CN110090960A - A kind of preparation method and product of the uniform composite polycrystal-diamond of microstructure - Google Patents
A kind of preparation method and product of the uniform composite polycrystal-diamond of microstructure Download PDFInfo
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- CN110090960A CN110090960A CN201910459388.4A CN201910459388A CN110090960A CN 110090960 A CN110090960 A CN 110090960A CN 201910459388 A CN201910459388 A CN 201910459388A CN 110090960 A CN110090960 A CN 110090960A
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- high temperature
- pressure
- pressure sintering
- sintering processes
- diamond
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- 239000010432 diamond Substances 0.000 title claims abstract description 78
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 106
- 238000000034 method Methods 0.000 claims abstract description 82
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000003595 mist Substances 0.000 claims description 2
- 239000011435 rock Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 230000032798 delamination Effects 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
Classifications
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
Abstract
The invention belongs to super-hard compound material technical fields, more particularly to a kind of preparation method and product of the uniform composite polycrystal-diamond of microstructure, the method includes to assembly diadust in hard alloy substrate and the high temperature and pressure sintering step after the completion of catalyst, the high temperature and pressure sintering step includes the high temperature and pressure sintering processes at least two stages sequentially carried out, and the temperature of each high temperature and pressure sintering processes sequentially increases, pressure is identical or sequentially increases.The sequentially progress that the present invention passes through multiple high temperature and pressure sintering processes, solve the problems, such as that composite polycrystal-diamond interfacial catalysis agent eruption type permeates the part to be formed and reunites, to increase substantially thermal stability, impact resistance of composite sheet etc., so improve composite sheet in use anti-collapse, delamination effect.
Description
Technical field
The invention belongs to super-hard compound material technical field more particularly to a kind of uniform polycrystalline diamond of microstructure are multiple
Close the preparation method and product of piece.
Background technique
Composite polycrystal-diamond be under high temperature and pressure (HTHP) environment, it is mutual with hard alloy substrate by diamond layer
It is sintered a kind of composite material formed, is applied to the wear-resisting cutting element of the boring tools such as petroleum, natural gas.However, traditional
The high-temperature high-pressure craft of single treatment, catalyst melting and increasing fast in hard alloy substrate, and then cause to be catalyzed in matrix
Agent eruption type penetrates into polycrystalline diamond layer, causes the presence of the catalyst or other matrixes locally reunited in polycrystalline diamond layer
Ingredient.Local catalyst or other matrix compositions substantially reduce the thermal stability of composite sheet, anti-impact in above-mentioned polycrystalline diamond layer
Hitting property etc., so that the problem of serious failure such as disintegrating tablet, delamination occurs in use for composite sheet.
Summary of the invention
The object of the present invention is to provide the preparation method and product of a kind of uniform composite polycrystal-diamond of microstructure,
The present invention solves composite polycrystal-diamond interfacial catalysis agent eruption type by the sequentially progress of multiple high temperature and pressure sintering processes
To increase substantially the thermal stability of composite sheet, impact resistance etc., and then improve multiple the problem of part that infiltration is formed is reunited
Close piece in use anti-collapse, delamination effect.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of preparation method of the uniform composite polycrystal-diamond of microstructure, including to assembling Buddha's warrior attendant in hard alloy substrate
High temperature and pressure sintering step after the completion of stone micro mist and catalyst, the high temperature and pressure sintering step include sequentially carrying out at least
The high temperature and pressure sintering processes in two stages, and the temperature of each high temperature and pressure sintering processes sequentially increases, pressure is identical or suitable
Secondary raising.
Preferably, the high temperature and pressure sintering step includes the first stage high temperature and pressure sintering processes sequentially carried out and
Two-stage high temperature and pressure sintering processes, under the conditions of two-stage processing has uniform pressure, first stage high temperature and pressure sintering processes
After, the catalyst quality accounting in polycrystalline diamond layer is at least 5 %；Second stage high temperature and pressure sintering processes terminate
Afterwards, the catalyst quality accounting in polycrystalline diamond layer is at least 10%.
Preferably, the temperature of the first stage high temperature and pressure sintering processes be 1450 DEG C, pressure be 9.0 GPa, second
The temperature of stage high temperature and pressure sintering processes is 1550 DEG C, and pressure is 9.0 GPa.
Preferably, the high temperature and pressure sintering step includes the first stage high temperature and pressure sintering processes sequentially carried out and
Two-stage high temperature and pressure sintering processes, after first stage high temperature and pressure sintering processes, the catalyst in polycrystalline diamond layer
Quality accounting is at least 10%；After second stage high temperature and pressure sintering processes, the catalyst quality in polycrystalline diamond layer is accounted for
Than being at least 15%.
