CN108941583A - A kind of sub-micron diamond compact and its preparation process - Google Patents

A kind of sub-micron diamond compact and its preparation process Download PDF

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CN108941583A
CN108941583A CN201810999120.5A CN201810999120A CN108941583A CN 108941583 A CN108941583 A CN 108941583A CN 201810999120 A CN201810999120 A CN 201810999120A CN 108941583 A CN108941583 A CN 108941583A
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powder
sub
cobalt
carbide
preparation process
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CN108941583B (en
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卢灿华
张涛
刘俊涛
窦明
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Zhongnan Diamond Co Ltd
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Zhongnan Diamond Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/02—Local etching
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/001—Starting from powder comprising reducible metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B22F3/101—Changing atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/28—Acidic compositions for etching iron group metals
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
    • C22C2026/006—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes with additional metal compounds being carbides
    • 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
    • C22C2026/007—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes with additional metal compounds being nitrides

Abstract

The invention discloses a kind of sub-micron diamond compact and its preparation process, preparation process include: 1) carbide matrix bottom surface take off cobalt；2) diadust purifies；3) polycrystalline diamond powder is prepared；4) complex component is prepared；5) composite sheet is prepared.The sub-micron diamond compact that the present invention is prepared can effectively prevent diamond crystals abnormal growth, it is hereby achieved that relatively fine, uniform tissue, to meet the requirement of finishing and microstoning.

Description

A kind of sub-micron diamond compact and its preparation process
Technical field
The invention belongs to technical field of superhard material, and in particular to a kind of sub-micron diamond compact and its preparation work Skill.
Background technique
Sub-micron diamond compact is by sub-micron diadust (0.1~1 μm) and hard alloy substrate in high pressure height Double-layer structure diamond compact made of being sintered under the conditions of temperature.Due to it have diamond grain size is small, even tissue with And wearability is good, while being widely used in having coloured gold with the feature that hard alloy shock resistance is strong and solderability is good again Belong to finishing and the microstoning field of material.
Currently, Sumitomo Electric Carbide company of the U.S. releases a kind of sub-micron (0.5 μm) for DA2200 The PCD trade mark, the PCD cutter of the trade mark it is processable go out high workpiece surface finish, and having almost can be with hard alloy The high intensity to match in excellence or beauty, the companies such as SUMITOMO CHEMICAL, element six are proposed 0.5 μm of sub-micro rice product below, improve the resistance to of cutter Mill property, toughness and processability.
Sub-micron diamond compact has excellent properties, however, since very small diamond particles have big table Area and volume ratio, when with iron family element, for example Co, Ni, Fe make bonding agent, since these metals are all the solvents of diamond, It include the process that diamond is dissolved and is precipitated in the solution in high pressure high temperature sintering process, if with less than 2 μm, especially Less than 1 μm Buddha's warrior attendant masonry raw material, then it is uneven to be easy diamond particles in long ambassador's diamond sinter for diamond particles.It is this Extremely the crystal grain poor quality grown up will cause and combine by force between the variation and diamond particles of polycrystalline diamond layer interior tissue The decrease of degree leads to performance depreciation, thus not can be used as finishing and the use of microstoning tool blank.
Summary of the invention
It is an object of the invention to propose a kind of preparation process of sub-micron diamond compact, the Asia of the technique preparation Micron diamond composite sheet can effectively prevent diamond crystals abnormal growth, it is hereby achieved that relatively fine, uniform tissue, To meet the requirement of finishing and microstoning.
To achieve the above object, the present invention prepares sub-micron diamond compact using following technique, comprising the following steps:
1) carbide matrix bottom surface takes off cobalt: using HNO3: H2O volume ratio be 1:(2.5~3) solution in etch carbide matrix 20~60 min of bottom upper surface, after be rinsed with water to neutrality, obtain surface take off cobalt cement carbide substrate.
2) diadust purifies: by diadust and sodium chloride 1:(2~3 in mass ratio) it mixes, after vacuum-sintering, It crosses 400 mesh screens and separates diadust with sodium chloride, then use 8~16h of boiling water rinses, until being mixed with diadust Deionized water conductivity value obtains the diadust that granularity is 0.5~1.0 μm less than 1 μ S/cm；Diadust granularity It is 0.5~1.0 μm, sodium chloride is 200~300 mesh.
3) it prepares polycrystalline diamond powder: being respectively that the purified diamond of 88~92% step 2 is micro- by weight percent Powder, 5~7% metallic bond and the mixing of 3~5% grain growth inhibitor, obtain powder mixture, in powder mixture Middle addition dehydrated alcohol, polyethylene glycol, sintered carbide ball mix 100~150h, obtain polycrystalline diamond powder；
4) it prepares complex component: cement carbide substrate being taken off into cobalt surface and is contacted with polycrystalline diamond, vacuum-sintering, being passed through has After the mixed gas reaction of reproducibility, then it is evacuated to air pressure 3 × 10-3Pa is hereinafter, obtain complex component.
