From another point of view; method for the preparation of polycrystalline diamond material is provided; described method comprises: a large amount of diamond particles or crystal grain are provided; with described diamond crystals or particle with contain the adhesive substance may that is useful on adamantine nonmetal character catalyst substance and contact; describedly comprise at least a ammonium compound and/or at least a halogenide for adamantine nonmetal character catalyst substance; make described diamond particles or crystal grain and adhesive substance may be combined together to form green compact; be thermodynamically stable temperature and pressure with making described green compact stand at diamond, sintering and form polycrystalline diamond material.
In some embodiments, described salt can merge with described diamond particles or crystal grain via diafiltration, mixing, grinding, chemical vapour deposition, colloid (sol-gel) deposition, ald, physical vapor deposition etc.
In some embodiments, can adopt suitable adhesive aid to mix described diamond particles or crystal grain and described adhesive substance may with powder type.
Can be so that described diamond particles or crystal grain be suspended in the liquid medium, described for adamantine nonmetal character catalyst substance in-situ precipitate to the surface of the corresponding diamond particles of this liquid medium or crystal grain to apply described diamond particles or crystal grain.
In some embodiments, with described diamond particles before described adhesive substance may contacts or crystal grain can have about 5 nanometers to about 50 microns or about 20 nanometers to about 20 microns or about 50 nanometers to about 10 microns average grain or grain-size.
In some embodiments, can provide diamond particles with different average grains or grain-size or the multimodal mixture of crystal grain.
Described polycrystalline diamond material can be that unsupported (stand-alone) composite sheet maybe can be attached to for example metal carbide substrate of base material.
Sintering can carry out under 4GPa or higher or 7GPa or higher pressure and 1000 ℃ or higher or 1700 ℃ or higher temperature, and sintering time is 10 minutes or longer, or sintering time is 30 seconds or longer or 1 minute or longer.
In some embodiments, sintering can carry out under 7GPa or lower pressure and 1800 ℃ or lower temperature.
According on the other hand, provide the anti-wear component that comprises aforesaid polycrystalline diamond material.
Described polycrystalline diamond material can obtain by one or more embodiments with respect to thermostability and ratio lower sintering temperature and pressure with regard to other is used for adamantine nonmetal character catalyst substance of raising for the glomerocryst material of common metal catalysis.
Embodiment
As used herein, " polycrystalline diamond " (PCD) material comprises a large amount of diamond crystalses, wherein significantly the diamond crystals of ratio directly mutually combine each other and wherein adamantine content be described material at least about 80 volume %.In an embodiment of PCD material, the gap between the described diamond crystals can be contained the adhesive substance may that is useful on adamantine nonmetal character catalyzer at least in part and be filled.
As used herein, " be used for adamantine nonmetal character catalyst substance " be can catalysis polycrystalline diamond particle or crystal grain diamond than graphite the material of intergrowth under the more thermodynamically stable temperature and pressure condition.
As used herein, " gap " or " interstitial area " is the zone between the diamond crystals of described PCD material.
The multimodal particle size distribution of great number of grains is understood to mean described crystal grain and has particle size distribution more than a peak value, and each peak value is corresponding to separately " state ".Typically by provide more than a kind of source of a plurality of crystal grain and will make from crystal grain or the particle blend in these sources together, each described source comprises the crystal grain with significantly different mean sizess to the multimodal aggregate.The measurement of the particle size distribution of described blend crystal grain has typically disclosed the different peak values corresponding to different states.When described crystal grain was sintered together with the formation aggregate, their particle size distribution was further changed, because described crystal grain is compressed together each other and is broken, caused whole decline of size of described crystal grain.Howsoever, the multimodality of described crystal grain usually also from the image analysis of the goods of sintering clearly as seen.
As used herein, but green compact are to be sintered or to have been partially sintered the goods that do not formed the finished product as yet by tight burning.It generally can be self-supporting and can have the general shape of the goods that will finish.
