CN105349965A - Polycrystalline diamond compact and manufacturing method thereof - Google Patents
Polycrystalline diamond compact and manufacturing method thereof Download PDFInfo
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- CN105349965A CN105349965A CN201510734565.7A CN201510734565A CN105349965A CN 105349965 A CN105349965 A CN 105349965A CN 201510734565 A CN201510734565 A CN 201510734565A CN 105349965 A CN105349965 A CN 105349965A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/271—Diamond only using hot filaments
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Abstract
The invention provides a polycrystalline diamond compact and a manufacturing method thereof. The polycrystalline diamond compact comprises a cylindrical compact base body and a working end face. The compact base body comprises a hard alloy base layer and a polycrystalline diamond layer covering the upper surface of the hard alloy base layer. The working end face is located on the upper end face of the polycrystalline diamond layer and provided with multiple nanodiamond layers. Each nanodiamond layer comprises two nanocrystalline layers of different average grain sizes. The manufacturing method of the polycrystalline diamond compact includes the steps of firstly, compact base body manufacturing, secondly pretreatment, thirdly CVD film coating and fourthly nanodiamond layer surface polishing after which the compact is obtained. The outer layer of the compact is coated with the nanodiamond layers, the abrasion resistance, impact resistance and toughness of the polycrystalline diamond compact are improved, and the service life of the compact is prolonged; and the polycrystalline diamond compact manufactured through the method is good in abrasion resistance, high-temperature resistance and impact resistance.
Description
Technical field
The present invention is specifically related to a kind of polycrystalline diamond compacts (PDCs) and preparation method thereof.
Background technology
Polycrystalline diamond compacts (PDCs) (PolycrystallineDiamondCompact, lower abbreviation PDC composite sheet) a kind ofly covers by polycrystalline diamond layer the matrix material that cemented carbide substrate surfaces forms.It has had the high-wearing feature of polycrystalline diamond layer and the advantage such as toughness, weldability of Wimet concurrently, therefore becomes efficient cutting tool material and excellent high-abrasive material, and is widely used in oil and the field such as geological drilling and mechanical workout.
In actual applications, because the catalyzer of polycrystalline diamond compacts (PDCs) (PDC) is containing Co, Ni, Fe etc., the existence of Co makes composite sheet can not tolerate the high temperature of 700 DEG C at ambient pressure, and, Co is present in the interface of diamond DD key, Co is different with the adamantine coefficient of expansion, can produce thermal stresses, thus causes the stress damage of composite sheet.
At present, high-end composite sheet all improves wear resistance, the high thermal resistance of composite sheet by de-cobalt process, but de-cobalt process can only make the de-Co in surface, internal layer Co still exists, after certain wearing and tearing, new wearing surface occurs, the existence of Co still becomes the reason of the comprehensive mechanical performance reducing composite sheet.Studies have found that: after the polycrystalline diamond compacts (PDCs) containing Co is taken off Co process, composite sheet surface there will be a large amount of small holes, and then reduces the wear resistance of composite sheet.
Research is separately had to point out: with the PDC surface of chemical deposition (CVD) after de-Co or the millimetre-sized diamond thin of inside deposition or thick film, to form diamond nucleation, the wear resistance of composite sheet can be promoted.But the method still has the following disadvantages: namely because the Co of polycrystalline diamond compacts (PDCs) inside still exists, and CVD temperature is generally at 800 ~ 1000 DEG C, when temperature is higher than 400 DEG C, Co starts to expand between diamond crystals, Co volume becomes large, thermal stresses causes the distortional strain energy at itself and diamond contact position to increase, and occurs a large amount of thermal defects, cause degradation in polycrystalline diamond inside.
Also have research to point out: polycrystalline diamond compacts (PDCs) uses not containing the binding agent of Co, although eliminate the impact of remaining Co on the thermostability of polycrystalline diamond compacts (PDCs), this polycrystalline diamond compacts (PDCs) does not close for DD bond, and the wear resistance of composite sheet is deteriorated.
Summary of the invention
The object of the invention is to provide a kind of polycrystalline diamond compacts (PDCs), provides the preparation method of this polycrystalline diamond compacts (PDCs) to be second goal of the invention of the present invention simultaneously.