Preferably, the temperature of the first stage high temperature and pressure sintering processes is 1420 DEG C, pressure 8.0GPa, second-order
The temperature of section high temperature and pressure sintering processes is 1550 DEG C, pressure 9.2GPa.
Preferably, the high temperature and pressure sintering step includes the first stage sequentially carried out, second stage and phase III
High temperature and pressure sintering processes, under the conditions of three-phase process has uniform pressure, after first stage high temperature and pressure sintering processes,
Catalyst quality accounting in polycrystalline diamond layer is at least 4%；After second stage high temperature and pressure sintering processes, plycrystalline diamond gold
Catalyst quality accounting in hard rock layer is at least 6%；After phase III high temperature and pressure sintering processes, polycrystalline diamond layer
In catalyst quality accounting be at least 10%.
Preferably, the temperature of the first stage high temperature and pressure sintering processes is 1400 DEG C, pressure 9.0GPa, second-order
The temperature of section high temperature and pressure sintering processes is 1480 DEG C, pressure 9.0GPa；The temperature of phase III high temperature and pressure sintering processes
It is 1550 DEG C, pressure 9.0GPa.
Preferably, the high temperature and pressure sintering step includes the first stage sequentially carried out, second stage and phase III
High temperature and pressure sintering processes, under the conditions of the pressure of the high temperature and pressure sintering processes of three phases sequentially increases, first stage high temperature
High-pressure sinter after treatment, the catalyst quality accounting in polycrystalline diamond layer are at least 5%；Second stage high temperature and pressure is burnt
After treatment is tied, the catalyst quality accounting in polycrystalline diamond layer is at least 8%；Phase III high temperature and pressure sintering processes
After, the catalyst quality accounting in polycrystalline diamond layer is at least 12%.
Preferably, the temperature of the first stage high temperature and pressure sintering processes is 1365 DEG C, pressure 7.6GPa, second-order
The temperature of section high temperature and pressure sintering processes is 1450 DEG C, pressure 8.5GPa；The temperature of phase III high temperature and pressure sintering processes
It is 1550 DEG C, pressure 9.2GPa
Product made from the preparation method of the above-mentioned uniform composite polycrystal-diamond of microstructure, i.e. microstructure are uniformly gathered
Diamond composite sheet, more specifically, the catalyst in the composite sheet is from carbide interface into polycrystalline diamond layer
No more than about 50 μm of development length, and eruption type infiltration is substantially not present in catalyst, and is dispersed in the polycrystalline diamond layer
At least partly gap area.
The catalyst includes but is not limited to Co etc., and the catalyst is all in composite polycrystal-diamond preparation process
Conventional addO-on therapy.
Compared with the prior art, the invention has the following advantages: the present invention passes through the suitable of multiple high temperature and pressure sintering processes
Secondary progress solves the problems, such as that composite polycrystal-diamond interfacial catalysis agent eruption type permeates the part to be formed and reunites, thus substantially
Degree improves thermal stability, the impact resistance etc. of composite sheet, so improve composite sheet in use anti-collapse, delamination effect
Fruit, so that composite polycrystal-diamond can bear high-temperature operation environment severe under deep geologic, to extend the entirety of drill bit
Service life.
Detailed description of the invention
Fig. 1 is the microstructure schematic diagram of composite polycrystal-diamond made from embodiment 1；
Fig. 2 is the microstructure schematic diagram of composite polycrystal-diamond made from embodiment 2；
Fig. 3 is the microstructure electron microscope of composite polycrystal-diamond made from embodiment 1；
Fig. 4 is the microstructure electron microscope of composite polycrystal-diamond made from embodiment 2.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
The present embodiment carries out preparing polycrystalline diamond compound using the high temperature and pressure sintering process of single treatment in the prior art
Piece, specifically, after the completion of to diadust and catalyst is assembled in hard alloy substrate, in 1550 DEG C, 9.0GPa pressure
Under the conditions of be sintered 320s, finally after equipment is cooling release to get composite polycrystal-diamond, microstructure as shown in Figure 1,
Catalyst penetrates into polycrystalline diamond layer 100 from 210 eruption type of the interface of hard alloy substrate 200, and forms local reunion
201, while catalyst granules 102 is also dispersed within the portion gap region of diamond particles 101 in the polycrystalline diamond layer 100
In 103.
