CN113059161A - Polycrystalline diamond compact and preparation method thereof - Google Patents
Polycrystalline diamond compact and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F7/08—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 with one or more parts not made from powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B22F3/14—Both compacting and sintering simultaneously
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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Abstract
The invention relates to the technical field of synthesis of superhard materials, and provides a polycrystalline diamond compact which consists of a polycrystalline diamond working layer and a hard alloy substrate layer, wherein the raw material of the polycrystalline diamond working layer is a mixture of a degassing agent and diamond particles with certain surface cleanliness; the diamond particles consist of main diamond particle size particles and auxiliary diamond particle size particles, and the main diamond particle size particles account for 70-100% of the diamond particles by weight. Also provides a preparation method of the polycrystalline diamond compact, which comprises the following steps: the raw material of the polycrystalline diamond working layer is placed on a hard alloy substrate layer and is sintered and synthesized through two sections of high temperature and high pressure. The polycrystalline diamond compact disclosed by the invention has high chipping resistance, high impact strength, high wear resistance and finish surface smoothness, so that the polycrystalline diamond compact has higher service performance and service life.
Description
Technical Field
The invention relates to the technical field of synthesis of superhard materials, in particular to a polycrystalline diamond compact and a preparation method thereof.
Background
The structure of the polycrystalline diamond compact generally consists of a polycrystalline diamond working layer and a hard alloy substrate layer, and the existing preparation method of the polycrystalline diamond compact is mainly characterized in that diamond particles and the hard alloy substrate layer are assembled and then sintered and synthesized under the conditions of high temperature and high pressure. Polycrystalline diamond compacts are mainly used in fields such as drill bits and cutting tools.
In the drilling industry, polycrystalline diamond compacts on drill bits are required to have relatively good impact strength and wear resistance. In the cutting tool industry, polycrystalline diamond compacts on tools are required to have a high cutting finish and resistance to chipping. However, in actual production, the impact strength, wear resistance, cutting smoothness and chipping resistance of the polycrystalline diamond compact are mainly adjusted by adjusting the particle size of raw diamond particles of a polycrystalline diamond working layer of the polycrystalline diamond compact, so that the particle size of the diamond particles is increased, the wear resistance and impact strength of the sintered and synthesized polycrystalline diamond working layer can be improved, but the chipping resistance and cutting smoothness are reduced; reducing the grain size of the diamond grains can improve the chipping resistance and the cutting smoothness of the sintered and synthesized polycrystalline diamond working layer, but the wear resistance and the impact strength are reduced. From the actual production of the current polycrystalline diamond compact, the two are contradictory, so that raw diamond particles with reasonable particle size are selected mainly according to the application requirements of actual use occasions. For example, polycrystalline diamond working layers on polycrystalline diamond compacts used in drill bits for drilling typically have diamond feedstock particle sizes in the range of 6 microns to 30 microns, with typical diamond particle sizes in the range of 8 microns to 20 microns. The diamond grain size is less than 8 microns, and the abrasion resistance is poor. The diamond granularity is higher than 20 microns, the chipping resistance is poor, and the service life is shortened. The granularity of diamond raw materials of a polycrystalline diamond working layer on a polycrystalline diamond composite sheet used on a cutting tool is generally 1-30 micrometers, when the polycrystalline diamond composite sheet is used for finish machining or super-finish machining, the raw material diamond particles of about 1-5 micrometers are selected, the polycrystalline diamond working layer on the polycrystalline diamond composite sheet synthesized by sintering is good in chipping resistance and high in cutting finish, and the cutting roughness can reach Ra0.1 micrometer; when the method is used for rough machining, raw material diamond particles with the average particle size of about 10 microns and the particle size of 10 microns are selected, and the obtained polycrystalline diamond working layer is high in wear resistance and impact strength, but poor in chipping resistance and low in smoothness.
However, with the continuous progress of technology and the complexity of the machining environment, both for drilling and cutting tools, higher demands are made on the overall performance of polycrystalline diamond compacts. Accordingly, there is a need for improvements in polycrystalline diamond compacts and methods of making the same.