Based on above-mentioned purpose, the present invention adopts following technical scheme: a kind of polycrystalline diamond compacts (PDCs), comprise columned composite sheet matrix and operative end surface, described composite sheet matrix comprises the polycrystalline diamond layer of cemented carbide substrate and the covering of cemented carbide substrate upper surface, described operative end surface is positioned at the upper surface of polycrystalline diamond layer, described operative end surface is provided with multi-layer nano diamond layer, and every layer of Nano diamond layer comprises the different nano-crystalline layers of two-layer average grain size.
The side of described polycrystalline diamond layer or the side of composite sheet matrix are equipped with multi-layer nano diamond layer.
The average grain size of the two-layer nano-crystalline layers that every layer of Nano diamond layer comprises is respectively 20 ~ 40nm and 60 ~ 80nm; The thickness of every layer of nano-crystalline layers is 0.3 ~ 0.5 μm.Research finds, if when the crystalline size of crystal layer is larger, when reaching micron-sized crystalline size, fragility is comparatively large, and easily produces cleavage surface cleavage, and microcrystalline region easily cracks, and can not effectively stop crackle to arrive hard alloy substrate from crystal boundaries.
The total thickness of multi-layer nano diamond layer is 6 ~ 20 μm.
A preparation method for polycrystalline diamond compacts (PDCs), comprises the following steps:
(1) composite sheet matrix is prepared: described composite sheet matrix comprises the polycrystalline diamond layer of cemented carbide substrate and the covering of cemented carbide substrate upper surface, and the upper surface of described polycrystalline diamond layer is processed with operative end surface;
(2) pre-treatment: after composite sheet matrix surface finish, oil removing, cleaning and oven dry, through chloroazotic acid acidifying 2 ~ 5s or with sandblast machine to after its surface sand-blasting, then enter filming process after surface degreasing, cleaning, oven dry;
(3) CVD plated film: the composite sheet matrix after pre-treatment is placed on the chip bench of CVD heated filament Diamond Equipment, at the operative end surface deposit multilayer Nano diamond layer of composite sheet matrix, every layer of Nano diamond layer comprises the different nano-crystalline layers of two-layer average grain size;
(4) namely polycrystalline diamond compacts (PDCs) is obtained to Nano diamond layer surface finish process.
In step (3), while the operative end surface deposit multilayer Nano diamond layer to composite sheet matrix, to deposit multilayer Nano diamond layer on the side of polycrystalline diamond layer or the side of composite sheet matrix.
The concrete operations preparing composite sheet matrix are: by bortz powder and binding agent mixing, with hard aluminium alloy matrix at 5 ~ 5.5GPa, sinter 3 ~ 8min at 1400 ~ 1600 DEG C and obtain the composite sheet matrix blank that cemented carbide substrate upper surface is coated with polycrystalline diamond layer, composite sheet matrix blank is processed with the composite sheet matrix of operative end surface by the upper surface obtaining polycrystalline diamond layer after mill processing, precision work process; With volume percentage, described bortz powder is 45 ~ 90%, binding agent is 10 ~ 55%; Described binding agent is superhard refractory ceramics nitride material; Described bortz powder is by following volume parts preparation: 55 ~ 60 parts, 2 ~ 4 μm bortz powders, 30 ~ 40 parts, 6 ~ 8 μm bortz powders 5 ~ 20 parts.
Described binding agent is one or more combination of the nitride being arranged in the periodic table of chemical element IVB, VIB, IIIA, IVA element.
Described binding agent is the mixture of the three kinds or more in TiN, ZrN, CrN, AlN and SiN.
CVD plated film specifically comprises the following steps:
A) composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, is evacuated to 0.6 ~ 0.8Pa heated substrate temperature to 700 ~ 900 DEG C, passes into CH
4and H
2, vacuum tightness to 0.1 ~ 0.3Pa, composite sheet matrix surface forming core, passes into protection of inert gas, the air pressure 0.1 ~ 0.5Pa of rare gas element simultaneously;
B) adjust hot-wire temperature, the operative end surface of composite sheet matrix deposits the nano-crystalline layers that one deck 0.3 ~ 0.5 μm is thick, and the average grain size of this nano-crystalline layers is 20 ~ 40nm;
C) adjust hot-wire temperature, the nano-crystalline layers that previous step is formed deposits the thick nano-crystalline layers of one deck 0.3 ~ 0.5 μm again, and the average grain size of this nano-crystalline layers is 60 ~ 80nm;
D) repeating step b) and c) until plated film terminates.