As used herein, the superhard wear element is to comprise the element of superhard material and will be used to wear applications that for example fragmentation, boring, cutting or machining comprise in the workpiece or object of hard or high-abrasive material.
Comprise the diamond that for the diamond composite of the solvent sintering of routine, has the thermostability of raising according to the polycrystalline diamond material of some embodiments.In some embodiments, described polycrystalline diamond material comprises and contains the binding agent that is useful on adamantine nonmetal character catalyst substance.Be used for adamantine nonmetal character catalyst substance and comprise at least a nitrogen compound and/or at least a halogen contained compound that is derived from ammonium compound.
In some embodiments, for the preparation of the method for polycrystalline diamond material comprise with a large amount of diamond particles or crystal grain with contain the adhesive substance may that is useful on adamantine nonmetal character catalyst substance and contact.Being used for adamantine nonmetal character catalyst substance is at least a ammonium compound and/or at least a halogenide.
Described salt can merge with diamond by for example following mode: diafiltration, mix, other similar technology that grinding, chemical vapour deposition, colloid (sol-gel) deposition, ald, physical vapor deposition and those skilled in the art will expect.
Described nonmetal character adhesive substance may can merge with described diamond particles or the crystal grain of powder type.It typically for example can be mixed in the presence of the methyl alcohol at grinding aid in conventional hybrid technique, for example planetary type ball-milling technology.Mill ball for example the Co-WC mill ball can be used to described binding agent and diamond powder are milled together.Then, can be typically under 50-100 ℃ temperature dry described binding agent and diamond matrix and be consolidated into the green compact of preparing to be used for sintering afterwards removing methyl alcohol and other volatile residue.
In an alternate embodiment, described nonmetal character adhesive substance may and described diamond particles or crystal grain can be merged in sol-gel technology.Under vigorous stirring, diamond powder floated on a liquid to form the diamond suspensoid.Described liquid typically is water, but those skilled in the art will recognize that and can use any suitable liquid medium.Can select first salt of required ammonium cation and/or halogen negatively charged ion to make it dissolve in the solvent, but form insolubility salt with the negatively charged ion of selecting/positively charged ion, depend on the circumstances, in described diamond suspensoid.Can select required negatively charged ion/cationic second salt so that it dissolves in the solvent, but described negatively charged ion/positively charged ion form insolubility salt with the ammonium cation of described first salt and/or halogen negatively charged ion respectively.
The solution that will contain described two kinds of salt dropwise joins together and makes in the described diamond suspensoid and form on the surface of diamond particles or crystal grain separately by being used for insolubility throw out that adamantine nonmetal character catalyst substance forms.
During dropwise adding, stir and contain the diamond particles of described suspension or the liquid of crystal grain.This stirring can be finished by well heater-agitator and magnetic stirring apparatus or by the cantilevered agitator or by ultrasonication or any other suitable method that can effectively described diamond particles be dispersed in the described liquid.
Can from suspensoid, remove the salt of diamond powder and precipitation and dry under the temperature that is fit to remove any residual suspension medium that may exist or solvent.Described drying temperature can typically be about 50-100 ℃, or the temperature that can not make the volatilization of described ammonium or halide compound.As an alternative, can be in a vacuum under moderate temperature or room temperature dry diamond with salt of precipitation.Described diamond with salt of precipitation can maybe can be that the mode that improves drying efficiency or speed is stirred, disturbance or mobile during drying for static.Described diamond particles and adhesive substance may is fixed to form green compact.
With before described adhesive substance may contacts, described diamond particles can have about 5 nanometers to about 50 microns average particle size particle size.
In case form, be positioned over described green compact in the suitable containers and introduce high pressure and the high temperature press in.Exert pressure with heat so that described diamond particles sintering is in the same place, typically under about 4-7GPa or higher pressure and about 1000-1700 ℃ or higher temperature.
