CN110090960B - Preparation method of polycrystalline diamond compact with uniform microstructure and product - Google Patents
Preparation method of polycrystalline diamond compact with uniform microstructure and product Download PDFInfo
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- CN110090960B CN110090960B CN201910459388.4A CN201910459388A CN110090960B CN 110090960 B CN110090960 B CN 110090960B CN 201910459388 A CN201910459388 A CN 201910459388A CN 110090960 B CN110090960 B CN 110090960B
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 76
- 239000010432 diamond Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 107
- 238000011282 treatment Methods 0.000 claims abstract description 91
- 239000003054 catalyst Substances 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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Classifications
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- 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
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- 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
Abstract
The invention belongs to the technical field of superhard composite materials, and particularly relates to a preparation method and a product of a polycrystalline diamond compact with a uniform microstructure. According to the invention, through the sequential implementation of a plurality of high-temperature and high-pressure sintering treatments, the problem of local agglomeration formed by eruption type permeation of the catalyst at the interface of the polycrystalline diamond compact is solved, so that the thermal stability, the impact resistance and the like of the compact are greatly improved, and the anti-collapse and anti-delamination effects of the compact in the using process are further improved.
Description
Technical Field
The invention belongs to the technical field of superhard composite materials, and particularly relates to a preparation method of a polycrystalline diamond compact with a uniform microstructure and a product.
Background
Polycrystalline diamond compacts are composite materials formed by sintering a diamond layer and a hard alloy matrix mutually in a high-temperature high-pressure (HTHP) environment, and are applied to wear-resistant cutting elements of drilling tools such as petroleum and natural gas. However, in the conventional single-treatment high-temperature and high-pressure process, the catalyst in the cemented carbide substrate is melted and rapidly increased, and the catalyst in the substrate is caused to eruptively penetrate into the polycrystalline diamond layer, so that the locally agglomerated catalyst or other substrate components exist in the polycrystalline diamond layer. The thermal stability, impact resistance and the like of the composite sheet are greatly reduced by the local catalyst or other matrix components in the polycrystalline diamond layer, so that the composite sheet has serious failure problems of chipping, delaminating and the like in the using process.
Disclosure of Invention
The invention aims to provide a preparation method and a product of a polycrystalline diamond compact with a uniform microstructure.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a polycrystalline diamond compact with a uniform microstructure comprises a high-temperature high-pressure sintering step after diamond micro powder and a catalyst are assembled in a hard alloy matrix, wherein the high-temperature high-pressure sintering step comprises high-temperature high-pressure sintering treatment in at least two stages which are sequentially carried out, and the temperature of each high-temperature high-pressure sintering treatment is sequentially increased, and the pressure is the same or sequentially increased.
Preferably, the high-temperature and high-pressure sintering step comprises a first-stage high-temperature and high-pressure sintering treatment and a second-stage high-temperature and high-pressure sintering treatment which are sequentially performed, the two-stage treatment has the same pressure, and after the first-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 5%; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass percentage of the catalyst in the polycrystalline diamond layer is at least 10%.
Preferably, the temperature of the first-stage high-temperature high-pressure sintering treatment is 1450 ℃, the pressure is 9.0GPa, and the temperature of the second-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.0 GPa.
Preferably, the high-temperature and high-pressure sintering step comprises a first-stage high-temperature and high-pressure sintering treatment and a second-stage high-temperature and high-pressure sintering treatment which are sequentially performed, and after the first-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 10%; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass percentage of the catalyst in the polycrystalline diamond layer is at least 15%.
Preferably, the temperature of the first-stage high-temperature high-pressure sintering treatment is 1420 ℃, the pressure is 8.0GPa, and the temperature of the second-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.2 GPa.
Preferably, the high-temperature high-pressure sintering step comprises a first stage, a second stage and a third stage of high-temperature high-pressure sintering treatment which are sequentially carried out, the three-stage treatment has the same pressure, and the mass of the catalyst in the polycrystalline diamond layer is at least 4% after the first stage of high-temperature high-pressure sintering treatment is finished; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 6%; and after the third-stage high-temperature and high-pressure sintering treatment is finished, the mass percentage of the catalyst in the polycrystalline diamond layer is at least 10%.