Embodiment 2
The present embodiment prepares polycrystalline diamond using two successively carried out stage high temperature and pressure sintering processes of the present invention
Composite sheet, specifically, first carrying out the first rank to it after the completion of to diadust and catalyst is assembled in hard alloy substrate
Section high temperature and pressure sintering processes, the temperature of first stage high temperature and pressure sintering processes is 1450 DEG C, pressure is 9.0 GPa, sintering
Time is 100s；Then second stage high temperature and pressure sintering processes, the temperature of second stage high temperature and pressure sintering processes are carried out again
It is 9.0 GPa, sintering time 220s for 1500 DEG C, pressure, finally release is compound to get polycrystalline diamond after equipment is cooling
Piece, 15.88 mm of composite polycrystal-diamond diameter made from the present embodiment, 13.2 mm of height.Its microstructure such as Fig. 2,4 institutes
Show, the catalyst in the composite sheet from development length of the carbide interface 210 into polycrystalline diamond layer 100 no more than about
It 50 μm or is not present, while catalyst granules 102 is also dispersed within the part of diamond particles 101 in the polycrystalline diamond layer 100
In gap area 103.
Embodiment 3
The present embodiment prepares polycrystalline diamond using two successively carried out stage high temperature and pressure sintering processes of the present invention
Composite sheet, specifically, first carrying out the first rank to it after the completion of to diadust and catalyst is assembled in hard alloy substrate
Section high temperature and pressure sintering processes, the temperature of first stage high temperature and pressure sintering processes is 1420 DEG C, pressure is 8.0 GPa, sintering
Time is 85s；Then second stage high temperature and pressure sintering processes are carried out again, and the temperature of second stage high temperature and pressure sintering processes is
1550 DEG C, pressure be 9.2 GPa, sintering time 250s, it is compound that polycrystalline diamond is made in the finally release after equipment is cooling
Piece, finally to get composite polycrystal-diamond, composite polycrystal-diamond made from the present embodiment is straight for release after equipment is cooling
15.88 mm of diameter, 13.2 mm of height.
Embodiment 4
The present embodiment prepares polycrystalline diamond using the three phases high temperature and pressure sintering processes of the present invention successively carried out
Composite sheet, specifically, first carrying out the first rank to it after the completion of to diadust and catalyst is assembled in hard alloy substrate
Section high temperature and pressure sintering processes, the temperature of first stage high temperature and pressure sintering processes is 1400 DEG C, pressure is 9.0 GPa, sintering
Time is 60s；Then second stage high temperature and pressure sintering processes are carried out again, and the temperature of second stage high temperature and pressure sintering processes is
1480 DEG C, pressure 9.0GPa, sintering time 180s；Phase III high temperature and pressure sintering processes are carried out again, and the phase III is high
The temperature of warm high-pressure sinter processing is 1550 DEG C, pressure 9.0GPa, sintering time 100s, and end-use device is cooling, release.So
The release after equipment is cooling afterwards, is made composite polycrystal-diamond.
Embodiment 5
The present embodiment prepares polycrystalline diamond using the three phases high temperature and pressure sintering processes of the present invention successively carried out
Composite sheet, specifically, first carrying out the first rank to it after the completion of to diadust and catalyst is assembled in hard alloy substrate
Section high temperature and pressure sintering processes, the temperature of first stage high temperature and pressure sintering processes is 1365 DEG C, pressure 7.6GPa, when sintering
Between be 80s；Then second stage high temperature and pressure sintering processes are carried out again, and the temperature of second stage high temperature and pressure sintering processes is
1450 DEG C, pressure 8.5GPa, sintering time 100s；Phase III high temperature and pressure sintering processes are carried out again, and the phase III is high
The temperature of warm high-pressure sinter processing is 1550 DEG C, pressure 9.2GPa, sintering time 100s, and end-use device is cooling, release.So
The release after equipment is cooling afterwards, is made composite polycrystal-diamond.
After being tested using existing test method composite polycrystal-diamond made from embodiment 1,2,3,4,5, embodiment
2,3,4,5 compared to composite polycrystal-diamond made from embodiment 1, and heat resistance is respectively increased 50%, 60%, 55% and 72%；Anti-impact
Hitting property is respectively increased 100%, 110%, 113% and 110%.
Claims (10)
1. a kind of preparation method of the uniform composite polycrystal-diamond of microstructure, including it is golden to being assembled in hard alloy substrate
High temperature and pressure sintering step after the completion of hard rock micro mist and catalyst, which is characterized in that the high temperature and pressure sintering step includes
The high temperature and pressure sintering processes at least two stages sequentially carried out, and the temperature of each high temperature and pressure sintering processes sequentially rises
Height, pressure is identical or sequentially increases.
2. the preparation method of the uniform composite polycrystal-diamond of microstructure as described in claim 1, which is characterized in that institute
Stating high temperature and pressure sintering step includes that the first stage high temperature and pressure sintering processes sequentially carried out and second stage high temperature and pressure are burnt
Knot processing, under the conditions of two-stage processing has uniform pressure, after first stage high temperature and pressure sintering processes, polycrystalline diamond
Catalyst quality accounting in layer is at least 5 %；After second stage high temperature and pressure sintering processes, in polycrystalline diamond layer
Catalyst quality accounting is at least 10%.