5) it prepares composite sheet: the complex component that step 4) obtains being placed in synthesis assembling block inner cavity, synthesis is assembled Block is sintered to arrive the composite sheet of sub-micron diamond in cubic hinge press.
The design parameter of vacuum-sintering in step 2 are as follows: be evacuated to air pressure 3 × 10-3Pa hereinafter, temperature rise to 700~ 800 DEG C of 1~2h of heat preservation.
Metallic bond is composed of the following weight percentages of raw materials in step 3): cobalt powder 98.5~99%, tungsten powder 0.3~ 0.5%, 0.2~0.3 % of 0.2~0.3 % of rubidium powder, 0.3~0.4 % of cerium powder and antimony powder, the metallic bond partial size be 60~ 100nm。
Grain growth inhibitor is composed of the following weight percentages of raw materials in step 3): carborundum powder 73~84%, carbonization Tungsten powder 4~7%, titanium carbonitride powder 3.5~6%, zirconium cyanonitride powder 3~4%, 3~5 % of boron carbide powder, carbonized titanium powder 0.5~1%, nitrogen Change titanium valve 0.5~1%, carbonization vanadium powder 0.5~1%, carbonization 0.5~1 % of chromium powder and cubic boron nitride micro mist 0.5~1%, the crystalline substance Grain growth inhibitor partial size is 60~100nm.
Powder mixture, dehydrated alcohol, polyethylene glycol, sintered carbide ball are 1:(0.2~0.25 in step 3)): (0.02 ~0.05): the weight ratio mixing of (5~6)；Sintered carbide ball is by the sintered carbide ball that diameter is 8~φ of φ 10mm and diameter The sintered carbide ball of 3~φ of φ 5mm is mixed according to the weight ratio of 1:1, and the material trade mark of the sintered carbide ball is YG8.
The concrete mode that powder mixture, dehydrated alcohol, polyethylene glycol, sintered carbide ball mix in step 3) are as follows: use The mode wet ball mill of alternate-running counterclockwise clockwise, revolving speed is 60~80 r/min, revolving speed when counterclockwise when operating clockwise For 60~80 r/min, alternate-running, the alternating clockwise time is 5~10min, and alternately the time counterclockwise is 8~12min, is handed over It is 0.5~1 min for interval stand-by time.
The design parameter of step 4) mesocomplex component vacuum-sintering are as follows: be evacuated in furnace air pressure up to 8 × 10-2Pa with Under, 180~230 DEG C of 0.5~1h of heat preservation are heated to, then proceed to vacuumize while being heated to 750~800 DEG C, until furnace internal pressure is steady It is scheduled on 3 × 10-3Pa or less is evacuated to air pressure 3 × 10 in furnace again-3Then Pa is hereinafter, stop vacuumizing in 750~800 DEG C of items Be filled under part into vacuum furnace mixed gas that air pressure in furnace is 60~80Mbar to complex component reduction treatment 3~ 4h, then it is evacuated to air pressure 3 × 10 in furnace-3Pa is hereinafter, the hydrogen and 60 that the mixed gas is 35~40% by percent by volume ~65% carbon dioxide composition.
Sintering process is specific as follows in step 5): after being passed through 900-1500A electric current when pressure rises to 2~3GPa, boosting To 5~6GPa, 1400~1500 DEG C are warming up to, after keeping 5~10min, with the rate of temperature fall of 90~120 DEG C/min by cavity Temperature is down to 750~850 DEG C, and cavity temperature is then down to room temperature with the rate of temperature fall of 10~15 DEG C/min again, while with Chamber pressure is down to normal pressure by the rate of pressure reduction of 0.085~0.095GPa/min.
The sub-micron diamond compact that above-mentioned preparation process obtains, including cement carbide substrate and be compounded in hard conjunction The polycrystalline diamond layer of gold substrate upper surface, cement carbide substrate upper surface take off cobalt layers with a thickness of 50~100 μm, and de- cobalt layers cobalt contains Amount is 1~1.2%.
The invention has the advantages that:
1) de- cobalt purification is carried out to the surface that cement carbide substrate is contacted with polycrystalline diamond in the present invention, reduces carbide matrix Bottom and diamond layer interface metal phase cobalt content make the reduction of Metals in Environments phase locating for diamond near interface, prevent gold The nucleation of hard rock abnormal grain growth takes off cobalt purification through hard alloy and closes to reduce the possibility of interface abnormal grain growth At diamond compact, do not occur the crystal of abnormal grain growth, explanation on the interface between hard alloy and diamond layer Hard alloy, which takes off cobalt purification, certain inhibiting effect to the abnormal grain growth at the interface between hard alloy and diamond layer.