In some embodiments, the crystal boundary of described diamond particles or crystal grain can contain the pollutent of the residue that is derived from initial salt of the level of reduction, therefore makes stronger diamond-diamond combination and the material character of improvement become possibility.In the situation of ammonium cation, the pollutent of expection low concentration, this is to form hydrogen and nitrogen because described ammonium cation will dissociate under sintering condition, they are used as gas and discharge.
In some embodiments, the PCD of sintering can contain nitrogen or the hydrogen of a certain amount of dissolving.The expection of the hydrogen that discharges during the HPHT has such beneficial effect: help that carbon monoxide or carbonic acid gas intermediate are reduced into diamond and make thus and use lower pressure and temperature to become possibility.
In other embodiments, for example wherein use halid those, also can use lower pressure and temperature to come sintering PCD.For example, with the more conventional 8GPa that is used for more conventional nonmetal character catalyst system or higher and 2300 ℃ or higher opposite, can use 7GPa or lower and 1800 ℃ or lower pressure and temperature.Although do not wish to be subjected to theory constraint, it is believed that destroying the C-O key by chlorion has reduced the become temperature of catalytic activity of salt of wormwood.
For example use therein in some embodiments of the compound contain ammonium cation, described negatively charged ion can be in following one or more: carbonate, phosphate radical, hydroxide radical, oxide compound negatively charged ion, sulfate radical, borate, titanate radical, silicate, halogen ion etc.
For example use therein in some embodiments of the compound contain the halogen ion, described positively charged ion can be in following one or more: basic metal, alkaline-earth metal and transition metal.Described examples for compounds can comprise lithium chloride, sodium-chlor, Repone K, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, bariumchloride, Yttrium trichloride, zirconium chloride, zinc chloride, niobium chloride, their all oxidation state and their mixture.
In some embodiments, can use the mixture of ammonium compound and halide compound.
Diamond grain size in the PCD of sintering can be for about 5 nanometers to about 50 microns or about 20 nanometers to about 20 microns or about 50 nanometers to about 10 microns.Adamantine distribution of sizes can be for unimodal or multimodal.
Described nonmetal character PCD can maybe can be attached to for example Co-WC base material of suitable substrates for all-in-one-piece.Interface between described PCD and the described base material can be smooth or non-flat forms.
Any suitable the leaching process portion or all leach described nonmetal character PCD that can use those skilled in the art to understand.
Embodiment
Describe some embodiments in more detail with reference to following embodiment, these embodiments are not intended to the restriction effect of playing.
Embodiment 1:
With CaCO
3And Ca (OH)
2Approximate eutectic mixture and NH
4Cl is with 0.4mol CaCO
3With 0.4mol Ca (OH)
2With 0.2mol NH
4The mixed of Cl.With this binder mixtures and diamond with the 4.5g diamond: the mixed of 0.5g binder mixtures.The mixture of this merging is pressed in the airtight metal vessel that is suitable for the HPHT processing densely.Then this container being stood HPHT handles to being higher than 1500 ℃ temperature and being higher than the pressure of 6.8GPa and keeping time of 10 minutes to 60 minutes.Be expected at HPHT and handle the diamond compact that will have intergrowth afterwards.
Embodiment 2:
With MgCO
3And Mg (OH)
2Wait molar mixture (under situation about not existing for the phasor of the obtained document of this system, supposing etc. that molar mixture will be fully near eutectic composition) and NH
4Cl is with 0.4mol MgCO
3With 0.4mol Mg (OH)
2With 0.2mol NH
4The mixed of Cl.With this binder mixtures and diamond with the 4.5g diamond: the mixed of 0.5g binder mixtures.The mixture of this merging is pressed in the airtight metal vessel that is suitable for the HPHT processing densely.Then this container being stood HPHT handles to 1500 ℃ temperature and is higher than the pressure of 6.8GPa and keeps time of 10 minutes to 60 minutes.Be expected at HPHT and handle the diamond compact that will have intergrowth afterwards.