Compared with the prior art, beneficial effect of the present invention is:
1) skin of composite sheet provided by the present invention is provided with multi-layer nano diamond layer, coordinates with cemented carbide substrate and polycrystalline diamond layer, improves the wear resistance of polycrystalline diamond compacts (PDCs) goods, and shock resistance and toughness extend the work-ing life of composite sheet;
2) multi-layer nano diamond layer of the present invention adopts the nano-crystalline layers of 20 ~ 40nm and 60 ~ 80nm, two kinds of different average grain sizes to replace arrangement to form, overall formation protective film, on the one hand, the mode of this alternately arrangement is adopted to be conducive to stopping the extension of crackle, make the crackle sponging part at the nano-crystalline layers place that grain-size is large, further increase shock resistance and the toughness of composite sheet; On the other hand, research finds, when crystalline size is comparatively large, when reaching micro-crystal, fragility is comparatively large, and easily produces cleavage surface cleavage, and microcrystalline region easily cracks, and can not effectively stop crackle to arrive matrix from crystal boundaries.Therefore the average grain size of nano-crystalline layers of the present invention controls in nano-scale range, the adamantine total surface area of settled layer increases, extraneous crackle is expanded along crystal boundary, the increase of diamond total surface area, delay the process that crackle is expanded to adamantine depths, therefore the shock resistance of composite sheet and the anti-coating shedding ability of stress effect also strengthen, and can greatly strengthen the life-span extending composite sheet;
In addition, multi-layer nano diamond layer is arranged alternately is convenient to coating, is also conducive to the thickness controlling the coating of multi-layer nano diamond layer, handled easily simultaneously;
Finally, after polished finish is carried out to the surperficial later stage of Nano diamond layer, the smooth finish on course of processing surface can be increased;
3) binding agent in the present invention in polycrystalline diamond adopts superhard high temperature resistant nitride material, has higher hardness, and can the pyroprocessing of resistance to CVD, makes the PDC composite sheet obtained not only have higher hardness, and can the pyroprocessing of resistance to CVD; In preparation process, after carrying out polished finish to outer field Nano diamond layer, the smooth finish on surface increases, and decreases the heat that drill bit and rock frictional test produce, thus delays the work-ing life of drill bit;
4) in the present invention, the raw material bortz powder of polycrystalline diamond layer is screened further, find that the effect reached when adopting the different diadust of particle diameter to carry out composite is best, namely, evade bulky diamond, adopt fine-grained diamond as the principal phase of different grain size proportioning, specific surface increases, active increase, promote the interfacial diffusion effect of diamond and solid phase bonding agent, increase the bonding strength of diamond and bonding agent, improve sintered density and the homogeneity of sintering reaction.
Accompanying drawing explanation
Fig. 1 is the structural representation of polycrystalline diamond compacts (PDCs) in embodiment 1;
Fig. 2 is the structural representation of polycrystalline diamond compacts (PDCs) in embodiment 2;
Fig. 3 is the structural representation of polycrystalline diamond compacts (PDCs) in embodiment 3;
Fig. 4 is the structural representation of Nano diamond layer in embodiment 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
embodiment 1
A kind of polycrystalline diamond compacts (PDCs), as shown in Figure 1 and Figure 4, comprise columned composite sheet matrix and operative end surface 3, composite sheet matrix comprises the polycrystalline diamond layer 2 of cemented carbide substrate 1 and the covering of cemented carbide substrate 1 upper surface, and cemented carbide substrate 1 and polycrystalline diamond layer 2 are sintered into one by High Temperature High Pressure; Operative end surface 3 is positioned at the upper surface of polycrystalline diamond layer 2, operative end surface 3 is coated with multi-layer nano diamond layer 4, and the total thickness of multi-layer nano diamond layer 4 is 6 μm.