2) present invention is by silicon carbide, tungsten carbide, titanium carbonitride, zirconium cyanonitride, boron carbide, titanium carbide, titanium nitride, carbonization Vanadium, chromium carbide and cubic boron nitride composition crystal grain inhibit growth stimulator, and when sintering can make metal in diamond and metallic bond Liquid phase is reduced, and growing up for diamond particles can be controlled.These metallic compounds and cubic boron nitride are in metallic bond gold Belong to and being partly dissolved in liquid phase, is then precipitated and is deposited to diamond crystal surface, to inhibit the abnormal growth of diamond particles. The diamond compact that crystal grain inhibits growth stimulator is added, polycrystalline diamond even tissue is fine and close, and average particle size is less than or equal to 0.75 μ There is not diamond anomaly and grows up phenomenon in m.
3) present invention uses the purification method of diadust vacuum high-temperature together with sodium chloride, obtains diamond surface Fully purify；Wet type method for mixing is ground by using pellet, and is added to a small amount of polyethylene glycol and initial diamond is mixed Material carries out pre-treatment, according to dimond synneusis layer raw material composition and the thinner feature of granularity, by ball mill mixing machine parameter tune It is whole, it determines optimised process range, further increases compounding effect, keep metallic bond, grain growth inhibitor and diamond micro- Powder is sufficiently mixed and disperses.The secondary granule of Gold Samples hard rock of the micro mist synthesis handled in this way significantly reduces, metal Phase is evenly distributed, and considerably reduces abnormal grain growth condition.Obtain the uniformity consistency of diamond compact product Further improve.
4) present invention uses hydrogen and carbon dioxide gas mixture reduction diadust and metal under high vacuum state The anisotropic atom of bonding agent, diamond surface and adhesive surface absorption is pumped out, and purification has activated its surface, it is easy to make it Chemical action occurs, improve the performances such as wearability and the thermal stability of the diamond compact.It restores micro- according to diamond The reduction characteristic of the granularity of powder thinner feature and metal bonding agent material, has selected optimised process range.
5) composite sheet sintering of the present invention avoids abnormal grain growth existing by the way of " the primary primary heating of boosting " As occurring, while stress when in order to reduce cooling and release after composite sheet sintering, use the slow decompression annealing process side of slow cooling Case has the effect of stress relief annealing, substantially reduces the thermal residual strain of submicron polycrystalline diamond compact, improves multiple Close piece service life.
6) performance indicator of the sub-micron diamond compact obtained by: dimond synneusis average grain size is less than or equal to 0.75μm；Wear resistance ratio 32~340,000；Thermal stability: after 700 DEG C roast 2 minutes, wear resistance ratio 30~320,000 meet finishing The requirement of work and microstoning.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but the following example is only used for The bright present invention, without that should be to limit the scope of the invention.
The room temperature is 25 ± 5 DEG C.The molybdenum box used and system in following embodiment, in diadust purifying step Metal cup used in standby composite sheet component step is that the tool for holding material is commonly used in existing production, prepares and applies in composite sheet To synthesis assembling block structure and application method disclosed in CN107362750A, this will not be repeated here.
Ct used below is quality (weight) unit carat of jewel, now surely 1 carat be equal to 0.2 gram or 200 milligrams.
Heretofore described nitric acid is commercially available concentrated nitric acid.Concentration of nitric acid is 69% in following embodiments.
Embodiment 1
A kind of preparation process of sub-micron diamond compact, comprising the following steps:
1) carbide matrix bottom surface takes off cobalt: polytetrafluoroethylene (PTFE) protection materials are coated on to the bottom surface and side of cement carbide substrate Then face is placed on HNO3: H2O volume ratio is 20 min of etch in the solution of 1:2.5, takes out cement carbide substrate and uses ionized water It rinses and obtains the cement carbide substrate that surface takes off cobalt to neutrality, take off cobalt layers with a thickness of 50 μm, take off cobalt layers cobalt content for 1.0%(weight Measure percentage)；
Wherein the material trade mark of cement carbide substrate is YG10, and specification is φ 45mm × 3.0mm；
