CN104661776A - Method for transceiving downlink signal in wireless communication system and apparatus therefor - Google Patents
Method for transceiving downlink signal in wireless communication system and apparatus therefor Download PDFInfo
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- CN104661776A CN104661776A CN201380049660.2A CN201380049660A CN104661776A CN 104661776 A CN104661776 A CN 104661776A CN 201380049660 A CN201380049660 A CN 201380049660A CN 104661776 A CN104661776 A CN 104661776A
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- superhard
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
- E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
- E21B10/56—Button-type inserts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
- B24D3/06—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements
- B24D3/10—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements for porous or cellular structure, e.g. for use with diamonds as abrasives
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
- E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
- E21B10/56—Button-type inserts
- E21B10/567—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
- E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
- E21B10/56—Button-type inserts
- E21B10/567—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts
- E21B10/5676—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts having a cutting face with different segments, e.g. mosaic-type inserts
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
- E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
- E21B10/56—Button-type inserts
- E21B10/567—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts
- E21B10/573—Button-type inserts with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts characterised by support details, e.g. the substrate construction or the interface between the substrate and the cutting element
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
- E21B10/46—Drill bits characterised by wear resisting parts, e.g. diamond inserts
- E21B10/54—Drill bits characterised by wear resisting parts, e.g. diamond inserts the bit being of the rotary drag type, e.g. fork-type bits
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Mining & Mineral Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Earth Drilling (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Powder Metallurgy (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
Abstract
A superhard polycrystalline construction comprises a body of polycrystalline superhard material formed of a mass of superhard grains exhibiting inter-granular bonding and defining a plurality of interstitial regions therebetween, the superhard grains having an associated mean free path; and a non-superhard phase at least partially filling a plurality of the interstitial regions and having an associated mean free path. The average grain size of the superhard grains is less than or equal to 25 microns; and the ratio of the standard deviation in the mean free path associated with the non-superhard phase to the mean of the mean free path associated with the non-superhard phase is greater than or equal to 80% when measured using image analysis techniques at a magnification of 1000. There is also disclosed a method of forming such a superhard polycrystalline construction.
Description
Technical field
The present invention relates to the method for superhard construction and this structure of manufacture, special but be not limited to comprise polycrystalline diamond (PCD) structure being attached to substrate, and be used as the cutting insert (cutter insert) of drill bit or the structure of element of earth's crust probing (boring into theearth).
Background technology
Polycrystalline superhard material such as polycrystalline diamond (PCD) and polycrystal cubic boron nitride (PCBN) can be used to multiple types of tools, and these instruments are used for cutting, machining, boring or crushing hard or grinding-material as rock, metal, pottery, composite and containing wood material.Particularly, the tool inserts comprising cutting element (cutting element) form of PCD material is widely used in carrying out earth's crust probing with the drill bit of recover petroleum or natural gas.The working life of sintered carbide tools inserts can comprise by the fracture (fracture) of superhard material peels off (spalling) and cracked (chipping) limit, or limit by the wearing and tearing of tool inserts.
As the cutting element for rock drill bit or other cutting element typically has substrate and superhard material formal subject, described substrate has interface edge/surface, and described superhard material forms by such as sintering process the cutting lay being incorporated into the interface surface of substrate.Substrate is made up of the tungsten-cobalt carbide alloy sometimes referred to as cemented tungsten carbide usually, and ultra hard material layer typically is polycrystalline diamond (PCD), polycrystal cubic boron nitride (PCBN) or thermally-stabilised product TSP material as thermally-stabilised polycrystalline diamond.
Polycrystalline diamond (PCD) is an example of superhard material (also referred to as super hard abrasive material), it comprises the diamond crystals of a large amount of intergrowth substantially, forms the skeleton body (skeletal mass) in the gap limited between diamond crystals.PCD material typically comprises the diamond at least about 80 volume %, and usually by making the aggregation of diamond crystals stand such as to be greater than the hyperpressure of about 5GPa and manufacture at least about the temperature of 1200 DEG C.The material of filling described gap whole or in part can be called as filler or adhesive material.
PCD is typically formed under the existence of sintering aid as cobalt, and sintering aid promotes the intergrowth of diamond crystals.The sintering aid be applicable to for PCD dissolves diamond and its reppd function of catalysis to a certain extent due to it, is usually also referred to as adamantine solvent-catalyst material.Be understood to can to promote adamantine growth under diamond thermodynamically stable pressure and temperature condition for adamantine solvent-catalyst or between diamond crystals direct diamond to the material of adamantine intergrowth.Therefore remaining solvent-catalyst material can be filled with whole or in part in the gap in the PCD product of sintering.Most typical, PCD is formed in cobalt-cemented tungsten carbide substrate, and this substrate is the source that PCD provides cobalt solvent-catalyst.Do not promote that the material of basic coherent growth mutually between diamond crystals itself can form strong combination with diamond crystals, but its solvent-catalyst be not applicable to is sintered for PCD.
The cemented tungsten carbide that can be used to form applicable substrate, by the carbide particle be scattered in cobalt matrix, is formed by tungsten carbide particle/crystal grain and cobalt being mixed then to be heating and curing.In order to be formed, there is the cutting element of ultra hard material layer as PCD or PCBN; by diamond particles or crystal grain or CBN crystal grain and cemented tungsten carbide main body is contiguous in refractory metal cover (enclosure) is as niobium cover places; and stand high pressure and high temperature; thus the intercrystalline occurred between diamond crystals or CBN crystal grain combines (inter-grain bonding), form polycrystalline diamond or polycrystalline CBN layer.
In some cases, substrate fully can be solidified before being attached to ultra hard material layer, and in other cases, substrate can be raw (green), does not namely solidify completely.In the case of the latter, substrate fully can be solidified in HTHP sintering process.Substrate can be powder type, and can be cured in the sintering process for sintering ultra hard material layer.
Make constantly to increase the demand of the material for rock cutting to the continuous increase of the driving force improving productivity in earth's crust drilling field.Specifically, the PCD material of the wearability and resistance to impact with improvement is needed to realize cutting rate and longer life tools faster.
Cutting element for rock-boring and other operation needs high-wearing feature and resistance to impact.The successful factor of restriction polycrystalline diamond (PCD) wear-resisting cutting members is the heat produced due to the friction between PCD and rapidoprint.This heat causes the thermal degradation (thermaldegradation) of diamond layer.Breaking and peeling off increase and cause the reversal of diamond to graphite of wearing and tearing increase due to PCD layer, thermal degradation adds the rate of depreciation of cutting members.
Method for improving the wearability of PCD composite usually causes the resistance to impact of composite to reduce.Therefore need that there is the wearability of improvement and the PCS composite of resistance to impact, and form the method for this composite.
Invention summary
From first aspect, the invention provides a kind of ultrahard polycrystalline structure, it comprises by the following polycrystalline superhard material main body formed:
A large amount of superhard crystal grain, it demonstrates intergranular and combines and limit multiple gap area betwixt, and described superhard crystal grain has relevant mean free path;
Non-superhard phase, it fills multiple described gap area at least partly, and has relevant mean free path;
Wherein:
The average grain diameter of described superhard crystal grain is less than or equal to 25 microns; And
When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of non-superhard mutually relevant mean free path with the ratio of the mean value of non-superhard relevant mean free path.
From second aspect, the invention provides a kind of method forming ultrahard polycrystalline structure, comprising:
There is provided a large amount of superhard material crystal grain, described superhard material crystal grain comprises Part I and Part II, and described Part I has the first average-size, and described Part II has the second average-size,
Arrange that a large amount of superhard crystal grain is to form pre-sintered components (pre-sinter assembly); And
Under the hyperpressure of about 6GPa or larger and at the described superhard material temperature thermodynamically more stable than graphite, under the existence of the catalyst/solvent material for described superhard crystal grain, process described pre-sintered components, by grained sintered for described superhard material together to form polycrystalline superhard construction, described superhard crystal grain demonstrates intergranular and combines and limit multiple gap area betwixt, to be non-ly superhardly filled at least partly mutually in multiple gap area; Wherein said non-ly superhardly have relevant mean free path mutually; And
Wherein:
The average grain diameter of described superhard crystal grain is less than or equal to 25 microns; And
When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of non-superhard mutually relevant mean free path with the ratio of the mean value of non-superhard relevant mean free path.
On the other hand, the invention provides a kind of instrument, it comprises ultrahard polycrystalline as defined above structure, and described instrument is used for cutting, grinding (milling), grinding (grinding), boring (drilling), earth's crust probing (earth boring), rock-boring (rock drilling) or other abrasive applications.
Described instrument can comprise, such as the earth's crust probing or rock-boring drill bit, for oil and natural gas probing industry rotation fix cut drill or roller cone drill bits, drilling tool, bloat tool (expandable tool), drill or other earth's crust boring tool.
From other aspect, the invention provides a kind of drill bit, cutting members or the assembly for it that comprise ultrahard polycrystalline as defined above and construct.
Brief Description Of Drawings
Mode by embodiment is also described with reference to accompanying drawing by the present invention, wherein:
Fig. 1 is attached to suprabasil polycrystalline diamond (PCD) structure;
Fig. 2 shows the schematic sectional view of the embodiment of a part for PCD structure;
Fig. 3 shows the schematic longitudinal section figure of PCD element embodiment;
Fig. 4 shows the schematic longitudinal section figure of PCD element embodiment;
Fig. 5 shows the schematic perspective view of a part for earth's crust probing drill bit embodiment;
Fig. 6 A shows the schematic longitudinal section figure of the pre-sintered components embodiment for PCD element;
Fig. 6 B shows the schematic longitudinal section figure of PCD element embodiment;
Fig. 7 A, 7B, 7C and 7D show the schematic sectional view of a part for PCD constructive embodiment;
Fig. 8 is the stereogram with the cutting element of non-planar interface of an embodiment;
Fig. 9 a is the stereogram of multiple projections of Fig. 8 in free space;
Fig. 9 b is the schematic plan view of the substrate of the cutting element of Fig. 8;
Fig. 9 c is the schematic sectional view of the substrate along axle A-A as shown in figure 9b;
Fig. 9 d is the schematic perspective view of the substrate of the cutting element of Fig. 8;
Figure 10 is the stereogram of the cutting element of an embodiment;
Figure 11 is the stereogram of the substrate of another embodiment;
Figure 12 a is the stereogram of the substrate of the cutting element of another embodiment;
Figure 12 b is the schematic plan view of the substrate of the cutting element of Figure 12 a;
Figure 12 c is the schematic sectional view of the substrate along the axle A-A shown in Figure 12 b;
Figure 13 is the interval graph of the cracked height of an embodiment and two conventional reference cutting members;
Figure 14 is from illustrating that the percent of pass (passrate) of an embodiment and two conventional reference cutting members falls the figure of test (high energy drop test) to the high energy falling energy (drop energy);
Figure 15 be an embodiment and five conventional reference cutting members pierce into the figure of the degree of depth relative to penetration rate.
Detailed Description Of The Invention
As used herein, " superhard material " is the material that Vickers hardness is at least about 28GPa.Diamond and cubic boron nitride (cBN) material are the examples of superhard material.