Disclosure of Invention
The present invention is directed to a polycrystalline diamond compact to solve the above problems of the related art.
The invention aims to provide a preparation method of a polycrystalline diamond compact, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme: a polycrystalline diamond compact is composed of a polycrystalline diamond working layer and a hard alloy substrate layer, the raw material of the polycrystalline diamond working layer is a mixture of diamond particles with certain surface cleanliness and a degassing agent, and the porosity of the raw material of the polycrystalline diamond working layer is 30% -45% at room temperature; the diamond particles consist of diamond primary particle size particles and diamond secondary particle size particles, and the particle size of the diamond primary particle size particles is 35-275 microns; the grain diameter of the diamond auxiliary grain size particles is less than or equal to 1/4 grain diameter of the diamond main grain size particles, and the weight percentage of the diamond main grain size particles in the diamond grains is 70-100%; the degassing agent accounts for 0.1-3.0% of the weight of the diamond particles; the hard alloy base layer is made of tungsten carbide containing cobalt.
Preferably, the degassing agent is one or more of metal zirconium powder, zirconium copper alloy, zirconium aluminum alloy, zirconium nickel alloy, zirconium carbide, metal titanium powder, titanium alloy and titanium carbide.
Preferably, the cobalt content of the cemented carbide substrate layer is 12-16 wt%.
Preferably, the surface cleanliness of the diamond particles is: the grain diameter of the diamond particles is less than 3 microns, and the surface impurity content of the diamond particles is less than 55 ppm; the grain diameter of the diamond particles is 3-40 microns, and the surface impurity content of the diamond particles is less than 40 ppm; the grain diameter of the diamond particles is 40-60 microns, and the surface impurity content of the diamond particles is less than 27 ppm; the diamond particles have a particle size of greater than 60 microns and a surface impurity level of less than 15 ppm.
A preparation method of a polycrystalline diamond compact comprises the steps of placing raw materials of a polycrystalline diamond working layer on a hard alloy substrate layer, and sintering the raw materials at high temperature and high pressure for two sections to synthesize the polycrystalline diamond compact;
high temperature and high pressure in the first stage: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 3.5-6 minutes;
second-stage high-temperature high-pressure: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 8-16 minutes.
Preferably, the diamond particles are divided into a plurality of continuous particle size sections according to the particle size, the main particle size particles of the diamond are selected from one particle size section or the mixture of two to three adjacent particle size sections, and the auxiliary particle size particles of the diamond are selected from one particle size section or the mixture of a plurality of finer particle size sections.
Preferably, the raw material of the polycrystalline diamond working layer and the cemented carbide substrate layer are placed in a refractory metal cup.
Preferably, the high-temperature resistant metal cup is made of one or a combination of more of tantalum, molybdenum, niobium and zirconium.
Has the advantages that: 1. the diamond main particle size particles of 35-275 microns are used as main raw materials, and the wide cobalt penetration line is favorable for the sweeping penetration of cobalt of the hard alloy substrate layer to the diamond working layer. The total surface area of the large-particle-size diamond main-particle-size particles in the polycrystalline diamond working layer is favorable for the growth of recrystallized diamond among diamond crystal faces. The generated polycrystalline diamond working layer has uniform structure and few internal defects. The impact strength of the polycrystalline diamond compact product prepared by the method is greatly improved.
2. Most of the recrystallized diamond between the diamond particles forms bond-bonded recrystallized diamond to form a relatively complete integral diamond working layer, and the problem of poor anti-tipping performance of the large-particle polycrystalline diamond compact is solved.
3. According to the polycrystalline diamond compact disclosed by the invention, the volume ratio of diamond particles in the polycrystalline diamond working layer is more than 96%, and the volume ratio of cobalt metal in the polycrystalline diamond working layer to the polycrystalline diamond working layer is less than 2%. The structure greatly improves the wear resistance of the polycrystalline diamond compact product prepared by the invention.