2) diadust purifies: diadust being mixed with the sodium chloride of 200 mesh 1:2 in mass ratio, molybdenum is packed into after mixing It in box, is placed in vacuum sintering furnace, is evacuated in furnace air pressure 3 × 10-3Pa is hereinafter, temperature rises to 700 DEG C of heat preservation 1h；Vacuum Diadust is separated after 400 mesh screens with sodium chloride after processing, then boils rinsing diadust with deionized water 8h, until the deionized water conductivity value for being mixed with diadust dries less than 0.9 μ S/cm and obtains granularity as 0.5~1.0 μ The diadust of m；
3) it prepares polycrystalline diamond powder: being respectively the gold of the purified diadust of 88% step 2,7% by weight percent Belong to bonding agent and the grain growth inhibitor mixing of 5 %, obtain powder mixture, pour into the ball grinder of polytetrafluoroethylene (PTFE), It mixes, is subsequently placed in by powder mixture, dehydrated alcohol, polyethylene glycol, the weight ratio that sintered carbide ball is 1:0.2:0.02:5 Alternate-running mode ball milling wet type mixing 100h clockwise, counterclockwise is used on ball mill, obtains polycrystalline diamond powder；
Wherein, metallic bond is composed of the following weight percentages of raw materials: cobalt powder 98.5%, tungsten powder 0.5%, 0.3 % of rubidium powder, cerium 0.3 % of 0.4 % of powder and antimony powder, the metallic bond partial size are 60nm；
Grain growth inhibitor is composed of the following weight percentages of raw materials: carborundum powder 73%, 7 % of tungsten carbide powder, titanium carbonitride Powder 6%, 4 % of zirconium cyanonitride powder, 5 % of boron carbide powder, 1 % of carbonized titanium powder, nitridation 1 % of titanium valve, carbonization 1 % of vanadium powder, carbonization chromium powder 1 1 % of % and cubic boron nitride micro mist, the grain growth inhibitor partial size are 60nm；
The sintered carbide ball that sintered carbide ball is φ 3mm by the sintered carbide ball that diameter is φ 8mm and diameter is according to the weight of 1:1 Than mixing, the material trade mark of the sintered carbide ball is YG8；
In ball milling wet type mixing, revolving speed is 60 r/min when operating clockwise, and revolving speed is 60 r/min when counterclockwise, alternately up time The needle time is 5min, and alternately the time counterclockwise is 8min, and alternate intervals stand-by time is 0.5 min.
4) it prepares complex component: the polycrystalline diamond powder of 26Ct first being poured into metal cup, after striking off, then hard closed Gold substrate takes off cobalt surface and is placed in metal cup downward on polycrystalline diamond powder materials, buckles metal cup lid, is placed in vacuum-sintering In furnace, air pressure is evacuated in furnace up to 8 × 10-2Pa is hereinafter, being heated to 180 DEG C of heat preservation 0.5h, then proceeding to vacuumize while adding Heat is to 750 DEG C, until furnace internal pressure is stablized 3 × 10-3Then Pa is hereinafter, stop vacuumizing under the conditions of 750 DEG C to vacuum furnace Inside being filled with mixed gas makes the mixed gas of air pressure 60Mbar in furnace to complex component reduction treatment 3h, then is evacuated to furnace Interior 3 × 10- of air pressure3Pa is hereinafter, obtain complex component；
Wherein, mixed gas is grouped as by the group of following volumes percentage: hydrogen 35%, carbon dioxide 65%.Plycrystalline diamond Buddha's warrior attendant Contain oxide, gas and impurity in stone powder, removes while the purpose vacuumized can extract gas and inhaled with gas Impurity out can carry out reduction treatment to mixture after being passed through gas reaction.
5) it prepares composite sheet: the complex component that step 4) obtains being placed in synthesis assembling block inner cavity, synthesis is assembled Block is sintered to arrive the composite sheet of sub-micron diamond in cubic hinge press；
Sintering process is specific as follows: being passed through 900A electric current when pressure rises to 2GPa, later, boosts to 5GPa, be warming up to 1400 DEG C, after keeping 5min, cavity temperature is down to 750 DEG C with the rate of temperature fall of 90 DEG C/min, then again with the drop of 10 DEG C/min Cavity temperature is down to room temperature by warm rate, while chamber pressure is down to normal pressure with the rate of pressure reduction of 0.085GPa/min.
It is prepared that diameter is φ 45mm, total thickness 3mm, polycrystalline diamond thickness are 0.5mm's in detection the present embodiment Sub-micron diamond compact performance indicator:
Sub-micron diamond compact diamond layer average grain size is 0.73~0.75 μm；
Wear resistance ratio 330,000；
Thermal stability: after 700 DEG C roast 2 minutes, wear resistance ratio 31.5 ten thousand.
The wear resistance ratio and thermal stability of the composite sheet are also effectively improved and are improved, and diamond layer even tissue is fine and close, Without Phenomena of Grain Growth.Diamond layer institutional framework is observed with JSM-7610F scanning electron microscope and measures diamond crystals Size, the testing standard of wear resistance ratio are JB/T3235-2013 " diamond sintered body Measurement of abrasion ratio method ".