As used herein, " superhard construction " refers to the structure containing polycrystalline superhard material main body.In such configuration, described main body can be attached with substrate, or polycrystalline material main body can be self-supporting (free-standing) and linerless (unbacked).
As used herein, polycrystalline diamond (PCD) is a class polycrystalline superhard (PCS) material, it comprises a large amount of diamond crystals, and major part wherein directly combines each other, and wherein adamantine content be described material at least about 80 volume %.In an embodiment of PCD material, the gap between diamond crystals can be filled with the adhesive material comprised for adamantine catalyst at least in part.As used herein, " gap " or " gap area " is the region between the diamond crystals of PCD material.In the embodiment of PCD material, gap or gap area can be filled with the material beyond diamond substantially or partly, or they can be empty substantially.PCD material can comprise at least one region, and from this region, catalyst material removes from gap, leaves the interstitial void between diamond crystals.
As used herein, PCBN (polycrystal cubic boron nitride) material refers to a class superhard material, and it contains intramatrical cubic boron nitride (cBN) crystal grain being scattered in and comprising metal or pottery.PCBN is an example of superhard material.
" catalyst material " for superhard material can promote growth or the sintering of superhard material.
As used herein, term " substrate " refers to any substrate forming ultra hard material layer thereon.Such as, as used herein " substrate " another suprabasil transition zone can be formed in.In addition, as used herein, term " radial (radial) " and " circumferential (circumferential) " and similar term also do not mean that the feature described by restriction is positive round (perfect circle).
Superhard construction 1 shown in Fig. 1 can be suitable as such as the cutting insert of the drill bit of earth's crust probing.
In all the drawings, identical Ref. No. is for representing identical feature.
In the embodiment shown in figure 1, cutting element 1 comprises substrate 10, forms superhard material main body 12 on the substrate 10.Described substrate can by hard material as cemented tungsten carbide be formed.Superhard material can be that such as polycrystalline diamond (PCD), polycrystal cubic boron nitride (PCBN) or thermally-stabilised product are as thermally stable P CD (TSP).Cutting element 1 can be installed to bit body as in drag bit body (not shown).With substrate back to the top surface of exposure of superhard material form cutting face 14, this is the surface of in use carrying out along its edge 16 cutting.
Be the interface surface 17 with superhard material main body 12 interface cohesion in one end of substrate 10, superhard material main body 12 is attached with substrate 10 in this interface surface.Substrate 10 is normally columniform, and has outer surface 18 and periphery top edge 19.
Superhard material crystal grain in starting mixt before sintering such as diamond crystals or particle can be such as bimodulus (bimodal), and that is, charging comprises the mixture of diamond crystals coarse component and diamond crystals fine fraction.In some embodiments, coarse component can have the average grain/grain size range of such as about 10 to 60 microns." average grain or crystallite dimension " refers to that individual particle/crystal grain has a size range, and this size range has the average grain/crystallite dimension of expression " mean value ".Average grain/the crystallite dimension of fine fraction is less than the size of coarse component, and such as, between about 1/10 to 6/10 of the size of coarse component, and scope of embodiments is such as about 0.1 to 20 microns in some embodiments.
In some embodiments, brait part is to the weight ratio of fine diamond part in the scope of about 50% to about 97% brait, and the weight ratio of fine diamond part can be about 3% to about 50%.In other embodiments, coarse component to the weight ratio of fine fraction by about 70:30 to about 90:10 scope in.
In other embodiments, coarse component can in the scope of such as about 60:40 to about 80:20 to the weight ratio of fine fraction.
In some embodiments, the domain size distribution of coarse grain and fine fraction is not overlapping, and in some embodiments, between the independent particle size fraction of composition multimodal distribution, the one-tenth of the different size of briquet (compact) separates an order of magnitude.
Described embodiment can be made up of at least one the wide bimodal size distribution between the coarse grain and fine fraction of superhard material, but some embodiments can comprise the size pattern of three or even four or more, these patterns such as can separate an order of magnitude dimensionally, and such as average grain diameter is 20 microns, 2 microns, the mixing of the particle diameter of 200 nanometers and 20 nanometers.
In some embodiments, the average grain diameter of superhard crystallite aggregate is less than or equal to 25 microns.In some embodiments, described average grain diameter is between about 8-20 micron.
The size of diamond particles/crystal grain is become fine fraction, coarse component or other size in-between to pulverize to have come compared with king kong stone crystal grain and similar method as sprayed by known method.
Be in the embodiment of polycrystalline diamond abrasive compact at superhard material, the diamond crystals for the formation of polycrystalline diamond abrasive compact can be natural or Prof. Du Yucang.
As used herein, term " stress state " refers to compressive stress state, unstress state or tensile stress state.Compressive stress state and tensile stress state can be understood as reciprocal stress state.In columned geometrical system, stress state can be axial, radial or circumference or netted stress state.
In some embodiments, the superhard material main body 12 shown in Fig. 1 can be bedded structure or have multiple region, as described below and as shown in Fig. 2-5c.First other embodiment illustrates with reference to Fig. 2, and Fig. 2 illustrates an example of PCD structure 12, and it comprises at least two constricted zones 21 being in residual compressive stress state spatially separated and at least one is in the stretch-draw region 22 of tensile residual stresses state.Stretch-draw region 22 is coupled between the constricted zone 21.
The mechanical performance of PCD material can be selected, as the change of density, elastic modelling quantity, hardness and thermal coefficient of expansion (CTE), to obtain the structure in the stretch-draw region between two constricted zones.This change can pass through content and type, the Size Distribution of PCD crystal grain or the change of average-size of diamond crystals content, packing material, and obtains to use the PCD of different brackets with itself or with the diamond matrix of the mixture comprising PCD grade.
With reference to Fig. 3, another example is that PCD structure 12 is integrally connected to sintered-carbide supporting mass 10.PCD structure 12 comprises several constricted zones 21 and several stretch-draw regions 22 of (interlocking) layer form alternately.The shape of PCD structure 12 can be essentially cylindric, is positioned at working end and limits working surface 14.PCD structure 12 can be connected to supporting mass 10 in non-planar interface 17.The thickness in constricted zone 21 and stretch-draw region 22 is in the scope of about 5 microns to about 200 microns, or in some embodiments, in the scope of about 5 microns to about 300 microns, described region can be set to substantially parallel with the working surface 14 of PCD structure 12.The region 26 being roughly annular can be arranged around the non-planar parts 31 stretched out from supporting mass 10.
With reference to Fig. 4, the example of PCD element 1 is included in the PCD structure 12 that non-planar interface 25 is integrally connected to sintered-carbide supporting mass 10, and this interface 25 is relative with the working surface 14 of PCD structure 12.PCD structure 12 can comprise the constricted zone 21 replaced and the stretch-draw region 22 of the layer form that about 10-20 extends.In this embodiment, the region 26 not containing layer can be disposed adjacent with interface 25.Layer 21,22 can be bending or arc, and usually aligns with interface 25, and can be crossing with the side surface 27 of PCD structure.Some layers can be crossing with working surface 14.
In some embodiments, the thickness in region 26 can than independent layer 21,22 much thick, in some embodiments, the thickness comprising the region of alternating layer 21,22 can be thicker than the thickness in the region 26 adjacent with the sintered-carbide supporting mass 10 of the substrate forming PCD material.
In some embodiments, the region 26 adjacent with supporting mass 10 can comprise multiple layers of (not shown), their the single layer of Thickness Ratio 21,22 much thick, such as, the thickness of layer 21,22 is in the scope of about 5-200 micron, and the thickness of layer in the region 26 adjacent with supporting mass 10 is greater than about 200 microns.
In some embodiments, such as in the embodiment shown in Fig. 2-4, the thickness of alternating layer 21,22 is in the scope of about 5-300 micron, and diamond is by the PCD with two or more different average diamond grain size, the mixture of the PCD of such as two or more grades is formed.Such as, the gathering diamond matrix that layer 21 can be A and B by average diamond grain size is formed, and layer 22 also can be A with B by average diamond grain size but the diamond matrix different from the ratio of layer 21 is formed.In interchangeable embodiment, the diamond matrix that layer 21 can be A and B by average diamond grain size is formed, and the diamond matrix that layer 22 can be C by average diamond grain size is formed.It should be understood that other order/mixing any of two or more diamond grain size also can be used for forming alternating layer 21,22.In these embodiments, adjacent with supporting mass 10 region 26 can be formed by than independent layer 21, the single layer of 22 much thick (such as, being greater than about 200 microns).Or, region 26 can by the diamond matrix being used for forming layer 21,22 comprise multiple layers that average grain size is the diamond crystals of A and B and/or C, single layer formed, or another material or diamond grain size can be used for forming the layer in this region 26 adjacent with supporting mass 10.
In some embodiments, diamond layer 21,22 and/or the layer (not shown) formed in the region 26 adjacent with supporting mass 10 can comprise following in one or more, such as up to Nano diamond additive, salt system, the boride of the Nano diamond powder form of 20wt%, the metal carbides of Ti, V, Nb, or any one in metal Pd or Ni.
In some embodiments, layer 21,22 and/or the layer that formed in the region 26 adjacent with supporting mass 10 can be in the longitudinal axis constructing 1 with diamond and extend in the substantially vertical plane of the plane passed through.Such as owing to bearing super-pressure in sintering process, layer can be plane, bending, arc, dome-shaped or distortion.Alternatively, the planar registration that the longitudinal axis that alternating layer 21,22 can construct 1 with diamond at a predetermined angle extends through, thus affect performance by controlling Crack Extension.
Fig. 5 is the schematic diagram of the embodiment of earth's crust probing drill bit 39, inserts multiple cutting elements 1 of type as shown in Figure 1 in the earth's crust.Cutting element 1 can comprise any one modification shown in all the other accompanying drawings.
With reference to Fig. 6 A, example for the manufacture of the pre-sintered components 40 of PCD element can comprise supporting mass 30, comprise the region 46 of the diamond crystals that the on-plane surface end against supporting mass 30 loads, and be stacked on region 46 usual with disk or wafer 41,42 form multiple replace containing diamond aggregation.In some versions, aggregation can be the form of loose diamond crystals or particle (granule).Pre-sintered components can be heated, to remove the adhesive material be included in stacking disk.
With reference to Fig. 6 B, the example of PCD element 100 comprises PCD structure 200, PCD structure 200 and comprises multiple alternating layer 210,220 formed by the PCD material of each different multimode grade, and does not comprise the part 260 of layer.Part 260 can be formed according to the form fit of the on-plane surface end of supporting mass 300, and is integrally combined with this on-plane surface end in ultra high pressure treatment process.The alternating layer 210,220 of the mixture of the PCD of different brackets or diamond grain size or grade is combined by direct diamond-diamond intergrowth, to form entirety, the firm and PCD structure 200 of layering.Owing to subjected to super-pressure, the shape of PCD layer 210,220 can be bending, arc or distortion to a certain extent.In some schemes of the method, consider that structure may be out of shape in super-pressure and high-temperature process, aggregation can be arranged in pre-sintered components, to obtain other Rotating fields multiple in PCD structure.