In conclusion, the polycrystalline diamond compact of the present invention has high chipping resistance, high impact strength, high wear resistance, and a finished surface finish, and thus has higher service performance and service life.
Drawings
Fig. 1 is a schematic cross-sectional view of a polycrystalline diamond compact of the present invention prior to synthesis and compaction.
Fig. 2 is a schematic cross-sectional view of a polycrystalline diamond compact of the present disclosure during synthetic compaction.
Fig. 3 is a schematic cross-sectional view of a polycrystalline diamond compact of the present disclosure after synthesis and compaction.
Fig. 4 is a schematic structural view of a polycrystalline diamond compact of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are intended to provide those skilled in the art with a more complete, accurate and thorough understanding of the concepts and technical solutions of the present invention, and to facilitate its implementation.
As shown in fig. 4, the polycrystalline diamond compact of the present invention is composed of a polycrystalline diamond working layer 10 and a cemented carbide substrate layer 20, the raw material of the polycrystalline diamond working layer is a mixture of diamond particles with a certain surface cleanliness and a degassing agent, and the porosity of the raw material of the polycrystalline diamond working layer is 30% to 45% at room temperature; the diamond particles consist of diamond primary particle size particles and diamond secondary particle size particles, and the particle size of the diamond primary particle size particles is 35-275 microns; the grain diameter of the diamond auxiliary grain size particles is less than or equal to 1/4 grain diameter of the diamond main grain size particles, and the weight percentage of the diamond main grain size particles in the diamond grains is 70-100%; the degassing agent accounts for 0.1-3.0% of the weight of the diamond particles; the hard alloy base layer is made of tungsten carbide containing cobalt.
Specifically, the degassing agent is one or more of metal zirconium powder, zirconium copper alloy, zirconium aluminum alloy, zirconium nickel alloy, zirconium carbide, metal titanium powder, titanium alloy and titanium carbide.
Specifically, the cobalt content of the cemented carbide substrate layer is 12-16 wt%.
Specifically, the polycrystalline diamond working layer is prepared from raw materials with air porosity of 30-45% at room temperature.
Specifically, the diamond particles are subjected to acid treatment, high-temperature alkali treatment, purified water cleaning or ultrasonic cleaning and other cleaning procedures, so that the surface cleanliness of the diamond particles at least meets the following conditions: the grain diameter of the diamond particles is less than 3 microns, and the surface impurity content of the diamond particles is less than 55 ppm; the grain diameter of the diamond particles is 3-40 microns, and the surface impurity content of the diamond particles is less than 40 ppm; the grain diameter of the diamond particles is 40-60 microns, and the surface impurity content of the diamond particles is less than 27 ppm; the diamond particles have a particle size of greater than 60 microns and a surface impurity level of less than 15 ppm.
A preparation method of a polycrystalline diamond compact comprises the steps of placing raw materials of a polycrystalline diamond working layer on a hard alloy substrate layer, and sintering the raw materials at high temperature and high pressure for two sections to synthesize the polycrystalline diamond compact;
high temperature and high pressure in the first stage: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 3.5-6 minutes;
second-stage high-temperature high-pressure: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 8-16 minutes.
Specifically, the diamond particles are divided into a plurality of particle size segments according to the average particle size as shown in table 1, the main particle size particles of the diamond are selected from one particle size segment or a mixture of two to three adjacent particle size segments, and the auxiliary particle size particles of the diamond are selected from one particle size segment or a mixture of a plurality of finer particle size segments.
TABLE 1 particle size distribution of diamond particles and average particle diameter of each particle size distribution
Specifically, the raw material of the polycrystalline diamond working layer and the hard alloy substrate layer are placed in a high-temperature resistant metal cup.
Specifically, the high-temperature resistant metal cup is made of one or a combination of more of tantalum, molybdenum, niobium and zirconium.