Embodiment 2
1) carbide matrix bottom surface takes off cobalt: polytetrafluoroethylene (PTFE) protection materials are coated on to the bottom surface and side of cement carbide substrate Then face is placed on HNO3: H2O volume ratio is 60 min of etch in the solution of 1:3, takes out cement carbide substrate and is rushed with ionized water It is washed till neutrality, obtains the cement carbide substrate that surface takes off cobalt, takes off cobalt layers with a thickness of 100 μm, taking off cobalt layers cobalt content is 1.2%(weight Percentage)；
Wherein the material trade mark of cement carbide substrate is YG10, and specification is φ 45mm × 3.0mm；
2) diadust purifies: diadust being mixed with the sodium chloride of 300 mesh 1:3 in mass ratio, molybdenum is packed into after mixing It in box, is placed in vacuum sintering furnace, is evacuated in furnace air pressure 3 × 10-3Pa is hereinafter, temperature rises to 800 DEG C of heat preservation 2h；Vacuum Diadust is separated after 400 mesh screens with sodium chloride after processing, then boils rinsing diadust with deionized water 16h, for the deionized water conductivity value up to being mixed with diadust less than 1 μ S/cm, drying and obtaining granularity is 0.5~1.0 μm Diadust；
3) it prepares polycrystalline diamond powder: being respectively the gold of the purified diadust of 92% step 2,5% by weight percent The grain growth inhibitor mixing for belonging to bonding agent and 3%, obtains powder mixture, pours into the ball grinder of polytetrafluoroethylene (PTFE), press Powder mixture, dehydrated alcohol, polyethylene glycol, the weight ratio that sintered carbide ball is 1:0.25:0.05:6 mix, and are subsequently placed in ball Alternate-running mode ball milling wet type mixing 150h clockwise, counterclockwise is used on grinding machine, obtains polycrystalline diamond powder；
Wherein, metallic bond is composed of the following weight percentages of raw materials: cobalt powder 99%, tungsten powder 0.3%, 0.2 % of rubidium powder, cerium powder 0.2 % of 0.3 % and antimony powder, the metallic bond partial size are 100nm；
Grain growth inhibitor is composed of the following weight percentages of raw materials: carborundum powder 84%, 4 % of tungsten carbide powder, titanium carbonitride Powder 3.5%, 3 % of zirconium cyanonitride powder, 3 % of boron carbide powder, 0.5 % of carbonized titanium powder, nitridation 0.5 % of titanium valve, carbonization 0.5 % of vanadium powder, carbon Change 0.5 % of chromium powder and 0.5 % of cubic boron nitride micro mist, the grain growth inhibitor partial size is 100nm；
The sintered carbide ball that sintered carbide ball is φ 5mm by the sintered carbide ball that diameter is φ 10mm and diameter is according to the weight of 1:1 Amount is YG8 than mixing, the material trade mark of the sintered carbide ball；
In ball milling wet type mixing, revolving speed is 80 r/min when operating clockwise, and revolving speed is 80 r/min when counterclockwise, is alternately transported Turn, the alternating clockwise time is 10min, and alternately the time counterclockwise is 12min, and alternate intervals stand-by time is 1 min.
4) it prepares complex component: the polycrystalline diamond powder of 26Ct first being poured into metal cup, after striking off, then hard closed Gold substrate takes off cobalt surface and is placed in metal cup downward on polycrystalline diamond powder materials, buckles metal cup lid, is placed in vacuum-sintering In furnace, air pressure is evacuated in furnace up to 8 × 10-2Pa is then proceeded to vacuumize while heated hereinafter, be heated to 230 DEG C of heat preservation 1h To 800 DEG C, until furnace internal pressure is stablized 3 × 10-3Then Pa is hereinafter, stop vacuumizing under the conditions of 800 DEG C into vacuum furnace Being filled with mixed gas makes the mixed gas of air pressure 80Mbar in furnace to complex component reduction treatment 4h, then is evacuated in furnace Air pressure 3 × 10-3Pa is hereinafter, obtain complex component；
Wherein, mixed gas is grouped as by the group of following volumes percentage: hydrogen 40%, carbon dioxide 60%.
5) it prepares composite sheet: the complex component that step 4) obtains being placed in synthesis assembling block inner cavity, synthesis is assembled Block is sintered to arrive the composite sheet of sub-micron diamond in cubic hinge press；
Sintering process is specific as follows: being passed through 1500A electric current when pressure rises to 3GPa, later, boosts to 6GPa, be warming up to 1500 DEG C, after keeping 10min, cavity temperature is down to 850 DEG C with the rate of temperature fall of 120 DEG C/min, then again with 15 DEG C/min's Cavity temperature is down to room temperature by rate of temperature fall, while chamber pressure is down to normal pressure with the rate of pressure reduction of 0.095GPa/min.
It is prepared that diameter is φ 45mm, total thickness 3mm, polycrystalline diamond thickness are 0.5mm's in detection the present embodiment Sub-micron diamond compact performance indicator:
Sub-micron diamond compact diamond layer average grain size is 0.73~0.74 μm；
Wear resistance ratio 330,000；Thermal stability:
After 700 DEG C roast 2 minutes, wear resistance ratio 320,000.
The wear resistance ratio and thermal stability of the composite sheet are also effectively improved and are improved, and diamond layer even tissue is fine and close, Without Phenomena of Grain Growth.Diamond layer institutional framework is observed with JSM-7610F scanning electron microscope and measures diamond crystals Size, the testing standard of wear resistance ratio are JB/T3235-2013 " diamond sintered body Measurement of abrasion ratio method ".