Due to the average diamond grain size that layer is different, layer 21,22,210,220 can comprise different each PCD grades.The catalyst material of different amount can penetrate in the dissimilar disk 410,420 comprised in pre-sintered components, because the diamond crystals that they comprise has different average-sizes, the bulk thus between diamond crystals is different.The PCD layer 21,22,210,220 replaced accordingly can therefore comprise different, alternately amount for adamantine catalyst material.In stretch-draw region, the volume percent content of filler can be greater than the volume percent content of the filler in each constricted zone.
In an example, the average-size of the diamond crystals of compression layer can be larger than the average-size of the diamond crystals of stretch-draw layer.
Although do not wish by specific theory constraint, when the High-temperature cooling allowing the PCD structure of layering to be formed from it, the alternating layer comprising the Metal catalyst materials of different amount can shrink with different speed.This may be that metal contracts is more much bigger in fact than diamond because when from High-temperature cooling.This different shrinkage factor can cause adjacent layer each other towards the other side's pushing, produces relative stress thus in them.
The PCD element 100 described with reference to Fig. 6 B can change its shape by grinding, thus is formed substantially as the PCD element of Fig. 4 description.This may relate to the part removing some bending layers, to be formed substantially for the working surface of plane with substantially for columned side surface.Catalyst material can remove from the region with working surface or side surface or the working surface PCD structure adjacent with side surface.This can by realizing by acid treatment PCD structure, with elimination catalyst material between diamond crystals, or by other method as electrochemical method realizes.Therefore can provide the basic heat-staple region for porous, this region extends from the surface of PCD structure at least about 50 microns or at least about the degree of depth of 100 microns.Illustrate that some have the embodiment of 50 to 80 micron thick layer (in this thick-layer, this leaches the degree of depth about 250 microns), shown the performance significantly improved, such as, compared with the PCD product of non-leaching, double in performance after leaching.In an example, the basic region for porous can comprise the catalyst material of 2wt% at the most.
By the difference of such as binder content, use the alternating layer with various grain sizes, can controllably obtaining different structures when implementing the acid-hatching of young eggs to PCD structure 1,100, especially adhesive not comprised to the embodiment of V and/or Ti.Such structure can be that different tungsten residual volume in each layer causes in HCl acid-hatching of young eggs process.In essence, leaching rate can be different (except non-usage is containing the acid of HF) in each layer, and this can especially in the preferential leaching in the edge of PCD material.When layer thickness is greater than 120 microns, this understands more obvious.If use the HF acid-hatching of young eggs to PCD material, then this can not occur.Reason is, in such a process, HCl acid is removed Co and leaves tungsten, and the HF acid-hatching of young eggs can remove any element in adhesive component.
With reference to Fig. 7 A, it is the layers 210,220 of plane substantially that an exemplary variation of PCD structure 200 comprises at least three of being arranged in structure alternately, and it is arranged essentially parallel to the working surface 240 of PCD structure 200 and crossing with the side surface 270 of PCD structure.
With reference to Fig. 7 B, an exemplary variation of PCD structure 200 comprises at least three layers 210,220 be arranged in structure alternately, described layer has bending or arc shape, at least part of inclination of this layer, away from working surface 240 and the cutting edge (cutting edge) 280 of PCD structure.
With reference to Fig. 7 C, an exemplary variation of PCD structure 200 comprises at least three layers 210,220 be arranged in structure alternately, and at least part of inclination of this layer, away from the working surface 240 of PCD structure, and extends towards the cutting edge 280 of PCD structure usually.
With reference to Fig. 7 D, an exemplary variation example of PCD structure 200 comprises at least three layers 210,220 be arranged in structure alternately, the at least part of of some in layer aligns with the working surface 240 of PCD structure substantially, and at least part of of some in layer aligns with the side surface 270 of PCD structure usually.Layer can be the annular of part ring usually, and with PCD structure 200 be roughly columned side surface 270 essentially concentric.
PCD structure can have the surf zone adjacent with working surface, and this region comprises the PCD material with the most about 1050MPa or the most about 1000MPa Young's modulus.Surf zone can comprise thermally stable P CD material.
Some embodiments of PCD structure can have at least 3, at least 5, at least 7, at least 10 or even at least 15 constricted zones, and stretch-draw region is between them.
In some embodiments, the thickness of each layer can be at least about 5 microns, is at least about 30 microns in other embodiments, is at least about 100 microns in other embodiments, or is at least about 200 microns in other embodiments.In some embodiments, the thickness of each layer can be such as about 300 microns at the most, or about 500 microns at the most.In some exemplary embodiments, the thickness of each layer can be PCD structure from working surface one end a bit to the thickness a bit measured on relative surface at least about 0.05%, at least about 0.5%, at least about 1% or at least about 2%.In some embodiments, the thickness of each layer is at the most about 5% of the thickness of PCD structure.
Term used herein " residual stress state " refers to when not having the outside load forces applied, the stress state of main body or portion body.Comprise the PCD structure of Rotating fields residual stress state can by deformeter and little by little successively remove material measure.In some embodiments of PCD element, at least one constricted zone can have at least about 50MPa, at least about 100MPa, at least about 200Mpa, at least about 400MPa or even at least about the residual compressive stress of 600MPa.The difference in size of residual stress between adjacent layers can be at least about 50MPa, at least about 100MPa, at least about 200MPa, at least about 400MPa, at least about 600MPa, at least about 800Mpa or even at least about 1000MPa.In one embodiment, at least two continuous print constricted zones or stretch-draw region can have different residual stress.PCD structure can comprise at least three constricted zones or stretch-draw region, and each all has different residual compressive stress, and described region is arranged with the order of compression or tensile stress size increasing or decreasing respectively.
In an example, the average tenacities in each region can be 16MPa.m at the most
1/2.In some embodiments, the average hardness in each region can be at least about 50GPa or at least about 60GPa.The average Young's modulus in each region can be at least about 900MPa, at least about 950MPa, at least about 1000 or even at least about 1050MPa.
" horizontal breaking resistance " (TRS) used herein measures in the following manner: make the sample of the rod type with width W and thickness T stand the load applied three positions, wherein two positions are in the side of sample, a position is on relative side, and increase load, until sample fractures when load p with certain loading speed.Then calculate this TRS based on the size of load p, sample, span L, span L is the distance between two load position on side.Above-mentioned metering system also can be called three point bending test, and is described in " Ceramics, mechanical properties; failure behaviour; materials selection " (1999, Spring, Berlin) by D.Munz and T.Fett.The TRS measuring the PCD material corresponding to specific grade is realized by the TRS of the sample measuring the PCD be made up of this grade.
Although provide the PCD structure with the PCD layer containing compressive stress state alternately and tensile stress state to tend to increase the effective toughness of entirety of PCD structure, this can have the effect increasing potential layering incidence, and its middle level is tended to separately.Although do not wish the constraint by particular theory, if PCD layer is firm in not the residual stress stood between them, then may tend to occur layering.This result can be improved by selecting PCD grade and the special PCD grade forming stretch-draw region, thus has sufficiently high TRS.The TRS of the TRS of PCD grade or the PCD grade in formation stretch-draw region should be greater than its residual tensions that can stand.A kind of mode of the stress intensity that influence area may be born is, selects the relative thickness of adjacent area.Such as, by selecting the thickness in stretch-draw region, making it be greater than the thickness of adjacent constricted zone, the size of the tensile stress in stretch-draw region can be reduced.
The residual stress state in region can change along with temperature.In use, the temperature of PCD structure may have difference greatly close between the point of cutting edge and the point away from cutting edge.In some applications, the temperature near cutting edge can reach hundreds of degree Celsius.If temperature exceedes about 750 degrees Celsius, deposit in case at the catalyst material of such as cobalt, diamond may change graphite material into, and this is undesirable.Therefore, in some applications, the alternate stress state in adjacent area as herein described should be considered at up to the temperature of about 750 degrees Celsius.
The K of PCD disk is measured by the mode of diametral compression test (diametral compression test)
1c toughness, this is by Lammer (" Mechanical properties of polycrystallinediamonds ", Materials Science and Technology, volume 4,1988, and Miess (Miess p.23.), and Rai D., G., " Fracture toughness and thermal resistances ofpolycrystalline diamond compacts ", Materials Science and Engineering, 1996, volume A209, number 1to 2, pp.270-276) describe.
Young's modulus is a kind of elastic modelling quantity, and is reveal in the flexible range of stress, according to the uniaxial strain that uniaxial stress measures at material list.The method for optimizing measuring Young's modulus E is according to equation E=2 ρ .C
t 2(1+ υ) measures via the cross stream component of the velocity of sound of material and longitudinal component, υ=(1 – 2 (C in equation
t/ C
l)
2)/(2 – 2 (C
t/ C
l)
2), wherein C
land C
tbe the longitudinal velocity of sound via material and transverse sound velocity that record respectively, ρ is the density of material.It is known in the art that the ultrasonic measurement vertical and horizontal velocity of sound can be used.If material is the compound of different materials, then can by the average Young's modulus of one of three formula estimation, namely following harmonic wave formula, geometric formula and mixing principle formula: E=1/ (f
1/ E
1+ f
2/ E
2)); E=E
1 f1+ E
1 f2; And E=f
1e
1+ f
2e
2; Wherein different materials is divided into two parts, its respective volume fraction is f
1and f
2, f
1and f
2and be 1.
As described herein, the interface between superhard material main body and substrate can be plane or nonplanar substantially.The example of non-planar interface design can refer to description and the explanation of Fig. 8-12c.
In embodiment described herein, when raised or sunken be described to be formed on substrate surface time, be interpreted as its be formed on the contrary ultra hard material layer on the surface that substrate interface surface interface is combined, and contrary feature is formed in substrate.In addition, it will be appreciated that as the negative of interface surface or reverse side are formed on the ultra hard material layer be combined with substrate interface, thus make two interfaces form laminating coupling.
As shown in the embodiment that Fig. 8 illustrates, cutting element 400 comprises the substrate 410 with ultra hard material layer 412, and ultra hard material layer 412 is formed in substrate 410.Be the interface surface 418 with ultra hard material layer 412 interface cohesion in one end of substrate 410, ultra hard material layer 412 is attached to substrate 410 in this interface surface.Substrate 410 is normally columniform, and has outer surface 420 and periphery top edge 422.In the embodiment depicted in fig. 8, interface surface 418 comprises multiple projection 424 of spatially separating and second or the inner basic array for annular of the radial projection 426 arranged in the first array 424, described protruding 424 with the first array setting being substantially annular, and separates with neighboring 422.
As shown in Fig. 8 and 9a-9d, in this embodiment, described projection 424,426 of spatially separating is arranged among two arrays, and described two arrays are arranged in basic two passages for annular of the vertical central axis of substrate 410.But the present invention is not limited to this geometry, because such as protruding 424,426 can with orderly other than ring type arranged in arrays in interface surface 418, or described projection can Arbitrary distribution thereon, instead of be circular substantially or other oldered array distributes.In addition, in the embodiment that projection is arranged with annular array, it can be oval or asymmetrical, or can depart from the vertical central axis of substrate 410.Equally, although illustrate that the projection 426 of local array is nearer than the vertical central axis with substrate with external array 424, in other embodiments, the projection 426 of local array can be nearer with vertical central axis.