Every layer of Nano diamond layer 4 comprises the nano-crystalline layers 5 of average grain size 20nm and the nano-crystalline layers 6 of average grain size 60nm.The thickness of every layer of nano-crystalline layers is 0.3um.
Its preparation method, comprises the following steps:
(1) preparation of composite sheet matrix: bortz powder and binding agent are mixed (before mixing with bortz powder, first binding agent is mixed), with hard aluminium alloy matrix at 5.5GPa, sinter 3min at 1600 DEG C and obtain composite sheet matrix blank, by composite sheet matrix blank by mill processing, the composite sheet matrix blank that cemented carbide substrate upper surface is coated with polycrystalline diamond layer is obtained after precision work process, with volume percentage, bortz powder 45%, binding agent 55%, described binding agent is the mixture of CrN, AlN and SiN tri-kinds; Described bortz powder is by following volume parts preparation: 0.5 ~ 1 μm of bortz powder, 50 parts, 2 ~ 4 μm bortz powders, 30 parts, 6 ~ 8 μm bortz powders 20 parts.
(2) pre-treatment: after composite sheet matrix surface finish, oil removing, cleaning and oven dry, with sandblast machine to after its surface sand-blasting, then enters filming process after surface degreasing, cleaning, oven dry;
(3) CVD plated film: composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, at the operative end surface deposit multilayer Nano diamond layer of composite sheet matrix, every layer of Nano diamond layer is made up of the nano-crystalline layers that two-layer average grain size is different;
(4) namely polycrystalline diamond compacts (PDCs) is obtained to Nano diamond layer surface finish process.
Wherein CVD plated film concrete steps are:
A) composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, is evacuated to 0.8Pa heated substrate temperature to 900 DEG C, passes into CH
4, H
2, vacuum tightness to 0.3Pa, composite sheet matrix surface forming core, pass into protection of inert gas, the air pressure 0.5Pa of rare gas element, described rare gas element is Kr simultaneously;
B) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.3 μm in the operative end surface of composite sheet matrix, the average grain size of this nano-crystalline layers controls as 20nm;
C) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.3 μm in the operative end surface of composite sheet matrix, the average grain size of this nano-crystalline layers controls as 60nm;
D) step b) and c) be one deck Nano diamond layer, repeating step b) and c) until plated film terminates, its total thickness is 6 μm.
embodiment 2
As shown in Figure 2, in the present embodiment, multi-layer nano diamond layer is coated with in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer, the total thickness of multi-layer nano diamond layer 4 is 16 μm, and every layer of Nano diamond layer 4 comprises the two-layer nano-crystalline layers that average grain size is respectively 40nm and 60nm.The thickness of every layer of nano-crystalline layers is 0.4um.All the other are with embodiment 1.
Its preparation method, comprises the following steps:
(1) preparation of composite sheet matrix: by bortz powder and binding agent mixing, with hard aluminium alloy matrix at 5.5GPa, sinter 8min at 1400 DEG C and obtain composite sheet matrix blank, by composite sheet matrix blank by mill processing, the composite sheet matrix blank that cemented carbide substrate upper surface is coated with polycrystalline diamond layer is obtained after precision work process, by composite sheet matrix blank by mill processing, the upper surface obtaining polycrystalline diamond layer after precision work process is processed with the composite sheet matrix of operative end surface; With volume percentage, bortz powder 70%, binding agent 30%, described binding agent is the mixture of TiN, ZrN and CrN tri-kinds; Described bortz powder is by following volume parts preparation: 0.5 ~ 1 μm of bortz powder, 60 parts, 2 ~ 4 μm bortz powders, 30 parts, 6 ~ 8 μm bortz powders 10 parts.
(2) pre-treatment: after composite sheet matrix surface finish, oil removing, cleaning and oven dry, through chloroazotic acid acidifying 2s, then enters filming process after surface degreasing, cleaning, oven dry;
(3) CVD plated film: composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, at operative end surface and the polycrystalline diamond layer side deposit multilayer Nano diamond layer of composite sheet matrix, every layer of Nano diamond layer is made up of the nano-crystalline layers that two-layer average grain size is different;
(4) namely polycrystalline diamond compacts (PDCs) is obtained to Nano diamond layer surface finish process.