Embodiment 3
1) carbide matrix bottom surface takes off cobalt: polytetrafluoroethylene (PTFE) protection materials are coated on to the bottom surface and side of cement carbide substrate Then face is placed on HNO3: H2O volume ratio is etch 40min in the solution of 1:2.75, takes out cement carbide substrate and uses ionized water It rinses and obtains the cement carbide substrate that surface takes off cobalt to neutrality, take off cobalt layers with a thickness of 75 μm, take off cobalt layers cobalt content for 1.1%(weight Measure percentage)；
Wherein the material trade mark of cement carbide substrate is YG10, and specification is φ 45mm × 3.0mm；
2) diadust purifies: diadust being mixed with the sodium chloride of 250 mesh 1:2.5 in mass ratio, is packed into after mixing It in molybdenum box, is placed in vacuum sintering furnace, is evacuated in furnace air pressure 3 × 10-3Pa is hereinafter, temperature rises to 750 DEG C of heat preservation 1.5h； Diadust is separated after 400 mesh screens with sodium chloride after vacuum processing, then boils rinsing diamond with deionized water Micro mist 16h, for the deionized water conductivity value up to being mixed with diadust less than 0.5 μ S/cm, drying and obtaining granularity is 0.5 ~1.0 μm of diadust；
3) it prepares polycrystalline diamond powder: being respectively the gold of the purified diadust of 90% step 2,6% by weight percent The grain growth inhibitor mixing for belonging to bonding agent and 4%, obtains powder mixture, pours into the ball grinder of polytetrafluoroethylene (PTFE), press Powder mixture, dehydrated alcohol, polyethylene glycol, the weight ratio that sintered carbide ball is 1:0.225:0.035:5.5 mix, and then set In using alternate-running mode ball milling wet type mixing 125h clockwise, counterclockwise on ball mill, polycrystalline diamond powder is obtained；
Wherein, metallic bond is composed of the following weight percentages of raw materials: cobalt powder 98.75%, tungsten powder 0.4%, 0.25 % of rubidium powder, 0.25 % of 0.35 % of cerium powder and antimony powder, the metallic bond partial size are 80nm；
Grain growth inhibitor is composed of the following weight percentages of raw materials: carborundum powder 78.5%, tungsten carbide powder 5.5%, carbon nitrogen Change titanium valve 4.75%, zirconium cyanonitride powder 3.5%, 4 % of boron carbide powder, carbonized titanium powder 0.75%, nitridation titanium valve 0.75%, carbonization vanadium powder 0.75 %, carbonization 0.75 % of chromium powder and cubic boron nitride micro mist 0.75%, the grain growth inhibitor partial size are 80nm；
The sintered carbide ball that sintered carbide ball is φ 4mm by the sintered carbide ball that diameter is φ 9mm and diameter is according to the weight of 1:1 Than mixing, the material trade mark of the sintered carbide ball is YG8；
In ball milling wet type mixing, revolving speed is 70 r/min when operating clockwise, and revolving speed is 70 r/min when counterclockwise, is alternately transported Turn, the alternating clockwise time is 7min, and alternately the time counterclockwise is 10min, and alternate intervals stand-by time is 0.7 min.
4) it prepares complex component: the polycrystalline diamond powder of 26Ct first being poured into metal cup, after striking off, then hard closed Gold substrate takes off cobalt surface and is placed in metal cup downward on polycrystalline diamond powder materials, buckles metal cup lid, is placed in vacuum-sintering In furnace, air pressure is evacuated in furnace up to 8 × 10-2Pa then proceedes to vacuumize simultaneously hereinafter, be heated to 205 DEG C of heat preservation 0.75h 775 DEG C are heated to, until furnace internal pressure is stablized 3 × 10-3Then Pa is hereinafter, stop vacuumizing under the conditions of 775 DEG C to heating in vacuum Mixed gas is filled in furnace makes the mixed gas of air pressure 70Mbar in furnace to complex component reduction treatment 3.5h, then vacuumizes Air pressure 3 × 10 in furnace-3Pa is hereinafter, obtain complex component；
Wherein, mixed gas is grouped as by the group of following volumes percentage: hydrogen 37.5%, carbon dioxide 62.5%.
5) it prepares composite sheet: the complex component that step 4) obtains being placed in synthesis assembling block inner cavity, synthesis is assembled Block is sintered to arrive the composite sheet of sub-micron diamond in cubic hinge press；
Sintering process is specific as follows: being passed through 1200A electric current when pressure rises to 2.5GPa, later, boosts to 5.5GPa, be warming up to 1450 DEG C, after keeping 7.5min, cavity temperature is down to 800 DEG C with the rate of temperature fall of 105 DEG C/min, then again with 12.5 DEG C/cavity temperature is down to room temperature, while being down to chamber pressure with the rate of pressure reduction of 0.09GPa/min by the rate of temperature fall of min Normal pressure.