Projection 426 in second array can the spatial radial between the projection 424 in the first array be alignd.Projection 424,426 and spatial intersecting arrangement, the projection in an array and the space overlap in next array.In interface surface, the described staggered or unjustified distribution of three-dimensional feature can help distribution compression and tensile stress, and/or reduces the magnitude of stress field, and/or stops crackle to increase by the uninterrupted passage preventing crackle from increasing.
As shown in Fig. 8 and 9a-9d, in these embodiments, making all or most of protruding 424,426 to be configured as makes all or most of convex surfaces substantially not parallel with the plane that the cutting surface 414 of superhard material 412 or the longitudinal axis of substrate extend through.Equally, in the embodiment shown in Fig. 8-10 and 12a-12c, the interface surface 418 between projection in space is uneven.This may be interpreted as, but is not limited to, and covers that these are uneven, change, irregular, rugged, uneven and/or rough one or more space with peak and groove.The effect of this set is considered to suppress the continual Crack Extension along interface surface 418 and the contact surface area increased between substrate 410 interface and ultra hard material layer 412 interface.In addition, think that the effect of this structure is that " elasticity " ripple upset in material is formed and the crackle at interface is turned to.In some embodiments, the recess making each protruding 424,426 these spaces be separated with adjacent protrusion or injustice can be uniform, and can be uneven in other embodiments.
Protruding 424,426 upper surfaces can with smooth curved maybe can have the upper surface of inclination.In some embodiments, the shape of protruding 424,426 can be slightly irregular quadrangle or taper, and the interface surface place more close to its projection is the widest.
In Fig. 8 and 9a-9d, protruding 424,426 in each basic array for annular/around separate substantially equably, and each protruding 424,426 there is identical size in given array.But as mentioned above, protruding 424,426 can be formed as any required form, and are spatially separated from each other by even or uneven mode, to change the stress field in interface surface 418.As shown in the embodiment of Fig. 8 and 9, the projection 424 in external array is larger than the projection in local array.But these relative sizes can conversely, or the projection 424,426 in two arrays can have approximately uniform size, or the mixing of different size.
In the embodiment of Fig. 8 and 9a-9d, the quantity of the projection 424 that external array comprises is twices of local array, such as, be 10 and 5 projections respectively.This allows cutting element 400 to have pseudo-axial symmetry, thus makes freely to arrange cutting members in the instrument not requiring specific direction to use or drill bit.Projection 424,426 is arranged and is configured as and makes it suppress one or more continuous passage, and along described continuous passage, crackle can be expanded through interface surface 418.Equally, in some embodiments, all or most of projection and/or the space between it not substantially perpendicular or parallel any surface that can put on any load of cutting element 400 in use expection, substantially not perpendicular or parallel in its any outer surface yet.
The setting of protruding 424,426 and shape and the space between it can affect the stress distribution in cutting element 400, and effect can be such as by stop or to be transferred through among protruding 424,426, around or on the crackle of stressed zone increase and improve the resistance to crack growth resistance of cutting element, specifically, the resistance that the crackle along interface surface 418 is increased is improved.
As shown in the embodiment of Figure 10, in the vertical central axis peripheral region of substrate 410, the degree of depth of superhard material can be the degree of depth substantially identical with the degree of depth of the superhard material around ultra hard material layer 412.This can make the volume of the superhard material being in use exposed to working surface and area significantly can not decline with wearing and tearing progress, thus improves the life-span of cutting element 400.When axial direction load, it also contributes to making cutting element 400 hardening.In addition, it also contributes to reducing or slotting between the basic elimination operating period possibility of wearing and tearing and being formed.
Figure 11 illustrates another embodiment of substrate 450 and interface surface 451.The interface surface 451 of substrate 450 comprises the projection 454 of multiple adjacent row, and each convex shape is pyramidal substantially, and adjoins along protruding 454 protruding surfaces 450 and one or more adjacent projection along side bottom it.In this embodiment, all or most of protruding 454 any surfaces not being basically parallel to the plane extended through by the longitudinal axis of the superhard material cutting face (not shown) or substrate 450 that are attached to it.Protruding 454 can be highly all identical, or some convexities other is highly higher.
(not shown) in other embodiments, only most of interface surface 418,451 can be covered by the projection 454 adjoined, instead of the whole interface surface 418,451 shown in Figure 11 cover by protruding 454, and any interface surface 418,451 between any protruding 454 or do not covered by protruding 454 can be uneven, as described in above with reference to Fig. 8-10.
Another embodiment of substrate shown in Figure 12 a-12c.This embodiment and the difference shown in Fig. 8-9d are, from the shape difference of the projection 424,426 that interface surface 418 extends, and lacking shown in number ratio Fig. 8 of external array protrusions 424.In the embodiment of Figure 12 a-12c, these projections 424,426 have the peripheral shape with one or more non-planar surfaces.
In one or more above-mentioned embodiment, the parts (features) of interface surface 418,451 can be overall formation, although described substrate is formed by using the mould of suitable shape to place the material granule forming substrate in the mold.Alternatively, interface surface 418,451 projection and plane surface or just can not carry out generative process after such as having generated substrate by conventional mechanical process time and produce.Similar process can be applied to ultra hard material layer 12, to produce the interface surface for the formation of the respective shapes of mating with substrate.
By such as conventional braze technique or by using conventional high-pressure and high-temperature technology to carry out sintering, ultra hard material layer 12 can be attached to substrate.
If from ultra hard material layer 12 partially or even wholly filtration catalizer material in following process, or carry out further high pressure-temperature sintering circuit, then can further improve the durability comprising the cutting product of substrate and ultra hard material layer that there is above-mentioned interface feature and/or alleviate elastic stress wave in it.Described filtering can be carried out while ultra hard material layer 12 is attached to substrate, or such as by being separated described ultra hard material layer 12 from substrate, and the ultra hard material layer 12 that filtering is separated.In the later case, after having carried out filtering, use such as soldering processes or by use high-pressure high-temperature technology again sinter and ultra hard material layer 12 can be attached to substrate again.
Although illustrate and described specific embodiment, be understood that and can have carried out variations and modifications.Such as present substrate described herein by the mode of illustrating.Be interpreted as except tungsten carbide substrate, superhard material can also be attached to other carbide substrate, as the substrate manufactured by the carbide of W, Ti, Mo, Nb, V, Hf, Ta and Cr.In addition, although the embodiment shown in Fig. 1-12c is described as comprising the PCD structure with sharp edge and angle in the drawings, embodiment can also comprise the PCD structure with round, oblique or Chamfer Edge or angle.This embodiment by improving the resistance of cutting element to the cracking at the interface through the substrate or ultra hard material layer with unique geometry, cracked and fracture, can reduce internal stress, and therefore extending working life.
In some embodiments, binder catalyst/solvent can comprise cobalt or some other iron family element, as iron or nickel or its alloy.The carbide of the group IV-VI metal in the periodic table of elements, nitride, boride and oxide are other examples of the non-diamond materials that be introduced in sintered mixture.In some embodiments, binder/catalyst/sintering aid can be Co.
Cemented metal carbide substrate can be conventional on composition, thus, can comprise any IVB race, VB race or group vib metal, and it is pressed and sinters under the existence of the adhesive of cobalt, nickel or iron or its alloy.In some embodiments, metal carbides are tungsten carbides.
In some embodiments, such as diamond and carbide material main body add that sintering aid/binder/catalyst is used in powder form, and sinter in single UHP/HT process simultaneously.The mixture of diamond crystals and a large amount of carbide is positioned in HP/HT reaction tank assembly, and carries out HP/HT process.The HP/HT treatment conditions selected are enough to the intergranular realized between the adjacent particle of abrasive grain and combine, and the combination of optional sintered particles and cemented metal carbide support.In one embodiment, these treatment conditions generally include and apply to be about 3-120 minute at least about the temperature of 1200 DEG C and the super-pressure that exceedes about 5GPa.
In another embodiment, in the sintering process of superhard polycrystalline material, can be, in HP/HT compacting, substrate was carried out presintering in a separate step before combining.
In yet another embodiment, substrate and polycrystalline superhard material main body all carry out preformed.Such as, the bimodulus charging of superhard crystal grain/particle with optional be also powder type carbonate adhesive-catalyst mix together with, and this mixture is packed into the tank (canister) of suitable shape, then in compacting, stand extremely high pressure and temperature.Typically, this pressure is at least 5GPa, and temperature is at least about 1200 DEG C.Then the preform of polycrystalline superhard material is positioned over the appropriate location on the upper surface of preformed carbide substrate (containing binder catalyst), and assembly is positioned in the tank of suitable shape.Then make assembly stand high temperature and high pressure in compacting, the amount grade of temperature and pressure is still respectively at least about 1200 DEG C and 5GPa.In the process, solvent/catalyst to move to superhard material main body from substrate and serves as adhesive-catalyst to realize the intergrowth in layer, and for polycrystalline superhard material layer is attached to substrate.Sintering process is also for being incorporated into substrate by superhard polycrystalline material body junction.
The much lower sintered-carbide grade of cobalt content is subject to following truth as the practical application of the substrate for PCD inserts and limits, and namely in sintering process, some Co need to enter PCD layer with the formation of catalysis PCD from substrate migration.It for this reason, the base material comprising lower Co content manufactures PCD more difficult, although may be desired.
An embodiment of superhard construction can obtain by the following method, comprise: cemented carbide substrate is provided, the surface contact of described substrate is assembled, substantially unconjugated a large amount of diamond particles is to form pre-sintered components, pre-sintered components is encapsulated in the sealed compartment (capsule) for super-pressure stove, this pre-sintered components is made to stand the pressure at least about 5.5GPa and the temperature at least about 1250 DEG C, and sintered diamond particles is to form PCD composite compact (composite compact) element, this element comprise to completely form in cemented carbide substrate and with the PCD structure of its combination.In some embodiments of the present invention, pre-sintered components can stand at least about 6GPa, at least about 6.5GPa, at least about 7GPa or even at least about the pressure of 7.5GPa or larger.
In yet another embodiment, substrate and polycrystalline superhard material main body all carry out preformed.Such as; the bimodulus of superhard crystal grain/particle or multimode charging with optional be also powder type carbonate adhesive-catalyst mix together with; and this mixture is packed in the tank (canister) of suitable shape with the form of alternating layer, then in compacting, stand extremely high pressure and temperature.Typically, this pressure is at least 5GPa, and temperature is at least about 1200 DEG C.Then the preform of polycrystalline superhard material is positioned over the appropriate location on the upper surface of preformed carbide substrate (containing binder catalyst), and assembly is positioned in the tank of suitable shape.Then make assembly stand high temperature and high pressure in compacting, the amount grade of temperature and pressure is still respectively at least about 1200 DEG C and 5GPa.In the process, solvent/catalyst to move to superhard material main body from substrate and serves as adhesive-catalyst to realize the intergrowth in layer, and for polycrystalline superhard material layer is attached to substrate.Sintering process is also for being incorporated into substrate by superhard polycrystalline material body junction.