Wherein CVD plated film specifically comprises the following steps:
A) PDC composite sheet is placed on the chip bench of CVD heated filament Diamond Equipment, is evacuated to 0.8Pa heated substrate temperature to 700 DEG C, passes into CH
4, H
2, vacuum tightness to 0.1Pa, composite sheet surface forming core, pass into protection of inert gas, the air pressure 0.1Pa of rare gas element, described rare gas element is Ar simultaneously;
B) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.4 μm in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer, the average grain size of this nano-crystalline layers controls as 40nm;
C) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.4 μm in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer, the average grain size of this nano-crystalline layers controls as 60nm;
D) step b) and c) be one deck Nano diamond layer, repeating step b) and c) until plated film terminates, its total thickness is 16 μm.
embodiment 3
In the present embodiment, as shown in Figure 3, be coated with multi-layer nano diamond layer 4 in the operative end surface of polycrystalline diamond layer and the side of composite sheet matrix, the total thickness of multi-layer nano diamond layer 4 is 20 μm.Every layer of Nano diamond layer 4 comprises the two-layer nano-crystalline layers that average grain size is respectively 40nm and 80nm.All the other are with embodiment 1.
Its preparation method, comprises the following steps:
(1) preparation of composite sheet: by bortz powder and binding agent mixing, with hard aluminium alloy matrix at 5.5GPa, sinter 6min at 1550 DEG C and obtain composite sheet matrix blank, by composite sheet matrix blank by mill processing, the composite sheet matrix blank that cemented carbide substrate upper surface is coated with polycrystalline diamond layer is obtained after precision work process, by composite sheet matrix blank by mill processing, the upper surface obtaining polycrystalline diamond layer after precision work process is processed with operative end surface composite sheet matrix; With volume percentage, bortz powder 90%, binding agent 10%, described binding agent is the mixture of ZrN, CrN and AlN tri-kinds; Described bortz powder is by following volume parts preparation: 0.5 ~ 1 μm of bortz powder, 55 parts, 2 ~ 4 μm bortz powders, 40 parts, 6 ~ 8 μm bortz powders 5 parts.
(2) pre-treatment: after composite sheet matrix surface finish, oil removing, cleaning and oven dry, through chloroazotic acid acidifying 5s, then enters filming process after surface degreasing, cleaning, oven dry;
(3) CVD plated film: composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, at operative end surface and the composite sheet matrix side deposit multilayer Nano diamond layer of composite sheet matrix, every layer of Nano diamond layer is made up of the nano-crystalline layers that two-layer average grain size is different;
(4) namely polycrystalline diamond compacts (PDCs) is obtained to Nano diamond layer surface finish process.
Wherein CVD plated film specifically comprises the following steps:
A) composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, is evacuated to 0.7Pa heated substrate temperature to 800 DEG C, passes into CH
4, H
2, vacuum tightness to 0.2Pa, composite sheet matrix surface forming core, pass into protection of inert gas, the air pressure 0.1 ~ 0.5Pa of rare gas element, described rare gas element is Ar simultaneously;
B) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.5 μm in the operative end surface of composite sheet matrix and composite sheet matrix side, the average grain size of this nano-crystalline layers controls as 40nm;
C) adjust hot-wire temperature, deposit the thick nano-crystalline layers of one deck 0.5 μm in the operative end surface of composite sheet matrix and composite sheet matrix side, the average grain size of this nano-crystalline layers controls as 80nm;
D) step b) and c) be one deck Nano diamond layer, repeating step b) and c) until plated film terminates, its total thickness is 20 μm.
comparative example A:
Non-coating composite sheet A in this comparative example, uncoated in operative end surface have Nano diamond layer, and other are with embodiment 1.
Its preparation method, with reference to the preparation of step (1) composite sheet in embodiment 1.
comparative example B:
Non-coating composite sheet B in this comparative example, uncoated on the side of operative end surface and polycrystalline diamond layer have Nano diamond layer, and other are with embodiment 1.