Preferably, the temperature of the first-stage high-temperature high-pressure sintering treatment is 1400 ℃, the pressure is 9.0GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1480 ℃, and the pressure is 9.0 GPa; the temperature of the third-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.0 GPa.
Preferably, the high-temperature and high-pressure sintering step comprises a first stage, a second stage and a third stage of high-temperature and high-pressure sintering treatment which are sequentially carried out, wherein the mass of the catalyst in the polycrystalline diamond layer is at least 5% under the condition that the pressure of the high-temperature and high-pressure sintering treatment of the three stages is sequentially increased after the high-temperature and high-pressure sintering treatment of the first stage is finished; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 8%; and after the third-stage high-temperature and high-pressure sintering treatment is finished, the mass percentage of the catalyst in the polycrystalline diamond layer is at least 12%.
Preferably, the temperature of the first-stage high-temperature high-pressure sintering treatment is 1365 ℃, the pressure is 7.6GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1450 ℃, and the pressure is 8.5 GPa; the temperature of the third-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.2GPa
The polycrystalline diamond compact with the uniform microstructure is prepared by the preparation method, namely the polycrystalline diamond compact with the uniform microstructure, more specifically, the extension length of the catalyst in the compact from the hard alloy interface to the polycrystalline diamond layer is not more than about 50 micrometers, and the catalyst basically has no eruption penetration and is dispersed in at least partial gap area of the polycrystalline diamond layer.
The catalyst includes but is not limited to Co, etc., and the catalyst is a conventional additive component in the preparation process of the polycrystalline diamond compact.
Compared with the prior art, the invention has the following advantages: according to the invention, through the sequential implementation of a plurality of high-temperature and high-pressure sintering treatments, the problem of local agglomeration formed by eruption type permeation of the catalyst at the interface of the polycrystalline diamond compact is solved, so that the thermal stability, the impact resistance and the like of the compact are greatly improved, the anti-collapse and anti-delamination effects of the compact in the use process are further improved, the polycrystalline diamond compact can bear a severe high-temperature operation environment under deep geology, and the integral service life of the drill bit is prolonged.
Drawings
Fig. 1 is a schematic view of the microstructure of a polycrystalline diamond compact made in example 1;
fig. 2 is a schematic view of the microstructure of the polycrystalline diamond compact prepared in example 2;
fig. 3 is an electron micrograph of the microstructure of the polycrystalline diamond compact prepared in example 1;
fig. 4 is an electron micrograph of the microstructure of the polycrystalline diamond compact prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
In this embodiment, a single-treatment high-temperature high-pressure sintering process in the prior art is adopted to prepare a polycrystalline diamond compact, specifically, after assembling diamond micro powder and a catalyst in a hard alloy matrix, sintering the hard alloy matrix at 1550 ℃ under a pressure of 9.0GPa for 320s, and finally, after cooling the equipment, releasing pressure to obtain the polycrystalline diamond compact, wherein a microstructure of the polycrystalline diamond compact is as shown in fig. 1, the catalyst eruptively penetrates into the polycrystalline diamond layer 100 from an interface 210 of the hard alloy matrix 200 to form local agglomerates 201, and meanwhile, catalyst particles 102 are also dispersed in a part of gap regions 103 of the diamond particles 101 in the polycrystalline diamond layer 100.