Present description is for the manufacture of another illustrative methods of PCD element.The aggregation of the sheet form containing the diamond crystals combined by adhesive material can be provided.This tablet can be manufactured by method well known in the prior art; such as by squeeze casting method or doctor-blade casting process; in these methods; to the diamond crystals of each Size Distribution that has and be applicable to manufacturing required each bimodulus or multimode PCD grade be comprised and the slurry of adhesive material spreads out from the teeth outwards, and make it become dry.Also other method manufacturing diamantiferous tablet can be used, such as, at United States Patent (USP) the 5th, 766, No. 394 and the 6th, the method described in 446, No. 740.Alternative methods for depositing diamantiferous layer comprises spraying process, such as thermal spraying.Adhesive material can comprise water base organic bond, such as methylcellulose or polyethylene glycol (PEG), and can provide different tablets, and it comprises the diamond crystals with different size distribution, diamond content or additive.Such as, adamantine at least two tablets comprising and there is different average-size can be provided, and first and second groups of respective disks can be cut out from the first and second tablets.Tablet also can contain such as, for adamantine catalyst material, cobalt, and/or for suppressing the additive of diamond crystals misgrowth or strengthening PCD material character.Such as, tablet can containing have an appointment 0.5 to about 5 % by weight vanadium carbide, chromium carbide or tungsten carbide.In an example, each group can comprise an about 10-20 disk.
Can provide the supporting mass comprising sintered-carbide, in sintered-carbide, gummed material or adhesive material comprise such as, for adamantine catalyst material, cobalt.Supporting mass can have on-plane surface end or substantially flat near-end, and described end is formed PCD structure, and described end forms interface.The molded non-planar that can arrange end reduces the less desirable residual stress between PCD structure and supporting mass.Cup can be provided, for diamantiferous tablet is assemblied in supporting mass.First and second groups of disks can with the sequence stack replaced in the bottom of cup.In a scheme of the method, the diamond crystals that one deck loosens substantially can be filled on the highest point of disk.Then can adopt the mode first putting into near-end that supporting mass is inserted into cup, and towards substantially loose diamond crystals pushing supporting mass, thus they are moved a little, and according to the shape localization of the on-plane surface end of supporting mass they itself, form pre-sintered components.
This pre-sintered components can be positioned in sealed compartment and be used for super-pressure compacting, and stand the super-pressure at least about 5.5GPa and the high temperature at least about 1300 DEG C, also form the PCD element comprising the PCD structure being integrally connected to supporting mass with sintered diamond crystal grain.In a scheme of the method, when pre-sintered components super-pressure and high-temperature process, the adhesive material in supporting mass melts, and infiltrates the layer of diamond crystals.The existence of melting catalyst material in supporting mass can promote the sintering of diamond crystals, to form the PCD structure of overall layering by intergrowth each other.
In some schemes of the method, aggregation can comprise substantially loose diamond crystals, or the diamond crystals combined by adhesive material.The aggregation of multimode particle can be the form of granule, disk, wafer or tablet, can contain for adamantine catalyst material and/or such as reducing the excrescent additive of diamond crystals, or this aggregation can substantially containing catalyst material or additive.In some embodiments, this aggregation can be assembled on sintered-carbide supporting mass.
In some embodiments, this pre-sintered components can stand at least about 6GPa, at least about 6.5GPa, at least about 7GPa or even at least about 7.5GPa or even higher pressure.
The hardness of cemented tungsten carbide substrate by standing super-pressure especially by this substrate and high temperature strengthens under diamond is thermodynamically stable pressure and temperature.The amplitude that hardness strengthens can be depending on pressure and temperature condition.Particularly, pressure is higher, can increase the strengthening of hardness.When not wishing the constraint by particular theory, it is relevant that this is considered to enter PCD with Co in compacting sintering process from basement migrate, because the degree that hardness increases directly depends on the reduction of Co content in substrate.
In cemented carbide substrate containing enough for adamantine solvent/catalyst, and PCD structure is intactly formed in suprabasil embodiment in ultra-high pressure sintering process, solvent/catalyst material can be included in or be introduced in the aggregation from the diamond crystals of the material source being different from cemented carbide substrate.This solvent/catalyst material can comprise the cobalt only penetrated into before ultra-high pressure sintering step and in ultra-high pressure sintering process from substrate the aggregation of diamond crystals.But, in cobalt or the lower embodiment of other solvent/catalyst material content in the substrate, particularly when its lower than cemented carbide material about 11 % by weight time, then may need to provide interchangeable source to guarantee the good sintering of aggregation, to form PCD.
Can be incorporated in the aggregation of diamond crystals by various method for adamantine solvent/catalyst, comprise solvent/catalyst material and the diamond crystals of mixed-powder form, in the deposited on silicon solvent/catalyst material of diamond crystals, or the part before the sintering step or as sintering step enters aggregation from the material source penetrating solvent/catalyst material being different from substrate.The method deposited on the surface of diamond crystals as cobalt for adamantine solvent/catalyst be well known in the art, it comprises chemical vapour deposition (CVD) (CVD), physical vapour deposition (PVD) (PVD), sputter coating, electrochemical method, chemical coating method and ald (ALD).It should be understood that the merits and demerits of often kind of method depends on the character of sintering aid material and coated structure to be deposited, and the characteristic of particle.
In an embodiment of the inventive method, by following methods, cobalt is deposited on the surface of diamond crystals: first depositing precursor materials, then precursor material is converted into the material of containing element metallic cobalt.Such as, in a first step, following reaction can be used to be deposited on the surface of diamond crystals by cobalt carbonate:
Co(NO
3)
2+Na
2CO
3→CoCO
3+2NaNO
3
Can be realized by the method described in PCT patent publication No. WO2006/032982 for adamantine cobalt or the carbonate of other solvent/catalyst or the deposition of other precursor.Then such as by pyrolysis as described below, cobalt carbonate is converted into cobalt and water:
CoCO
3→CoO+CO
2
CoO+H
2→Co+H
2O
In another embodiment of the inventive method, the precursor of cobalt powder or cobalt, as cobalt carbonate, can mix with diamond crystals.When the precursor using solvent/catalyst as cobalt, material described in heat treatment may be necessary, with before sintering aggregation, carry out reacting the solvent/catalyst material with generting element form.
In some embodiments, cemented carbide substrate can be formed by the tungsten carbide particle combined by adhesive material, and this adhesive material comprises the alloy of Co, Ni and Cr.This tungsten carbide particle can form at least 70wt% and the 95wt% at the most of substrate.Adhesive material can comprise the Ni about between 10-50wt%, the Cr about between 0.1 to 10wt%, and all the other percentage by weights comprise Co.In some embodiments, the Size Distribution of the tungsten carbide particle in cemented carbide substrate has following characteristics:
-be less than the particle diameter of the carbide particle of 17% for being equal to or less than about 0.3 micron;
The particle diameter of the tungsten carbide particle of-Yue 20-28% is about 0.3-0.5 micron;
The particle diameter of the tungsten carbide particle of-Yue 42-56% is about 0.5-1 micron;
-the tungsten carbide particle that is less than about 12% is greater than 1 micron; And
The average grain diameter of-tungsten carbide particle is about 0.6 ± 0.2 micron.
In some embodiments, adhesive comprises the tungsten about between 2-20wt% and the carbon about between 0.1-2wt% in addition.
The basalis adjacent with the interface of polycrystalline diamond abrasive compact main body can have the thickness of such as about 100 microns, and can comprise tungsten carbide crystal grain and adhesive phase.The feature of this layer can be the following basic composition having and measured by energy dispersion X-ray microscopic analysis (EDX):
Cobalt between-Yue 0.5-2.0wt%;
Nickel between-Yue 0.05-0.5wt%;
Chromium between-Yue 0.05-0.2wt%; And
-tungsten and carbon.
In another embodiment, comprise in the above-mentioned layer of the cobalt about between 0.5-2.0wt%, the nickel about between 0.05-0.5wt% and the chromium about between 0.05-0.2wt% in basic composition, remainder is tungsten and carbon.
Basalis can comprise free carbon further.
The magnetic characteristic of cemented carbide material can be relevant with composition characteristic to important structure.The concentration being connected into the tungsten of the dissolving of ratio in the middle of indirect inspection adhesive for measuring the most conventional technology of carbon content in sintered-carbide: the carbon content of dissolving in adhesive is higher, then the tungsten concentration of dissolving in adhesive is lower.W content in adhesive can by measurement magnetic moment σ or magnetic saturation M
sdetermine, M
s=4 π σ, these values and W content have contrary relation (Roebuck (1996), " Magneticmoment (saturation) measurements on cemented carbide materials ", Int.J.Refractory Met., Vol.14, pp.419-424.).Following formula can be used for magnetic saturation M
sassociate with the concentration of W with C in adhesive:
M
s∝ [C]/[W] × wt%Co × 201.9, unit is μ T.m
3/ kg
Adhesive cobalt content in cemented carbide material measures by various methods well known in the art, comprise indirect method as the magnetic characteristic of cemented carbide material or more directly by the method for energy dispersion X-ray microscopic analysis (EDX), or the method for Chemical Leaching based on Co.
Carbide particle such as the average grain diameter of WC particle such as can by checking the optical microscope photograph of the cross section of the cemented carbide material main body of microphoto or the metallurgical preparation using SEM (SEM) to obtain, and application average linear intercept method (mean linear intercept) technology is determined.Alternatively, the average-size of WC particle is estimated indirectly by the magnetic coercive force measuring cemented carbide material, the mean free path of the particle in the middle of described magnetic coercive force instruction Co, uses simple formula well known in the art can calculate WC particle diameter by this magnetic coercive force.This formula has quantized the inverse relationship between the magnetic coercive force of the WC cemented carbide material of Co gelling and the mean free path of Co, thus determines average WC particle diameter.Magnetic coercive force and MFP have inverse relationship.
As used herein, composite " mean free path " (MFP) as sintered-carbide be gelling in adhesive material gathering carbide grain between the measuring of average distance.The mean free path feature of cemented carbide material can use the microphoto of the polished silicon wafer of this material to measure.Such as, this microphoto can have the magnifying power of about 1000 times.This MFP can be determined by the distance measured between each crosspoint that uniform grid is reached the standard grade and crystal boundary.Matrix (matrix) line segment Lm is sued for peace, and crystal grain line segment Lg is sued for peace.The mean matrix line segment length adopting diaxon is " mean free path ".The mixture of multiple distributions of tungsten carbide particles sized may cause the wide distribution of the MFP value for same matrix content.Below this is explained in more detail.
In Co adhesive, the concentration of W depends on C content.Such as, under low C content, W concentration is obviously higher.In the Co adhesive of WC (WC-Co) material of Co gelling, W concentration and C content can be determined by magnetic saturation angle value.The magnetic saturation 4 π σ of hard metal (cemented tungsten carbide is an one example) or magnetic moment σ is defined as magnetic moment or the magnetic saturation of per unit weight.The magnetic moment σ of pure Co is that cubic meter every kilogram (μ T.m is multiplied by 16.1 micro-teslas
3/ kg), and the saturation induction of pure Co, being also referred to as magnetic saturation 4 π σ, is 201.9 μ T.m
3/ kg.
In some embodiments, cemented carbide substrate can have at least about 100Oe and the average magnetic coercive force of maximum about 145Oe, and the magnetic moment of specific magnetic saturation degree is minimum about 89% to the most about 97% relative to pure Co.