The diameter being prepared in detection the present embodiment is φ 45mm, total thickness 3mm, polycrystalline diamond thickness are 0.5mm Sub-micron diamond compact performance indicator:
Sub-micron diamond compact diamond layer average grain size is 0.74~0.75 μm, no Phenomena of Grain Growth；
Wear resistance ratio 340,000；
Thermal stability: after 700 DEG C roast 2 minutes, wear resistance ratio 31.8 ten thousand.
The wear resistance ratio and thermal stability of the composite sheet are also effectively improved and are improved.Diamond layer even tissue is fine and close, Without Phenomena of Grain Growth.Diamond layer institutional framework is observed with JSM-7610F scanning electron microscope and measures diamond crystals Size, the testing standard of wear resistance ratio are JB/T3235-2013 " diamond sintered body Measurement of abrasion ratio method ".
Comparative example 1
Difference from Example 1 is:
1) carbide matrix bottom surface takes off cobalt layers with a thickness of 49 μm, takes off cobalt layers cobalt content 1.3w%；
2) powder mixture is made of the material of following weight percent: diadust 87%, metallic bond 7.5% and crystal grain 5.5 % of growth inhibitor；
Composite sheet average grain size described in comparative example 1 is equal to 1 μm；Wear resistance ratio 280,000；Thermal stability: 2 points are roasted at 700 DEG C After clock, wear resistance ratio 250,000.Its wearability and thermal stability are poor.There are Phenomena of Grain Growth.
Comparative example 2
Difference from Example 1 is:
1) metallic bond is made of the raw material of following weight percent: cobalt powder 99.4%, tungsten powder 0.2%, 0.1 % of rubidium powder, cerium 0.1 % of powder 0.2% and antimony powder, metallic bond partial size are 60~100nm；
2) grain growth inhibitor is made of the raw material of following weight percent: carborundum powder 85%, 3.9 % of tungsten carbide powder, carbon Nitrogenize titanium valve 3.3%, zirconium cyanonitride powder 2.9%, 2.8 % of boron carbide powder, 0.45 % of carbonized titanium powder, nitridation 0.4 % of titanium valve, vanadium carbide 0.45 % of powder, carbonization chromium powder 0.4% and 0.4 % of cubic boron nitride micro mist, grain growth inhibitor partial size are 110nm.
Composite sheet average grain size described in comparative example 2 is equal to 1.2 μm；Wear resistance ratio 290,000；Thermal stability: at 700 DEG C After roasting 2 minutes, wear resistance ratio 260,000.Its wearability and thermal stability are poor.There are Phenomena of Grain Growth.
Comparative example 3
Difference from Example 3 is:
1) HNO3: H2The volume ratio of O is 1:2.4, and the etch time is 19 min；
The composite sheet average grain size that comparative example 3 is prepared is equal to 0.95 μm；Wear resistance ratio 300,000；Thermal stability: at 700 DEG C After roasting 2 minutes, wear resistance ratio 270,000.Its wearability and thermal stability are poor.There are Phenomena of Grain Growth.
Comparative example 4
Difference from Example 3 is:
1) diadust is mixed with the analysis pure sodium chloride 1:3.5 in mass ratio of 350 mesh；Temperature rises to 810 DEG C of heat preservation 2.5h； Rinsing diadust 17h is boiled with deionized water after vacuum processing, until being mixed with the deionized water conductivity of diadust 2 μ S/cm of numerical value；
Composite sheet average grain size obtained by comparative example 4 is less than or equal to 0.95 μm；Wear resistance ratio 270,000；Thermal stability: at 700 DEG C After roasting 2 minutes, wear resistance ratio 240,000.Its wearability and thermal stability are poor.There are Phenomena of Grain Growth.
It can be apparent from, sub-micron diamond compact average grain size made from embodiment 1-3 is less than or equal to 0.75 μ M not only has good wearability, but also the thermal stability of composite sheet is also effectively improved and is improved, diamond layer group Knit even compact, no Phenomena of Grain Growth.
Although to illustrate and describe the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention Many other change and modification can be made in the case where spirit and scope, it is, therefore, intended that in the claim All changes and modification including the scope of the invention belong to the scope of the present invention.