Example 1
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein the raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 70 wt% of diamond primary particle size particles and 30 wt% of diamond auxiliary particle size particles, the particle size section of the diamond primary particle size particles is 50/60 meshes, and the diamond auxiliary particle size particles comprise 6 wt% of diamond particles with the particle size section of 40-50 micrometers and 24 wt% of diamond particles with the particle size section of 22-36 micrometers. The degassing agent adopts a mixture of 0.25 percent of Ni30Zr70, 0.12 percent of Cu30Zr70, 0.55 percent of ZrC and 0.10 percent of Ti; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 3.5 minutes;
second-stage high-temperature high-pressure: the synthesis high pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 8 minutes.
Example 2
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein the raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 85 wt% of diamond primary particle size particles and 15 wt% of diamond auxiliary particle size particles, the particle size section of the diamond primary particle size particles is 80/100 meshes, and the diamond auxiliary particle size particles comprise 3 wt% of diamond particles with the particle size section of 8-16 micrometers and 12 wt% of diamond particles with the particle size section of 3-6 micrometers. The degassing agent adopts a mixture of 0.18 wt% of Ni30Zr70, 0.25 wt% of Cu30Zr70, 0.25 wt% of ZrC and 0.1 wt% of Ti; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 4.5 minutes;
second-stage high-temperature high-pressure: the synthesis high pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 12.5 minutes.
Example 3
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein the raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 85 wt% of diamond primary particle size particles and 15 wt% of diamond auxiliary particle size particles, the particle size section of the diamond primary particle size particles is 170/200 meshes, and the diamond auxiliary particle size particles comprise 3 wt% of diamond particles with the particle size section of 8-16 micrometers and 12 wt% of diamond particles with the particle size section of 3-6 micrometers. The degassing agent adopts a mixture of 0.17 wt% of Cu30Zr70, 0.13 wt% of Al30Zr70 and 0.3 wt% of TiC; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 5 minutes;
second-stage high-temperature high-pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 13.5 minutes.
Example 4
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein the raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 96 wt% of diamond main particle size particles and 4 wt% of diamond auxiliary particle size particles, the particle size section of the diamond main particle size particles is 40-60 micrometers, and the diamond auxiliary particle size particles are diamond particles with the particle size section of 3-6 micrometers. The degassing agent adopts a mixture of 0.12 wt% of Cu30Zr70, 0.26 wt% of Al30Zr70 and 0.8 wt% of TiC; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 6 minutes;
second-stage high-temperature high-pressure: the synthesis high pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 16 minutes.
Example 5
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 100 wt% of diamond primary-grain-size particles, the grain size section of the diamond primary-grain-size particles is 80/100 meshes, and the degassing agent adopts a mixture of 0.12 wt% of Cu30Zr70, 0.26 wt% of Al30Zr70 and 0.8 wt% of TiC; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 5.5 minutes;
second-stage high-temperature high-pressure: the synthesis high pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 15 minutes.
Example 6
A polycrystalline diamond compact comprises a polycrystalline diamond working layer and a hard alloy substrate layer, wherein raw materials of the polycrystalline diamond working layer comprise diamond particles and a degassing agent, the diamond particles comprise 100 wt% of diamond primary-grain-size particles, the diamond primary-grain-size particles comprise 60 wt% of diamond particles with the grain size section of 80/100 meshes and 40 wt% of diamond particles with the grain size section of 100/120 meshes, and the degassing agent adopts a mixture of 0.12 wt% of Cu30Zr70, 0.26 wt% of Al30Zr70 and 0.8 wt% of TiC; arrange the raw materials of polycrystalline diamond working layer in on the carbide stratum basale, by high temperature resistant metal cup parcel, carry out high temperature high pressure synthesis, first section high temperature high pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 5 minutes;
second-stage high-temperature high-pressure: the synthesis pressure is 7000MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 15.5 minutes.