MFP characteristic required in substrate can be realized by several method as known in the art.Such as, lower MFP value can realize by using lower metal binder content.The actual lower limit that cobalt is about 3wt% is applicable to sintered-carbide and conventional liquid phase sintering.Stand such as pressure in cemented carbide substrate to exceed in the super-pressure of about 5GPa and an embodiment of high temperature (such as exceeding about 1400 DEG C), the metal-to-metal adhesive of lower content can be realized as cobalt.Such as, when cobalt content is about 3wt% and the average-size of WC grain is about 0.5 micron, MFP will be about 0.1 micron, and when the average-size of WC grain is about 2 microns, MFP will be about 0.35 micron, and when the average-size of WC grain is about 3 microns, MFP will be about 0.7 micron.These average particle size particle size correspond to the pass the natural pulverizing process producing particle logarithm normal distribution and the single powder grade obtained.Higher matrix (adhesive) content can cause higher MFP value.
According to the details of powder-processed and mixing, change particle diameter by mixing different powder grade and change the full spectrum MFP value distributing and can realize for substrate.Explicit value must rule of thumb be determined.
In some embodiments, substrate comprises Co, Ni and Cr.
Adhesive material for substrate can comprise in solid solution at least about one or more in V, Ta, Ti, Mo, Zr, Nb and Hf of 0.1wt% to the highest about 5wt%.
In other embodiments, polycrystalline diamond (PCD) composite compact element can comprise at least about 0.01wt% and one or more in Re, Ru, Rh, Pd, Re, Os, Ir and Pt of maximum about 2wt%.
According to some embodiments, in corrosion test, recirculation rig (rig) produces lower than 2 × 10
-3g/cm
3the impact jet flow of liquid-solid slurry, under following test condition, polycrystalline structure can have the specific loss in weight: the temperature of 50 DEG C, the angle of shock of 45 °, the slurry flow velocity of 20m/s, the pH of 8.02, the duration of 3 hours, and the slurry composition in 1 cubic meter of water: 40kg bentonite; 2kg Na
2cO
3; 3kg carboxymethyl cellulose, 5 liters.
The sintered-carbide main body of some embodiments can be formed by providing the tungsten-carbide powder of average equivalent circular diameter (ECD) size in about 0.2 micron to about 0.6 micrometer range, ECD Size Distribution has further feature, and the carbide particle being namely less than 45% has the average-size being less than 0.3 micron; The carbide particle of 30% to 40% has at least 0.3 micron and the average-size of 0.5 micron at the most; The carbide particle of 18% to 25% has and is greater than 0.5 micron and the average-size of 1 micron at the most; The carbide particle being less than 3% has the average-size being greater than 1 micron.By tungsten-carbide powder with comprise Co, the adhesive material of Ni and Cr or chromium carbide grinds, and the total carbon equivalent be included in mixed-powder is such as relative to about 6% of tungsten carbide.Then by mixed-powder compacting to form green compact, green compact are carried out sinter to produce sintered-carbide main body.
Sintering green compact can sinter at least 65 minutes at the temperature of the highest 1440 DEG C and the time of maximum 85 minutes at such as at least 1400 DEG C.
In some embodiments, the total carbon equivalent (ETC) be included in cemented carbide material is about 6.12% relative to tungsten carbide.
In some embodiments, the feature of the Size Distribution of tungsten-carbide powder can be the standard deviation of 0.4 micron average ECD and 0.1 micron.
For assisting the heat endurance improving sintering structure, can be close to from polycrystal layer in the region of its exposed surface and removing catalysis material.Usually, this surface in the polycrystal layer side contrary with substrate, and will provide the working surface of polycrystalline diamond layer.The removal of catalysis material can use methods known in the art such as electrolytic etching, acidleach and evaporation technique to carry out.
Be explained in more detail embodiment of the present invention below with reference to the following example, these embodiments only provide by way of illustration, are not intended to limit the scope of the invention.
Embodiment 1
Ratio given according to the form below 1 prepares diamond powder mixture.
Table 1
| Grade 2 | Class 4 | Grade 12 | Grade 22 | Grade 30 |
| 10％ | 10％ | 45％ | 25％ | 10％ |
Then diamond dust is positioned in applicable HpHT container, adjacent with the tungsten carbide substrate with the adhesive component provided in table 2.And sinter at the temperature of the pressure of about 6.8GPa and about 1500 DEG C.
Table 2
| Cobalt (wt%) | Nickel (wt%) | Chromium (wt%) |
| 9.5-10 | 2.75-3.15 | 0.25-0.35 |
The PDC cutting members that Computer-Assisted Design, Manufacture And Test makes by above-mentioned attribute in cracked test.Result is in shown in Figure 13.This test by impacting the edge crumpling resistance testing sharp cutting members with the energy level of 5 joules, and repeats until 8 Secondary Shocks.As shown in figure 13, this test result that the level of statistically significant is verified is compared to the conventional PDC material of test, and the reference 1 namely shown in Figure 13 and reference 2, the embodiment of testing has higher edge crumpling resistance.
In order to test the integrality of the finished product PCD briquet formed according to above-described embodiment under shock loading, high energy being carried out to cutting members and two conventional cutting members of reference and falls test.Result in Figure 14 figure shown in.As seen from Figure 14, the cutting members of an embodiment shows the shock-resistant load obviously larger than the conventional PDC cutting members of carrying out same test (as shown in reference 1 and 2) under high energy.
About the test carried out above, the conventional PCD briquet/cutting members of the reference tested comprises reference 1 and 2, and it is at the fired under pressure of 5.5GPa, and is that the multimode mixture of the diamond crystals of about 10 microns is formed by average grain diameter.Multimode mixture is listed in following table 3.
Table 3
| Grade 2 | Class 4 | Class 6 | Grade 12 | Grade 22 | |
| Average grain diameter | 1.7 micron | 3.2 micron | 4.6 micron | 10.1 microns | 16.6 microns |
| Reference 1 and 2 | 5％ | 16％ | 7％ | 44％ | 28％ |
For reference 1 and 2, substrate is all the tungsten carbide substrate of the Co adhesive with 13wt%, and tungsten carbide particle diameter is mainly 1-4 micron.Before sintering, the magnetic characteristic of this substrate is:
Magnetic saturation (%): 11.5-12.5
Magnetic coercive force (κ A/m): 9.0-10.5
Difference between reference 1 and 2 is that non-planar interface designs.
Illustrated by Figure 13 and 14, although experiment test illustrates that the PDC cutting members of an embodiment has excellent crumpling resistance and resistance to impact, and as shown in the test result of Figure 15, the cutting members of an embodiment defines obviously longer durability and good penetration rate too, Figure 15 be an embodiment and five conventional reference cutting members pierce into the figure of the degree of depth relative to penetration rate.Once drill bit reaches " blunt condition (dull condition) ", illustrating that most of conventional cutting members lost efficacy to the observation of cutting members is because large degree polishes (wear flat), instead of due to (catastrophic failure) of serious failure.PDC cutting members due to embodiment is not that the repair cost therefore reusing this drill bit significantly reduces due to of serious failure and lost efficacy.Such as, such cutting members can rotate again and reuse in drill bit.
The test result of carrying out the cutting members example 1-5 tested is shown in Figure 15, and it is identical with reference to the reference 1 about the foregoing of Figure 13 and 14, but is arranged on by cutting members example 5 in the drill bit design being different from example 1-4, for this test purpose.
In polycrystalline diamond abrasive compact, independent diamond particles/crystal grain is attached on adjacent particle/crystal grain by Buddha's warrior attendant stone bridge or diamond neck (neck) to a considerable extent.This independent diamond particles/crystal grain keeps its uniformity (identity), or usually has different orientations.Average crystal grain/the particle size of these independent diamond crystals/particles can utilize image analysis technology to measure.SEM collects image and uses standard image analysis technology to analyze.From these images, representational diamond particles/grain size distribution can be extracted.
Usually, polycrystalline diamond abrasive compact main body will produce and be attached in cemented carbide substrate in HPHT process.In doing so, arrange adhesive phase and diamond particles, to make adhesive be uniformly distributed mutually and have small scale, this is favourable.
The homogeney of sintering structure or uniformity are defined by the statistical evaluation of the image collected in a large number.By using electron microscope easily the distribution of the distribution of adhesive phase with diamond phase to be distinguished, the distribution of adhesive phase then can be measured by the method similar with method disclosed in EP0974566.The method can carry out statistical evaluation to the average thickness of the adhesive phase of the line by microstructure drawn arbitrarily along several.To those skilled in the art, the measured value of this adhesive thickness is also referred to as " adhesive mean free path ".For entirety composition or binder content and the similar bi-material of average diamond particle diameter, the material that average thickness is less will be tending towards evenly, because this means the distribution at diamond " more the small scale " of middle adhesive mutually.In addition, the standard deviation of this measurement is less, and structure is more even.Large standard deviation shows that adhesive thickness alters a great deal in microstructure, and namely this structure uneven (even), extensively comprises different structure types.
Adhesive mean free path measured value and the standard deviation thereof of the various samples formed according to each embodiment is obtained below in the mode listed.Unless otherwise indicated herein, the mean free path size in PCD material main body refer to comprise PCD material main body surface on or it is by the cross section of this main body being measured and not carrying out the size of three-dimensional correction.Such as, obtain measured value by the graphical analysis carried out on a polished surface, and described data do not carry out Sa Ertekefu (Sltykov) correction herein.
In the mean value or other statistical parameter measured by graphical analysis of measuring amount, use multiple images of the different piece of surface or cross section (hereinafter referred to sample) to improve reliability and the accuracy of statistics.Can be such as 10 to 30 for measuring the picture number of a given amount or parameter.If the sample analyzed is uniform, the situation for PCD depends on magnifying power, can think that 10 to 20 width images represent this sample enough fully.
For will be clear that the object made from alternate boundary between particle, the resolution ratio of image needs enough high, for described measured value, employs the image area of 1280 × 960 pixels herein.The image for graphical analysis is obtained by the mode of the scanning electron micrograph (SEM) captured by use backscattered electron signal.Select backscatter mode to provide the high-contrast based on different atomicity, and reduce the susceptibility (compared with secondary electron imaging pattern) of effects on surface damage.
1. use EDM line to cut the exemplar of PCD sintered body and polishing.Use SEM with at least 10 width backscattered electron image of 1000 times of multiplication factor shooting sample surfaces.
2. original image is converted to gray level image.By guaranteeing that diamond peak intensity appears at the contrast level setting image between 10 to 20 in tonal gradation histogram.
3. automatic threshold characteristic is used for binary image, especially for the clear resolution ratio obtaining diamond and adhesive phase.
4. use from Soft Imaging
the software of the trade name analySIS Pro of GmbH (trade mark of Olympus Soft ImagingSolutions GmbH), and any particle getting rid of contact image border from analyze.This needs suitably to select image magnification ratio:
If a. too low, fine grain resolution ratio reduces.
If b. too Gao Ze:
I. the efficiency that coarse granule is separated reduces.
Ii. the coarse granule of high quantity is excised by the border of image, analyzes these less particles thus.
Iii must analyze more images thus to obtain the result having statistical significance.