Example 2
In this embodiment, a polycrystalline diamond compact is prepared by successively performing two stages of high-temperature high-pressure sintering treatment, specifically, after assembling diamond micro powder and a catalyst in a hard alloy substrate, a first stage of high-temperature high-pressure sintering treatment is performed, wherein the temperature of the first stage of high-temperature high-pressure sintering treatment is 1450 ℃, the pressure of the first stage of high-temperature high-pressure sintering treatment is 9.0GPa, and the sintering time is 100 s; and then carrying out second-stage high-temperature and high-pressure sintering treatment, wherein the temperature of the second-stage high-temperature and high-pressure sintering treatment is 1500 ℃, the pressure is 9.0GPa, the sintering time is 220s, and finally, after the equipment is cooled, pressure is relieved, so that the polycrystalline diamond compact is obtained, wherein the diameter of the polycrystalline diamond compact prepared by the embodiment is 15.88 mm, and the height of the polycrystalline diamond compact is 13.2 mm. The microstructure is shown in fig. 2 and 4, and the catalyst within the composite sheet extends no more than about 50 μm or is absent from the cemented carbide interface 210 into the polycrystalline diamond layer 100, while the catalyst particles 102 are also dispersed within the portion of the interstitial regions 103 of the diamond particles 101 in the polycrystalline diamond layer 100.
Example 3
In this embodiment, a polycrystalline diamond compact is prepared by successively performing two stages of high-temperature high-pressure sintering treatment, specifically, after assembling diamond micro powder and a catalyst in a hard alloy substrate, a first stage of high-temperature high-pressure sintering treatment is performed, wherein the temperature of the first stage of high-temperature high-pressure sintering treatment is 1420 ℃, the pressure is 8.0GPa, and the sintering time is 85 s; and then carrying out second-stage high-temperature and high-pressure sintering treatment, wherein the temperature and the pressure of the second-stage high-temperature and high-pressure sintering treatment are 1550 ℃, 9.2GPa and 250s, finally relieving pressure after the equipment is cooled to obtain a polycrystalline diamond compact, and finally relieving pressure after the equipment is cooled to obtain the polycrystalline diamond compact, wherein the diameter of the polycrystalline diamond compact prepared by the embodiment is 15.88 mm, and the height of the polycrystalline diamond compact is 13.2 mm.
Example 4
In this embodiment, a polycrystalline diamond compact is prepared by sequentially performing three stages of high-temperature high-pressure sintering treatment, specifically, after assembling diamond micro powder and a catalyst in a hard alloy substrate, a first stage of high-temperature high-pressure sintering treatment is performed, wherein the temperature of the first stage of high-temperature high-pressure sintering treatment is 1400 ℃, the pressure of the first stage of high-temperature high-pressure sintering treatment is 9.0GPa, and the sintering time is 60 s; then carrying out second-stage high-temperature high-pressure sintering treatment, wherein the temperature of the second-stage high-temperature high-pressure sintering treatment is 1480 ℃, the pressure is 9.0GPa, and the sintering time is 180 s; and then carrying out high-temperature high-pressure sintering treatment at 1550 ℃, 9.0GPa and 100s for the third stage, and finally cooling and releasing the equipment. And then, after the equipment is cooled, releasing the pressure to prepare the polycrystalline diamond compact.
Example 5
In this embodiment, the polycrystalline diamond compact is prepared by sequentially performing three stages of high-temperature high-pressure sintering treatment, specifically, after assembling diamond micro powder and a catalyst in a hard alloy substrate, the first stage of high-temperature high-pressure sintering treatment is performed, the temperature of the first stage of high-temperature high-pressure sintering treatment is 1365 ℃, the pressure of the first stage of high-temperature high-pressure sintering treatment is 7.6GPa, and the sintering time is 80 s; then carrying out second-stage high-temperature high-pressure sintering treatment, wherein the temperature of the second-stage high-temperature high-pressure sintering treatment is 1450 ℃, the pressure is 8.5GPa, and the sintering time is 100 s; and then carrying out high-temperature high-pressure sintering treatment at 1550 ℃, 9.2GPa and 100s for the third stage, and finally cooling and releasing the equipment. And then, after the equipment is cooled, releasing the pressure to prepare the polycrystalline diamond compact.
After testing the polycrystalline diamond compacts prepared in the embodiments 1, 2, 3, 4 and 5 by using the existing testing method, the heat resistance of the polycrystalline diamond compacts prepared in the embodiments 2, 3, 4 and 5 is respectively improved by 50%, 60%, 55% and 72% compared with that of the polycrystalline diamond compact prepared in the embodiment 1; the impact resistance is improved by 100%, 110%, 113% and 110%, respectively.