The working principle of this application does: in production and research, the applicant finds that the breakage resistance and the cutting finish of raw diamond particles adopting coarse particles gradually decrease with the increase of the particle size when the polycrystalline diamond compact is sintered and synthesized. The larger the particle size of the raw diamond particles is, the more wear-resistant the diamond is, and the impact strength of the polycrystalline diamond working layer is improved. However, the polycrystalline diamond compact has short service life and low cutting smoothness due to large particles falling off after processing abrasion and poor chipping resistance. The main reasons are as follows: the bonding between diamond particles is less, the bonding force is weak, and the diamond particles are easy to fall off. In order to increase the bonding strength between diamond particles, it is necessary to use highly clean diamond raw materials and synthesis environments. The impurities of silicon and metal on the surface of the diamond particles are removed, and air in the synthesis environment is removed. The impurities exist on the surfaces of the diamond particles and air exists among the diamond particles, under the conditions of high temperature and high pressure, the impurities and the oxygen and nitrogen elements in the air interfere with the graphitization of the surfaces of the diamond particles under the conditions of high temperature and high pressure, the graphite structure of the graphitized surfaces of the diamond particles is damaged, and stable and continuous diamond recrystallization cannot be formed in the diamond particles during recrystallization.
In the application, high cleanliness is firstly limited for the polycrystalline diamond working layer raw material, the hard alloy substrate layer and the high-temperature resistant metal cup, and the diamond particle micro powder abrasive material needs to reach the cleanliness requirement through acid treatment, high-temperature alkali treatment, purified water cleaning, ultrasonic cleaning and other treatment modes.
Specifically, the requirements for the surface cleanliness of the diamond particle micro powder abrasive are as follows. The diamond grain size is less than 3 microns, and the surface silicon and metal impurity content of the diamond grain size is less than 55 ppm. The diamond particle size is 3-40 microns, and the surface silicon and metal impurity content is less than 40 ppm. The diamond particle size is 40-60 microns, and the surface silicon and metal impurity content is less than 27 ppm. The diamond grain size is larger than 60 microns, and the surface silicon and metal impurity content of the diamond grain size is less than 15 ppm.
The high-temperature resistant metal cup, the polycrystalline diamond working layer raw material mixture in the high-temperature resistant metal cup and the hard alloy substrate layer are treated with high cleanliness. However, as mentioned above, there are still residual impurities on the surface of the diamond particles, and air, including oxygen and nitrogen, is in the gaps in the raw material mixture of the polycrystalline diamond working layer. These impurities still affect the performance of polycrystalline diamond compacts synthesized from coarse-grained diamond particles.
Prior to synthesis, a schematic cross-sectional structure of a polycrystalline diamond compact is shown in fig. 1. The polycrystalline diamond working layer 10 raw material mixture and the cemented carbide base layer alloy 20 are in a metal cup 60. The diamond primary particle size particles 30 are naturally stacked and uniformly distributed after being pressed under a pressure of less than 10 MP. The diamond secondary particle size particles 40 are uniformly distributed on the surface of the diamond primary particle size 30. The voids 50 in the polycrystalline diamond working layer feedstock mixture are air, and the volume of the voids is the volume of air. At room temperature before the polycrystalline diamond compact is synthesized, the porosity of the polycrystalline diamond working layer raw material mixture is about 40%. In the raw material mixture of the polycrystalline diamond working layer 10, the diamond main particle size particles 30, the diamond auxiliary particle size particles 40, the getter on the close contact surface of the diamond auxiliary particle size particles, silicon and metal oxide impurities and air are uniformly distributed and coexist.
And preparing the polycrystalline diamond compact, namely synthesizing the polycrystalline diamond compact at high temperature and high pressure. The synthesis pressure is 6500-7500MPa, the first-stage synthesis temperature is 1173.15-1373.15K, and the synthesis time is 3.5-6 minutes; the second stage synthesis temperature is 1723.15-1823.15K. The synthesis heating time is 8-16 minutes.