5. the quantity of contiguous pixels that each particle is formed eventually through it represents.
6.AnalySIS software program carry out detect and analysis chart picture in each particle.This process is repeated automatically to multiple image.
7. use tonal gradation to analyze ten width SEM images, to determine the binder pool (binder pool) distinguished out with other in sample.Then by selecting only to identify binder pool and the maximum getting rid of the binder pool content of other phases all (no matter grey or white) determines the threshold value of SEM.Once determine this threshold value, this threshold value is used to carry out binaryzation SEM image.
8. be superimposed upon on the width of whole binary image by line thick for pixel, every root line at a distance of 5 pixels (having enough representativenesses to guarantee to measure) on angle of statistics.Be excluded mutually outside these are measured by the adhesive that image boundary is excised.
9. to measure and the analyzed material of distance-often kind recorded between the binder pool along superposition line at least carries out 10000 times measures.The mean value of record non-diamond phase average free path.
Also the standard deviation of adhesive mean free path measured value is recorded.
Determine thus, when the magnifying power of 1000 times, when diamond mutually in average grain diameter be less than or equal to 25 microns, the ratio of the standard deviation of the non-diamond phase average free path of embodiment and the mean value of non-Buddha's warrior attendant phase average free path is greater than 80%.
In some embodiments, the ratio of the standard deviation of non-diamond phase average free path and the mean value of non-Buddha's warrior attendant phase average free path is greater than 80%, but is less than 150%, and is be greater than 80% but be less than 120% in other embodiments.
Also have been found that the multimodal distribution of some embodiments can contribute to realizing the diamond intergrowth of very high level, still keep enough percent opening to allow effective leaching simultaneously.Equally, found that the combination of following elements in embodiment provides beyond thought additional advantage compared to any single composition:
1, average presintering particle diameter is approximately be less than or equal to the multimodal domain size distribution of 25 microns, to realize good wearability.
2, the tungsten carbide substrate of Ni and Cr is added with, to provide corrosion resistance.
3, the minimized interface of interfacial stress is made.
4, be greater than the sintering condition of 6GPa, for improve composite densified and sintering.
Although be described various embodiment with reference to some embodiments, but it will be appreciated by one of skill in the art that, can make various change for element wherein and can be replaced by equivalent, and these embodiments are not intended the specific embodiments disclosed in restriction.
Claims (74)
1. ultrahard polycrystalline structure, it comprises polycrystalline superhard material main body, and described polycrystalline superhard material main body is formed by following:
A large amount of superhard crystal grain, it demonstrates intergranular and combines and limit multiple gap area betwixt, and described superhard crystal grain has relevant mean free path;
Non-superhard phase, it fills multiple described gap area at least partly, and has relevant mean free path;
Wherein:
The average grain diameter of described superhard crystal grain is less than or equal to 25 microns; And
When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
2. ultrahard polycrystalline structure according to claim 1, wherein said superhard crystal grain comprises diamond crystals that is natural and/or synthesis, described ultrahard polycrystalline formation of structure polycrystalline diamond stone construction.
3. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, wherein saidly non-ly superhardly comprise adhesive phase mutually.
4. ultrahard polycrystalline structure according to claim 3, wherein said adhesive comprises cobalt mutually, and/or one or more other iron family elements are as iron or nickel or its alloy, and/or one or more carbide of group IV-VI metal, nitride, boride and oxide in the periodic table of elements.
5. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, comprise the cemented carbide substrate along interface cohesion to described polycrystalline material main body further.
6. ultrahard polycrystalline structure according to claim 5, wherein said cemented carbide substrate comprises the tungsten carbide particle combined by adhesive material, and described adhesive material comprises the alloy of Co, Ni and Cr.
7. ultrahard polycrystalline according to claim 6 structure, wherein said tungsten carbide particle forms at least 70wt% and the 95wt% at the most of described substrate; Described adhesive material comprises the Cr of Ni, about 0.1 to the 10wt% of about 10-50wt%, and all the other percentage by weights comprise Co; And the Size Distribution of tungsten carbide particle has following characteristics described in wherein said cemented carbide substrate:
The particle diameter being less than the described carbide particle of 17% is equal to or less than about 0.3 micron;
The particle diameter of the described tungsten carbide particle of about 20-28% is about 0.3-0.5 micron;
The particle diameter of the described tungsten carbide particle of about 42-56% is about 0.5-1 micron;
The described tungsten carbide particle being less than about 12% is greater than 1 micron; And
The average grain diameter of described tungsten carbide particle is about 0.6 ± 0.2 micron.
8. ultrahard polycrystalline structure according to claim 7, wherein said adhesive also comprises the tungsten of about 2-20wt% and the carbon of about 0.1-2wt%.
9. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, the average grain diameter of wherein said superhard crystal grain is about 8-20 micron.
10. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, wherein when the magnifying power image analysis technology with 1000 is measured, be less than 150% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
11. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, wherein when the magnifying power image analysis technology with 1000 is measured, be less than 120% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
12. construct according to ultrahard polycrystalline in any one of the preceding claims wherein, wherein said polycrystalline superhard material main body comprises first area and the second area adjacent with described first area, and described second area is bonded to described first area by the intergrowth of superhard material crystal grain; Described first area comprises multiple alternating layer, and the thickness range of every one deck is about 5-300 micron; Described second area comprises multiple layer, and the thickness of one or more layers in described second area is greater than the thickness of the single layer in described first area, wherein:
Alternating layer in described first area comprises ground floor, and itself and the second layer replace, and described ground floor is in residual compressive stress state, and the described second layer is in tensile residual stresses state; And
Described first or second area in one or more layers comprise:
A large amount of superhard crystal grain, it demonstrates intergranular and combines and limit multiple gap area betwixt; With
Non-superhard phase, it fills multiple described gap area at least partly, and has relevant mean free path; When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
13. ultrahard polycrystalline structures according to claim 12, the thickness range of each layer in wherein said first area is about 30-300 micron or about 30-200 micron.
14. according to claim 12 or 13 ultrahard polycrystalline structure, the thickness of the described layer in wherein said second area is for being greater than about 200 microns.
15. according to any one of claim 12-14 ultrahard polycrystalline structure, the described layer in wherein said first area comprises two or more different average diamond grain size.
16. according to any one of claim 1-11 ultrahard polycrystalline structure, wherein said polycrystalline superhard material main body comprises first area and the second area adjacent with described first area, and described second area is bonded to described first area by the intergrowth of diamond crystals; Described first area comprises multiple alternating layer, and the thickness range of each layer in described first area is about 5-300 micron; One or more layers in described first area and/or described second area comprise:
A large amount of superhard particles, it demonstrates intergranular and combines and limit multiple gap area betwixt; With
Non-superhard phase, it fills multiple described gap area at least partly, and has relevant mean free path; Wherein:
When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
17. according to any one of claim 12-16 ultrahard polycrystalline structure, wherein said first area comprises in use the outer working surface on the virgin work surface forming PCD structure.
18. according to claim 16 or 17 ultrahard polycrystalline structure, the thickness of wherein said second area is greater than the thickness of single layer in described first area.
19. according to any one of claim 16-18 ultrahard polycrystalline structure, wherein said second area comprises multiple layer.
20. according to any one of claim 16-19 ultrahard polycrystalline structure, wherein said alternating layer comprises ground floor, and itself and the second layer replace, and described ground floor is in residual compressive stress state, and the described second layer is in tensile residual stresses state.
21. ultrahard polycrystalline structures according to any one of claim 12-20, the layer in wherein said first area and/or described second area comprises following one or more:
Up to the Nano diamond additive of the Nano diamond powder granular form of 20wt%;
Salt system;
The boride of at least one in Ti, V or Nb or metal carbides; Or
At least one in metal Pd or Ni.
22. according to any one of claim 12-21 ultrahard polycrystalline structure, wherein PCD structure has longitudinal axis, and the layer in described first area and/or described second area is arranged in the substantially vertical plane of the plane that extends through with the longitudinal axis of described PCD structure.
23. ultrahard polycrystalline structures according to any one of claim 12-22, wherein said layer is plane, bending, arc or dome-shaped substantially.
24. according to any one of claim 12-21 ultrahard polycrystalline structure, wherein PCD structure has longitudinal axis, and the layer in described first area and/or described second area is arranged in the angled plane of the plane that extends through with the longitudinal axis of described PCD structure.
25. according to any one of claim 12-24 ultrahard polycrystalline structure, the volume of wherein said first area is greater than the volume of described second area.
26. ultrahard polycrystalline structures according to any one of claim 12-25, working surface or the side surface of layer described in wherein one or more and PCD structure are crossing.
27. according to any one of claim 12-26 ultrahard polycrystalline structure, one or more each PCD grade that wherein each layer is at least 1000MPa by TRS is formed; A PCD grade in adjacent layer or multiple PCD grade have different thermal coefficient of expansions (CTE).
28. ultrahard polycrystalline structures according to claim 27, it is at least 3 × 10 that wherein said one or more layer comprises CTE
-6a PCD grade of mm/ DEG C or multiple PCD grade.
29. ultrahard polycrystalline structures according to any one of claim 12-28, wherein said first area at least partially substantially not containing for adamantine catalyst material, described part forms thermally-stabilised region.
30. ultrahard polycrystalline structures according to claim 29, wherein said thermally-stabilised region extends the degree of depth of at least 50 microns by the surface of described PCD structure.
31. ultrahard polycrystalline structures according to claim 29 or 30, wherein said thermally-stabilised region comprise 2wt% at the most for adamantine catalyst material.
32., according to superhard construction in any one of the preceding claims wherein, also comprise:
Substrate, it comprises periphery and interface surface and longitudinal axis; Wherein said polycrystalline superhard material main body is formed on described substrate, and have exposure outer surface, from its extend outer surface and interface surface,
One of the interface surface of wherein said substrate or the interface surface of described polycrystalline superhard material main body comprise:
Multiple projection of spatially separating, it is arranged to protrude from described interface surface, and the described interface surface between described projection of spatially separating is uneven.
33. superhard construction according to claim 32, all or most of interface surface between wherein said projection of spatially separating is un-flexed, and extend in one or more plane, described plane is not parallel to the plane of the outer surface of the described exposure of described polycrystalline superhard material main body substantially.
34. superhard construction according to claim 32 or 33, wherein said substrate has vertical central axis, all or most of interface surface between wherein said projection of spatially separating extends in one or more plane, the plane that the vertical central axis that described plane is not parallel to described substrate substantially extends through.
35. superhard construction according to any one of claim 32-34, wherein said projection be radial array setting around the one or more of described substrate vertical central axis substantially.
36. superhard construction according to claim 35, wherein said projection is arranged by the first array and the second array, the radial location in described first array of described second array.
37. superhard construction according to claim 36, wherein said first and second arrays and described substrate essentially concentric.
38. superhard construction according to claim 36 or 37, the protruding quantity that wherein said first array comprises is the twice of described second array substantially.
39. superhard construction according to any one of claim 36-38, the projection in wherein said first and second arrays is interlaced with each other.
40. superhard construction according to any one of claim 32-34, wherein said projection is arranged in one of the interface surface of described substrate or the interface surface of described ultra hard material layer at random.