Its preparation method, with reference to the preparation of step (1) composite sheet in embodiment 2.
comparative example C:
Non-coating composite sheet C in this comparative example, operative end surface has Nano diamond layer with the side of composite sheet matrix is uncoated, and other are with embodiment 1.
Its preparation method, with reference to the preparation of step (1) composite sheet in embodiment 3.
performance test
Carry out hardness test (adopt normal industry to test, Vickers hardness tester carries out diamond penetrator impression test), wear resistance ratio test and high temperature resistant test to the composite sheet that embodiment 1-3 and comparative example A, B, C obtain, it the results are shown in Table shown in 1.
Wherein, high temperature resistant testing method is: testing sample is put into retort furnace, air atmosphere, can be incubated 10-15min, not be oxidized after testing.
The test result of the composite sheet of table 1 embodiment 1-3 and comparative example A, B, C
As can be drawn from Table 1, compared with non-coating composite sheet, composite sheet (embodiment 1-3) overall performance (hardness and wear resistance ratio) after coating is improved, and thermotolerance and heat resisting temperature are all greatly improved, wherein embodiment 2 and 3 is suitable, all high than embodiment 1.
In addition, the performance that each performance of embodiment 2 and 3 is better than embodiment 1, comparative example B and C is better than comparative example A, adopts Vickers hardness tester to measure when this is hardness test, and pressure head is comparatively large, and hardness value is larger by the impact of matrix; Namely hardness value is subject to the result that in polycrystalline diamond, adamantine content influence is larger.In addition wear resistance ratio and hardness value proportional, hardness value is larger, and wear resistance ratio is larger.
thickness test and bonding force test
Respectively to embodiment 1-3 obtain composite sheet carry out thickness test and bonding force test, concrete grammar and result as follows:
1 thickness test: carry out ball hole instrument to it and measure thickness, record thickness average, concrete test result is shown in Table 2.
2 bonding force tests: carry out sandblasting test with dry blasting machine: SiC abrasive material, granularity, at 120 microns, carries out the test of sandblasting bonding force, 15S spray falls 5 microns for qualified.According to this criterion validation, the time that the diamond coatings sandblasting in the identical operative end surface region of composite sheet of Statistics Implementation example 1-3 is fallen, as shown in table 2.
The thickness of the composite sheet of table 2 embodiment 1-3 and bonding force test result
Learnt by upper table 2, the thickness of the composite sheet of embodiment 1-3 and bonding force are all qualified, reach service requirements.
Claims (10)
1. a polycrystalline diamond compacts (PDCs), comprise columned composite sheet matrix and operative end surface, described composite sheet matrix comprises the polycrystalline diamond layer of cemented carbide substrate and the covering of cemented carbide substrate upper surface, described operative end surface is positioned at the upper surface of polycrystalline diamond layer, it is characterized in that, described operative end surface is provided with multi-layer nano diamond layer, and every layer of Nano diamond layer comprises the different nano-crystalline layers of two-layer average grain size.
2. a kind of polycrystalline diamond compacts (PDCs) as claimed in claim 1, is characterized in that, the side of described polycrystalline diamond layer or the side of composite sheet matrix are equipped with multi-layer nano diamond layer.
3. a kind of polycrystalline diamond compacts (PDCs) as claimed in claim 1 or 2, is characterized in that, the average grain size of the two-layer nano-crystalline layers that every layer of Nano diamond layer comprises is respectively 20 ~ 40nm and 60 ~ 80nm; The thickness of every layer of nano-crystalline layers is 0.3 ~ 0.5um.
4. a kind of polycrystalline diamond compacts (PDCs) as claimed in claim 3, is characterized in that, the total thickness of multi-layer nano diamond layer is 6 ~ 20 μm.