Claims (1)
1. A preparation method of a polycrystalline diamond compact with a uniform microstructure comprises a high-temperature high-pressure sintering step after diamond micro powder and a catalyst are assembled in a hard alloy matrix, and is characterized in that the high-temperature high-pressure sintering step comprises high-temperature high-pressure sintering treatment of at least two stages which are sequentially carried out, and the temperature of each high-temperature high-pressure sintering treatment is sequentially increased, and the pressure is the same or is sequentially increased;
the high-temperature high-pressure sintering step comprises a first-stage high-temperature high-pressure sintering treatment and a second-stage high-temperature high-pressure sintering treatment which are sequentially carried out, the two-stage treatment has the same pressure condition, and the mass of a catalyst in the polycrystalline diamond layer accounts for at least 5% after the first-stage high-temperature high-pressure sintering treatment is finished; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 10%;
the temperature of the first-stage high-temperature high-pressure sintering treatment is 1450 ℃, the pressure is 9.0GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.0 Gpa;
or the high-temperature high-pressure sintering step comprises a first-stage high-temperature high-pressure sintering treatment and a second-stage high-temperature high-pressure sintering treatment which are sequentially carried out, wherein after the first-stage high-temperature high-pressure sintering treatment is finished, the mass percentage of the catalyst in the polycrystalline diamond layer is at least 10%; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 15%;
the temperature of the first-stage high-temperature high-pressure sintering treatment is 1420 ℃, the pressure is 8.0GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.2 Gpa;
or the high-temperature high-pressure sintering step comprises a first stage, a second stage and a third stage of high-temperature high-pressure sintering treatment which are sequentially carried out, the three-stage treatment has the same pressure condition, and the mass of the catalyst in the polycrystalline diamond layer accounts for at least 4% after the first stage of high-temperature high-pressure sintering treatment is finished; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 6%; after the third-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 10%;
the temperature of the first-stage high-temperature high-pressure sintering treatment is 1400 ℃, the pressure is 9.0GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1480 ℃, and the pressure is 9.0 GPa; the temperature of the high-temperature high-pressure sintering treatment in the third stage is 1550 ℃, and the pressure is 9.0 Gpa;
or the high-temperature high-pressure sintering step comprises a first stage, a second stage and a third stage of high-temperature high-pressure sintering treatment which are sequentially carried out, wherein the mass percentage of the catalyst in the polycrystalline diamond layer is at least 5% after the first stage of high-temperature high-pressure sintering treatment under the condition that the pressure of the high-temperature high-pressure sintering treatment of the three stages is sequentially increased; after the second-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 8%; after the third-stage high-temperature and high-pressure sintering treatment is finished, the mass of the catalyst in the polycrystalline diamond layer accounts for at least 12%;
the temperature of the first-stage high-temperature high-pressure sintering treatment is 1365 ℃, the pressure is 7.6GPa, the temperature of the second-stage high-temperature high-pressure sintering treatment is 1450 ℃, and the pressure is 8.5 GPa; the temperature of the third-stage high-temperature high-pressure sintering treatment is 1550 ℃, and the pressure is 9.2 Gpa.
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| 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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| US8361178B2 (en) * | 2008-04-21 | 2013-01-29 | Smith International, Inc. | Tungsten rhenium compounds and composites and methods for forming the same |
| BR112013008180A2 (en) * | 2010-10-08 | 2016-06-21 | Baker Hughes Inc | composite materials including nanoparticles, earth sounding tools and components including such composite materials, polycrystalline materials including nanoparticles, and related methods |
| US10046441B2 (en) * | 2013-12-30 | 2018-08-14 | Smith International, Inc. | PCD wafer without substrate for high pressure / high temperature sintering |
| US10358705B2 (en) * | 2014-12-17 | 2019-07-23 | Smith International, Inc. | Polycrystalline diamond sintered/rebonded on carbide substrate containing low tungsten |
| CN105840104B (en) * | 2016-03-25 | 2018-07-17 | 河南四方达超硬材料股份有限公司 | A kind of thermostable type high impact-resistant composite polycrystal-diamond and manufacturing method |
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