41. superhard construction according to any one of claim 32-40, wherein one or more surfaces of all or most of described projection are in the substantially uneven one or more plane of the plane of the exposed outer surface with described polycrystalline superhard material main body, and/or extend in the substantially uneven one or more plane of plane that the vertical central axis with described substrate extends through.
42. superhard construction according to any one of claim 32-41 are wherein substantially identical with the thickness of the polycrystalline superhard material main body at outer surface at the thickness of the longitudinal center of described substrate axial polycrystalline superhard material main body.
43. superhard construction according to any one of claim 32-42, the exposed outer surface of wherein said polycrystalline superhard material main body is plane substantially.
44. superhard construction according to any one of claim 32-43, wherein said projection has identical height.
45. superhard construction according to any one of claim 36-38, the height of the described projection in wherein said first array is greater than the height of the described projection in described second array.
46. superhard construction according to any one of claim 1-31, also comprise:
Substrate, it comprises periphery and interface surface and longitudinal axis; Wherein
Described polycrystalline superhard material main body is formed on described substrate, and have exposure outer surface, from its extend outer surface and interface surface;
One of the interface surface of wherein said substrate or the interface surface of described polycrystalline superhard material main body comprise:
Multiple projection, it is arranged to protrude from described interface surface, and on the surface having described projection to protrude, described projection adjoins along its edge and one or more adjacent projection, and extends in all or most of interface surface; And
Wherein one or more surfaces that are all or most of described projection extend in the substantially uneven one or more plane of the plane of the exposed outer surface with polycrystalline superhard material main body, and/or extend in the substantially uneven one or more plane of plane that the vertical central axis with described substrate extends through.
47. superhard construction according to claim 46, any interface surface that is wherein between any projection or that do not covered by described projection is uneven.
48. superhard construction according to claim 46 or 47, wherein said projection is pyramidal substantially.
49. superhard construction according to any one of claim 45-48, wherein said projection is arranged with orderly array in described interface surface.
50. superhard construction according to any one of claim 32-49, the described interface surface of wherein said substrate is the negative or reverse side of the interface surface of described polycrystalline superhard material main body, thus makes two interfaces form laminating coupling.
51. superhard construction according to any one of claim 32-50, wherein said superhard construction is cutting element.
52. earth's crust drill bits, comprise main body, described main body are provided with the superhard construction in any one of the preceding claims wherein as cutting element.
The method of the superhard construction of 53. formation according to any one of claim 1-51.
The method of 54. formation ultrahard polycrystalline structures, comprising:
There is provided a large amount of superhard material crystal grain, it comprises Part I and Part II, and described Part I has the first average-size, and described Part II has the second average-size,
Arrange described a large amount of superhard crystal grain, to form pre-sintered components; And
Under the hyperpressure of about 6GPa or larger and at the described superhard material temperature thermodynamically more stable than graphite, under the existence of the catalyst/solvent material for described superhard crystal grain, process described pre-sintered components, by grained sintered for described superhard material together to form polycrystalline superhard construction, described superhard crystal grain demonstrates intergranular knot and is incorporated in described intercrystalline and limits multiple gap area, and non-superhard phase fills multiple described gap area at least in part; Wherein said non-ly superhardly have relevant mean free path mutually; And
Wherein:
The average grain diameter of described superhard crystal grain is less than or equal to 25 microns; And
When the magnifying power image analysis technology with 1000 is measured, be more than or equal to 80% to the standard deviation of described non-superhard mutually relevant mean free path with the ratio of the mean value of described non-superhard relevant mean free path.
55. methods according to claim 55, the described step of a large amount of superhard material crystal grain is wherein provided to comprise the diamond crystals providing and have Part I and Part II in a large number, described Part I has the first average-size, described Part II has the second average-size, described Part I has the average grain diameter in about 10-60 micrometer range, and the average grain diameter of described Part II is less than the particle diameter of described thick part.
56. methods according to claim 54, wherein said Part II has the average grain diameter of about 1/10 to 6/10 of the particle diameter of described Part I.
57. methods according to any one of claim 54-56, the average grain diameter of wherein said Part I is about 10-60 micron, and the average grain diameter of described Part II is about 0.1-20 micron.
58. methods according to any one of claim 54-57, wherein said Part I is relative to the weight ratio of described Part II in the scope of about 50% to about 97%, and the weight ratio of described Part II is in the scope of about 3wt% to about 50wt%.
59. methods according to claim 58, wherein said Part I is about 60:40 for the ratio of the percentage by weight of described Part II.
60. methods according to claim 58, wherein said Part I is about 70:30 for the ratio of the percentage by weight of described Part II.
61. methods according to claim 58, wherein said Part I is about 90:10 for the ratio of the percentage by weight of described Part II.
62. methods according to claim 58, wherein said Part I is about 80:20 for the ratio of the percentage by weight of described Part II.
63. methods according to any one of claim 54-62, wherein providing the described step of a large amount of superhard material crystal grain to comprise provides the nonoverlapping crystal grain of domain size distribution of a large amount of described Part I and Part II.
64. methods according to any one of claim 54-63, wherein providing the described step of a large amount of superhard material crystal grain to comprise provides three kinds or more kind granularity pattern to form the multimodulus crystal grain comprising the particle diameter mixing with relevant average grain diameter.
65. methods according to any one of claim 54-64, it is an order of magnitude that the average grain diameter of wherein said part separates.
66. methods according to any one of claim 54-65, the superhard crystal grain of wherein said amount comprises the Part I with about 20 microns of average grain diameters, the Part II with about 2 microns of average grain diameters, has the Part III of about 200nm average grain diameter and have the Part IV of about 20nm average grain diameter.
67. 1 kinds of instruments, it comprises the ultrahard polycrystalline structure according to any one of claim 1-50, and described instrument is used for cutting, grinding, grinding, boring, earth's surface probing, rock-boring or other abrasive applications.
68. instruments according to claim 67, wherein said instrument comprises the drill bit for earth's surface probing or rock-boring.
69. instruments according to claim 67, cutting machine drill bit is fixed in the rotation that wherein said instrument comprises for oil and natural gas probing.
70. instruments according to claim 67, wherein said instrument is roller cone drill bits, drilling tool, bloat tool, drill or other earth's surface boring tool.
71. drill bit or cutting machine or its assemblies comprising the ultrahard polycrystalline structure according to any one of claim 1-50.
72. 1 kinds of ultrahard polycrystalline for earth's crust probing rotational shear drill bit or drill hammer construct, and comprise the ultrahard polycrystalline according to any one of claim 1-50 be combined with sintered-carbide supporting mass and construct.
The ultrahard polycrystalline structure of 73. 1 kinds of any one embodiments illustrated in the accompanying drawings of reference substantially as used in the description.
The manufacture method of the ultrahard polycrystalline structure of 74. 1 kinds of any one embodiments illustrated in the accompanying drawings of reference substantially as used in the description.
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| CN108698129A (en) * | 2016-01-01 | 2018-10-23 | 第六元素（英国）有限公司 | Superhard construction and its manufacturing method |
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| GB201215523D0 (en) * | 2012-08-31 | 2012-10-17 | Element Six Abrasives Sa | Polycrystalline diamond construction and method for making same |
| US9732563B1 (en) * | 2013-02-25 | 2017-08-15 | Us Synthetic Corporation | Polycrystalline diamond compacts including a cemented carbide substrate and applications therefor |
| US10030451B1 (en) | 2014-11-12 | 2018-07-24 | Us Synthetic Corporation | Polycrystalline diamond compacts including a cemented carbide substrate and applications therefor |
| WO2016085449A1 (en) | 2014-11-24 | 2016-06-02 | Halliburton Energy Services, Inc. | Determining the leaching profile of a cutter on a drilling tool |
| GB2554569A (en) | 2015-06-03 | 2018-04-04 | Halliburton Energy Services Inc | Electrochemical removal of metal or other material from polycrystalline diamond |
| US10492888B2 (en) | 2015-07-07 | 2019-12-03 | Align Technology, Inc. | Dental materials using thermoset polymers |
| US11761062B2 (en) | 2016-06-28 | 2023-09-19 | Schlumberger Technology Corporation | Polycrystalline diamond constructions |
| GB201622458D0 (en) * | 2016-12-31 | 2017-02-15 | Element Six Ltd | Superhard constructions & methods of making same |
| US10619422B2 (en) | 2017-02-16 | 2020-04-14 | Baker Hughes, A Ge Company, Llc | Cutting tables including rhenium-containing structures, and related cutting elements, earth-boring tools, and methods |
| GB201722310D0 (en) * | 2017-12-31 | 2018-02-14 | Element Six Uk Ltd | Polycrystalline diamond constructions |
| KR20210003915A (en) | 2018-05-04 | 2021-01-12 | 얼라인 테크널러지, 인크. | Curable composition for use in high temperature lithography-based photopolymerization process and method of preparing crosslinked polymer therefrom |
| WO2019219906A1 (en) * | 2018-05-18 | 2019-11-21 | Element Six (Uk) Limited | Polycrystalline diamond cutter element and earth boring tool |
| US20210237164A1 (en) * | 2018-06-19 | 2021-08-05 | Sumitomo Electric Hardmetal Corp. | Diamond joined body and method for manufacturing diamond joined body |
| GB201919480D0 (en) * | 2019-12-31 | 2020-02-12 | Element Six Uk Ltd | Polycrystalline diamond constructions & methods of making same |
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| CN101084168A (en) * | 2004-10-29 | 2007-12-05 | 六号元素（产品）（控股）公司 | Cubic boron nitride compact |
| CN101273151A (en) * | 2005-08-16 | 2008-09-24 | 六号元素（产品）（控股）公司 | Fine grained polycrystalline abrasive material |
| US20100300764A1 (en) * | 2009-06-02 | 2010-12-02 | Kaveshini Naidoo | Polycrystalline diamond |
| US20110024201A1 (en) * | 2009-07-31 | 2011-02-03 | Danny Eugene Scott | Polycrystalline diamond composite compact elements and tools incorporating same |
| US20110061944A1 (en) * | 2009-09-11 | 2011-03-17 | Danny Eugene Scott | Polycrystalline diamond composite compact |
| WO2011129422A1 (en) * | 2010-04-16 | 2011-10-20 | 株式会社タンガロイ | Coated sintered cbn |
| US20120186884A1 (en) * | 2011-01-20 | 2012-07-26 | Baker Hughes Incorporated | Polycrystalline compacts having differing regions therein, cutting elements and earth-boring tools including such compacts, and methods of forming such compacts |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108698129A (en) * | 2016-01-01 | 2018-10-23 | 第六元素（英国）有限公司 | Superhard construction and its manufacturing method |
| CN108698129B (en) * | 2016-01-01 | 2021-07-06 | 第六元素（英国）有限公司 | Superhard constructions and methods of making same |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2014020021A3 (en) | 2014-04-10 |
| WO2014020021A2 (en) | 2014-02-06 |
| US20150246427A1 (en) | 2015-09-03 |
| GB201213596D0 (en) | 2012-09-12 |
| GB201313571D0 (en) | 2013-09-11 |
| GB2506496A (en) | 2014-04-02 |
| US20170067294A1 (en) | 2017-03-09 |
| GB2506496B (en) | 2014-10-15 |
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