5. a preparation method for polycrystalline diamond compacts (PDCs), is characterized in that, comprises the following steps:
(1) composite sheet matrix is prepared: described composite sheet matrix comprises the polycrystalline diamond layer of cemented carbide substrate and the covering of cemented carbide substrate upper surface, and the upper surface of described polycrystalline diamond layer is processed with operative end surface;
(2) pre-treatment: after composite sheet matrix surface finish, oil removing, cleaning and oven dry, through chloroazotic acid acidifying 2 ~ 5s or with sandblast machine to after its surface sand-blasting, then enter filming process after surface degreasing, cleaning, oven dry;
(3) CVD plated film: the composite sheet matrix after pre-treatment is placed on the chip bench of CVD heated filament Diamond Equipment, at the operative end surface deposit multilayer Nano diamond layer of composite sheet matrix, every layer of Nano diamond layer comprises the different nano-crystalline layers of two-layer average grain size;
(4) namely polycrystalline diamond compacts (PDCs) is obtained to Nano diamond layer surface finish process.
6. the preparation method of polycrystalline diamond compacts (PDCs) as claimed in claim 5, it is characterized in that, in step (3), while the operative end surface deposit multilayer Nano diamond layer to composite sheet matrix, to deposit multilayer Nano diamond layer on the side of polycrystalline diamond layer or the side of composite sheet matrix.
7. the preparation method of the polycrystalline diamond compacts (PDCs) as described in claim 5 or 6, it is characterized in that, the concrete operations preparing composite sheet matrix are: by bortz powder and binding agent mixing, with hard aluminium alloy matrix at 5 ~ 5.5GPa, sinter 3 ~ 8min at 1400 ~ 1600 DEG C and obtain the composite sheet matrix blank that cemented carbide substrate upper surface is coated with polycrystalline diamond layer, composite sheet matrix blank is processed with the composite sheet matrix of operative end surface by the upper surface obtaining polycrystalline diamond layer after mill processing, precision work process; With volume percentage, described bortz powder is 45 ~ 90%, binding agent is 10 ~ 55%; Described binding agent is superhard refractory ceramics nitride material; Described bortz powder is by following volume parts preparation: 0.5 ~ 1 μm of bortz powder, 55 ~ 60 parts, 2 ~ 4 μm bortz powders, 30 ~ 40 parts, 6 ~ 8 μm bortz powders 5 ~ 20 parts.
8. the preparation method of polycrystalline diamond compacts (PDCs) as claimed in claim 7, it is characterized in that, described binding agent is one or more combination of the nitride being arranged in the periodic table of chemical element IVB, VIB, IIIA, IVA element.
9. the preparation method of polycrystalline diamond compacts (PDCs) as claimed in claim 8, it is characterized in that, described binding agent is the mixture of the three kinds or more in TiN, ZrN, CrN, AlN and SiN.
10. the preparation method of the polycrystalline diamond compacts (PDCs) as described in claim 5 or 6 or 8 or 9, it is characterized in that, CVD plated film specifically comprises the following steps:
A) composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipment, is evacuated to 0.6 ~ 0.8Pa heated substrate temperature to 700 ~ 900 DEG C, passes into CH
4and H
2, vacuum tightness to 0.1 ~ 0.3Pa, composite sheet matrix surface forming core, passes into protection of inert gas, the air pressure 0.1 ~ 0.5Pa of rare gas element simultaneously;
B) adjust hot-wire temperature, the operative end surface of composite sheet matrix deposits the nano-crystalline layers that one deck 0.3 ~ 0.5 μm is thick, and the average grain size of this nano-crystalline layers is 20 ~ 40nm;
C) adjust hot-wire temperature, the nano-crystalline layers that previous step is formed deposits the thick nano-crystalline layers of one deck 0.3 ~ 0.5 μm again, and the average grain size of this nano-crystalline layers is 60 ~ 80nm;
D) repeating step b) and c) until plated film terminates.
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| CN105665806A (en) * | 2016-04-26 | 2016-06-15 | 深圳市力博刀具技术有限公司 | PCD (polycrystalline diamond) milling cutter and machining method therefor |
| WO2018162321A1 (en) * | 2017-03-06 | 2018-09-13 | Audi Ag | Cutting element for a machining tool and method for producing such a cutting element |
| CN109128192A (en) * | 2017-06-28 | 2019-01-04 | 深圳先进技术研究院 | Composite polycrystal-diamond and preparation method thereof |
| CN109848761A (en) * | 2019-01-18 | 2019-06-07 | 株洲金佰利硬质合金有限公司 | A kind of carbide surface treatment process |
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