Embodiment 3
With CaCO
3And Ca (OH)
2Approximate eutectic mixture and NH
4Cl is with 0.4mol CaCO
3With 0.4mol Ca (OH)
2With 0.2mol NH
4The mixed of Cl.With this binder mixtures and diamond with the 9g diamond: the mixed of 1g binder mixtures.The mixture of this merging is pressed in the airtight metal vessel that is suitable for the HPHT processing densely.Then this container being stood HPHT handles to following temperature: the pressure of 1600 ℃, 1800 ℃ and 2000 ℃ and 8GPa also keeps time of 10 minutes.Be expected at HPHT and handle the diamond compact that under all these conditions, will have intergrowth afterwards.
Embodiment 4:
With MgCO
3With ammonium oxalate wait molar mixture as binding agent and diamond with the 4.5g diamond: the mixed of 0.5g binder mixtures.The mixture of this merging is pressed in the airtight metal vessel that is suitable for the HPHT processing densely.Then this container being stood HPHT handles to being higher than 1500 ℃ temperature and being higher than the pressure of 6.8GPa and keeping time of 10 minutes to 60 minutes.Be expected at HPHT and handle the diamond compact that will have intergrowth afterwards.
Embodiment 5:
With ammonium oxalate as binding agent and diamond with the 4.5g diamond: the mixed of 0.5g binder mixtures.The mixture of this merging is pressed in the sealed metal container that is suitable for the HPHT processing densely.Then this container being stood HPHT handles to being higher than 1500 ℃ temperature and being higher than the pressure of 6.8GPa and keeping time of 10 minutes to 60 minutes.Be expected at HPHT and handle the diamond compact that will have intergrowth afterwards.
Embodiment 6:
With K
2CO
3Descended dry 24 hours at 50 ℃ with KCl, carried out planetary type ball-milling respectively 45 minutes with 90rpm then, the mol ratio with 70:30 merges then.The diamond powder that with this mixture and average particle size particle size is 10 microns merges with the adamantine amount of 5vol% mixture: 95vol%.Owing to be very moisture absorption, therefore dry described salt mixture and ought being stored in the vacuum drying oven in case of necessity between step.Run into the practical difficulty that pressure produces, therefore in experiment, do not realized sintering.Yet, being expected at greater than 1000 ℃ and will causing sintering greater than sintering under the 7GPa greater than 5 minutes, 1260 ℃, 7.7GPa and expection in 1 hour produce the nonmetal character PCD of the good sintering with extraordinary thermostability and wear resisting property.These temperature usually are low for sintering PCD, and this advantage is considered to because due to the existence of chlorion, described chlorion can be so that their conducts of carbonate anion instability and increase be used for the reactivity of adamantine catalyst substance.
Claims (15)
1. polycrystalline diamond material; it comprises a large amount of diamond particles or the crystal grain that shows the intergranular combination and contains the adhesive substance may that is useful on adamantine nonmetal character catalyst substance, is used for adamantine nonmetal character catalyst substance and comprises at least a nitrogen compound and/or at least a halogenide that is derived from ammonium compound.
2. according to the polycrystalline diamond material of claim 1, wherein said ammonium compound comprises the negatively charged ion that is selected from carbonate, phosphate radical, hydroxide radical, oxide compound negatively charged ion, sulfate radical, borate, titanate radical, silicate, halogen ion and their combination.
3. according to the polycrystalline diamond material of claim 1, wherein said halogenide comprises the positively charged ion that is selected from basic metal, alkaline-earth metal, transition metal, ammonium and their combination.
4. according to the polycrystalline diamond material of claim 3, wherein saidly comprise following one or more for adamantine nonmetal character catalyst substance: lithium chloride, sodium-chlor, Repone K, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, bariumchloride, Yttrium trichloride, zirconium chloride, zinc chloride, niobium chloride, their oxidation state and their mixture.
5. according to the polycrystalline diamond material of aforementioned each claim, wherein said diamond particles or crystal grain have about 5 nanometers to about 50 microns average grain or grain-size.
6. according to the polycrystalline diamond material of aforementioned each claim, the diamond content of wherein said polycrystalline diamond material be described polycrystalline diamond material volume at least 80% and at the most 98%.