3. the preparation method of the uniform composite polycrystal-diamond of microstructure as claimed in claim 2, which is characterized in that institute
The temperature for stating first stage high temperature and pressure sintering processes is 1450 DEG C, and pressure is 9.0 GPa, at second stage high temperature and pressure sintering
The temperature of reason is 1550 DEG C, and pressure is 9.0 GPa.
4. the preparation method of the uniform composite polycrystal-diamond of microstructure as described in claim 1, which is characterized in that institute
Stating high temperature and pressure sintering step includes that the first stage high temperature and pressure sintering processes sequentially carried out and second stage high temperature and pressure are burnt
Knot is handled, and after first stage high temperature and pressure sintering processes, the catalyst quality accounting in polycrystalline diamond layer is at least
10%；After second stage high temperature and pressure sintering processes, the catalyst quality accounting in polycrystalline diamond layer is at least 15%.
5. the preparation method of the uniform composite polycrystal-diamond of microstructure as claimed in claim 4, which is characterized in that institute
The temperature for stating first stage high temperature and pressure sintering processes is 1420 DEG C, pressure 8.0GPa, at second stage high temperature and pressure sintering
The temperature of reason is 1550 DEG C, pressure 9.2GPa.
6. the preparation method of the uniform composite polycrystal-diamond of microstructure as described in claim 1, which is characterized in that institute
Stating high temperature and pressure sintering step includes the first stage sequentially carried out, second stage and phase III high temperature and pressure sintering processes,
Under the conditions of three-phase process has uniform pressure, after first stage high temperature and pressure sintering processes, in polycrystalline diamond layer
Catalyst quality accounting is at least 4%；After second stage high temperature and pressure sintering processes, the catalyst in polycrystalline diamond layer
Quality accounting is at least 6%；After phase III high temperature and pressure sintering processes, the catalyst quality in polycrystalline diamond layer is accounted for
Than being at least 10%.
7. the preparation method of the uniform composite polycrystal-diamond of microstructure as claimed in claim 6, which is characterized in that institute
The temperature for stating first stage high temperature and pressure sintering processes is 1400 DEG C, pressure 9.0GPa, at second stage high temperature and pressure sintering
The temperature of reason is 1480 DEG C, pressure 9.0GPa；The temperature of phase III high temperature and pressure sintering processes is 1550 DEG C, and pressure is
9.0GPa。
8. the preparation method of the uniform composite polycrystal-diamond of microstructure as described in claim 1, which is characterized in that institute
Stating high temperature and pressure sintering step includes the first stage sequentially carried out, second stage and phase III high temperature and pressure sintering processes,
Under the conditions of the pressure of the high temperature and pressure sintering processes of three phases sequentially increases, first stage high temperature and pressure sintering processes terminate
Afterwards, the catalyst quality accounting in polycrystalline diamond layer is at least 5%；After second stage high temperature and pressure sintering processes, plycrystalline diamond
Catalyst quality accounting in diamond layer is at least 8%；After phase III high temperature and pressure sintering processes, polycrystalline diamond
Catalyst quality accounting in layer is at least 12%.
9. the preparation method of the uniform composite polycrystal-diamond of microstructure as claimed in claim 8, which is characterized in that institute
The temperature for stating first stage high temperature and pressure sintering processes is 1365 DEG C, pressure 7.6GPa, at second stage high temperature and pressure sintering
The temperature of reason is 1450 DEG C, pressure 8.5GPa；The temperature of phase III high temperature and pressure sintering processes is 1550 DEG C, and pressure is
9.2GPa。
10. plycrystalline diamond made from the preparation method of any uniform composite polycrystal-diamond of microstructure of claim 1-9
Diamond compact.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910459388.4A CN110090960B (en) | 2019-05-29 | 2019-05-29 | Preparation method of polycrystalline diamond compact with uniform microstructure and product |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910459388.4A CN110090960B (en) | 2019-05-29 | 2019-05-29 | Preparation method of polycrystalline diamond compact with uniform microstructure and product |
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| CN110090960A true CN110090960A (en) | 2019-08-06 |
| CN110090960B CN110090960B (en) | 2021-05-18 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022085438A1 (en) * | 2020-10-22 | 2022-04-28 | 住友電工ハードメタル株式会社 | Diamond sintered body and tool provided with diamond sintered body |
| CN114833345A (en) * | 2022-05-31 | 2022-08-02 | 河南四方达超硬材料股份有限公司 | Polycrystalline diamond compact and preparation method thereof |
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| US20190022745A1 (en) * | 2010-10-08 | 2019-01-24 | Baker Hughes, A Ge Company, Llc | Composite materials including nanoparticles, earth-boring tools and components including such composite materials, polycrystalline materials including nanoparticles, and related methods |
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| CN110090960B (en) | 2021-05-18 |
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