Claims (9)

1. a kind of preparation process of sub-micron diamond compact, which comprises the following steps:
1) carbide matrix bottom surface takes off cobalt: using HNO3: H2O volume ratio be 1:(2.5~3) solution in etch carbide matrix 20~60 min of bottom upper surface, after be rinsed with water, obtain surface take off cobalt cement carbide substrate；
2) diadust purifies: by diadust and sodium chloride 1:(2~3 in mass ratio) it mixes, it, will be golden after vacuum-sintering Hard rock micro mist is separated with sodium chloride, then uses 8~16h of boiling water rinses, the diadust after being purified；
3) it prepares polycrystalline diamond powder: being respectively the purified diadust of 88~92% step 2,5 by weight percent ~7% metallic bond and 3~5% grain growth inhibitor mixing, obtain powder mixture, in powder mixture plus Enter dehydrated alcohol, polyethylene glycol, sintered carbide ball, mixes 100~150h, obtain polycrystalline diamond powder；
4) it prepares complex component: cement carbide substrate being taken off into cobalt surface and polycrystalline diamond powder contact, vacuum-sintering is passed through After mixed gas reaction with reproducibility, then it is evacuated to air pressure 3 × 10-3Pa is hereinafter, obtain complex component；
5) it prepares composite sheet: the complex component that step 4) obtains is placed in synthesis assembling block inner cavity, synthesis assembling block is existed It is sintered in cubic hinge press to get the composite sheet of sub-micron diamond is arrived.
2. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that vacuum is burnt in step 2 The design parameter of knot are as follows: be evacuated to air pressure 3 × 10-3Pa is hereinafter, temperature rises to 700~800 DEG C of 1~2h of heat preservation.
3. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that metal knot in step 3) Mixture is composed of the following weight percentages of raw materials: cobalt powder 98.5~99%, tungsten powder 0.3~0.5%, 0.2~0.3 % of rubidium powder, cerium 0.2~0.3 % of 0.3~0.4 % of powder and antimony powder, the metallic bond partial size are 60~100nm.
4. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that crystal grain is raw in step 3) Long inhibitor is composed of the following weight percentages of raw materials: carborundum powder 73~84%, tungsten carbide powder 4~7%, titanium carbonitride powder 3.5~6%, zirconium cyanonitride powder 3~4%, 3~5 % of boron carbide powder, carbonized titanium powder 0.5~1%, nitridation titanium valve 0.5~1%, vanadium carbide Powder 0.5~1%, carbonization 0.5~1 % of chromium powder and cubic boron nitride micro mist 0.5~1%, the grain growth inhibitor partial size are 60 ~100nm.
5. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that powder is mixed in step 3) Closing material, dehydrated alcohol, polyethylene glycol, sintered carbide ball is 1:(0.2~0.25): (0.02~0.05): the weight ratio of (5~6) Mixing；The sintered carbide ball that sintered carbide ball is 3~φ of φ 5mm by the sintered carbide ball that diameter is 8~φ of φ 10mm and diameter It is mixed according to the weight ratio of 1:1.
6. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that powder is mixed in step 3) Close the concrete mode that material, dehydrated alcohol, polyethylene glycol, sintered carbide ball mix are as follows: using alternate-running counterclockwise clockwise Mode wet ball mill, revolving speed is 60~80 r/min when operating clockwise, and revolving speed is 60~80 r/min when counterclockwise, is alternately transported Turn, the alternating clockwise time is 5~10min, and alternately the time counterclockwise is 8~12min, and alternate intervals stand-by time is 0.5~1 min。
7. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that step 4) mesocomplex The design parameter of component vacuum-sintering are as follows: be evacuated in furnace air pressure up to 8 × 10-2Pa is hereinafter, be heated to 180~230 DEG C of heat preservations 0.5~1h then proceedes to vacuumize while being heated to 750~800 DEG C, until furnace internal pressure is stablized 3 × 10-3Pa or less is vacuumized again Air pressure 3 × 10 in furnace-3Then Pa is hereinafter, stop vacuumizing being filled in furnace under the conditions of 750~800 DEG C into vacuum furnace Air pressure is the mixed gas of 60~80Mbar to complex component 3~4h of reduction treatment, then is evacuated to air pressure 3 × 10 in furnace- 3Pa or less；The mixed gas is that 35~40% hydrogen and 60~65% carbon dioxide form by percent by volume.
8. the preparation process of sub-micron diamond compact as described in claim 1, which is characterized in that sintered in step 5) Journey is specific as follows: after being passed through 900-1500A electric current when pressure rises to 2~3GPa, 5~6GPa is boosted to, it is warming up to 1400~ 1500 DEG C, after keeping 5~10min, cavity temperature is down to 750~850 DEG C with the rate of temperature fall of 90~120 DEG C/min, so Cavity temperature is down to by room temperature with the rate of temperature fall of 10~15 DEG C/min again afterwards, while with the drop of 0.085~0.095GPa/min Press rate that chamber pressure is down to normal pressure.
9. the sub-micron diamond compact obtained using any preparation process of claim 1-8, which is characterized in that described Sub-micron diamond compact include cement carbide substrate and be compounded in cement carbide substrate take off cobalt surface on plycrystalline diamond Buddha's warrior attendant Rock layers, cement carbide substrate upper surface take off cobalt layers with a thickness of 50~100 μm, and taking off cobalt layers cobalt content is 1~1.2%.
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