7. according to the polycrystalline diamond material of aforementioned each claim, wherein said polycrystalline diamond material comprises the adamantine nonmetal character catalyst substance that is used for of 20 volume % at the most.
8. method for preparing polycrystalline diamond material; this method comprises: a large amount of diamond particles or crystal grain are provided; with described diamond crystals or particle with contain the adhesive substance may that is useful on adamantine nonmetal character catalyst substance and contact; be used for adamantine nonmetal character catalyst substance and comprise at least a ammonium compound and/or at least a halogenide; make described diamond particles or crystal grain and adhesive substance may fixed to form green compact; be thermodynamically stable temperature and pressure with making described green compact stand at diamond, sintering and form polycrystalline diamond material.
9. method according to Claim 8, wherein said ammonium compound comprises the negatively charged ion that is selected from carbonate, phosphate radical, hydroxide radical, oxide compound negatively charged ion, sulfate radical, borate, titanate radical, silicate, halogen ion and their combination.
10. method according to Claim 8, wherein said halogenide comprises the positively charged ion that is selected from basic metal, alkaline-earth metal, transition metal, ammonium and their combination.
11. according to the method for claim 10, wherein be used for adamantine nonmetal character catalyst substance and comprise following one or more: lithium chloride, sodium-chlor, Repone K, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, bariumchloride, Yttrium trichloride, zirconium chloride, zinc chloride, niobium chloride, their all oxidation state and/or their mixture.
12. each method according to Claim 8-11, wherein said method are included under the existence of described nonmetal character catalyst substance described green compact are stood at diamond than the more thermodynamically stable pressure and temperature of graphite.
13. according to the method for claim 12, wherein said pressure is at least about 4GPa and described temperature is at least about 1000 ℃.
14. according to the method for claim 12, wherein said pressure is for about 8GPa and described temperature are about 2300 ℃ at the most at the most.
15. comprise the anti-wear component of each polycrystalline diamond material among the claim 1-7.
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US40572610P | 2010-10-22 | 2010-10-22 | |
US61/405,726 | 2010-10-22 | ||
GBGB1017924.0A GB201017924D0 (en) | 2010-10-22 | 2010-10-22 | Polycrystalline diamond material |
GB1017924.0 | 2010-10-22 | ||
PCT/EP2011/068305 WO2012052500A2 (en) | 2010-10-22 | 2011-10-20 | Polycrystalline diamond material |
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JP (1) | JP2013543830A (en) |
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CN105731449A (en) * | 2016-01-21 | 2016-07-06 | 湖南大学 | Preparation method of porous foamed diamond |
CN112756604A (en) * | 2020-12-22 | 2021-05-07 | 吉林大学 | Sintered polycrystalline diamond compact under mantle-like condition and preparation method thereof |
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JP6301689B2 (en) * | 2014-03-19 | 2018-03-28 | 国立大学法人福井大学 | Diamond composite particles and method for producing the same |
CN104690274B (en) * | 2014-12-31 | 2017-11-17 | 中石化石油机械股份有限公司 | A kind of polycrystal diamond hard alloy complex sheet and preparation method thereof |
CN106747445B (en) * | 2016-12-06 | 2019-08-27 | 富耐克超硬材料股份有限公司 | A kind of high-performance composite polycrystal-diamond |
KR20220084081A (en) * | 2019-10-04 | 2022-06-21 | 도메이 다이아 가부시키가이샤 | Diamond grit that can be crushed easily and its manufacturing method |
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Also Published As
Publication number | Publication date |
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WO2012052500A3 (en) | 2012-08-30 |
GB201118025D0 (en) | 2011-11-30 |
WO2012052500A2 (en) | 2012-04-26 |
JP2013543830A (en) | 2013-12-09 |
GB201017924D0 (en) | 2010-12-01 |
US20130326963A1 (en) | 2013-12-12 |
GB2484814A (en) | 2012-04-25 |
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