In the first stage of synthesis pressing, the cross-sectional structure of the polycrystalline diamond working layer 10 is schematically shown in fig. 2. The pressure of a synthesis cavity in the synthesis process is 6500-7500MPa, and the sintering temperature reaches 1173.15-1373.15K. The polycrystalline diamond working layer feedstock mixture 10 is highly compressed by about 70% and is almost uncompressed in the radial direction. Crystals of the irregularly shaped diamond primary particle size particles 30 start to deform, and diamond primary particle size particles 30 of the hexaoctahedral intact crystals are deformed little. The diamond secondary particle size particles 40 are compressively deformed or crushed at the close contact surface of the diamond primary particle size particles 30. The voids 50 in the polycrystalline diamond working layer feedstock mixture are compressed by a factor of about 10 and the air in the voids 50 is compressed by a factor of 10. The pressure of the void air at this time was about 4 MPa. The low pressure surface of the interstitial diamond crystals begins to graphitize.
The impurities silicon and metal on the surface of the diamond particles exist in the form of oxides. The non-metal oxide silicon oxide, the metal oxide calcium oxide, the metal oxide chromium oxide, the metal oxide iron oxide, the metal oxide magnesium oxide, the metal oxide manganese oxide, the metal oxide sodium oxide, the metal oxide nickel oxide, the metal oxide aluminum oxide and the like can be melted into the graphitized layer and are not easy to be taken away when cobalt is scanned and permeated.
In addition, oxygen in the interstices 50 between the diamond crystals reacts with the graphitized carbon to form oxycarbides which disrupt the graphite structure. The nitrogen in the voids slows down the growth of graphite, and the gas pressure is not conducive to graphitization.
To eliminate the adverse effects of oxides and oxygen and nitrogen, one or more degassing agents are added to the raw material mixture 10 of the polycrystalline diamond working layer of the present invention. These degassing agents are metallic zirconium powder, zirconium copper alloy, zirconium aluminum alloy, zirconium nickel alloy, zirconium carbide or compounds of metallic titanium powder, titanium alloy, titanium carbide and the like. The proportions are 0.1% to 3.0% respectively.
The melting point of the degassing agent is low and the molten degassing agent compound will dissolve the oxide of the uncompressed surface of the diamond primary particles 30 and diamond secondary particles 40 crystals at the temperature of the first stage. The melted degasifier compounds penetrate into crystal gaps of the primary diamond grain size particles 30 and the secondary diamond grain size particles 40 to dissolve the oxides. And cleaning the diamond surface. The molten degasser compound may also absorb oxygen and nitrogen in the voids, reducing or eliminating the gas pressure within voids 50. As mentioned above, a high cleanliness environment is created, and a high purity graphite layer is produced on the surface of the diamond crystal in the graphitization process.
In the second stage, the pressure of the synthesis cavity is 6500-7500MPa in the synthesis process, and the sintering temperature is raised to 1723.15-1823.15K in the second stage. Cobalt in the cemented carbide substrate layer sweeps across the polycrystalline diamond working layer raw material mixture voids 50 for cobalt infiltration. The interstices 50 of the polycrystalline diamond working layer feedstock mixture continue to be compressed by a factor of more than 17. When the primary diamond grain size 30 is between 35 microns and 275 microns, the interstices 50 of the polycrystalline diamond working layer feedstock mixture are compressed 17-27 times. The polycrystalline diamond working layer is highly compressed to 70% and below.
In the second stage, when the temperature exceeds 1573.15K, the cobalt in the cemented carbide substrate layer rapidly sweeps into the cobalt penetration line of the polycrystalline diamond working layer 10. After getters and silicon and metal oxide impurities in crystal planes of tight contact surfaces among the diamond main particle size particles 30, the diamond auxiliary particle size particles 40 and the diamond main particle size particles 30 and the diamond auxiliary particle size particles 40 are melted in cobalt liquid, the silicon and metal oxide impurities are dissolved in the adjacent getters, and the surface of the diamond is cleaned.
The front cobalt liquid brings the getters, which are melted into the oxides and absorb oxygen and nitrogen, to the upper surface of the polycrystalline diamond working layer 10, forming a diamond surface layer 70 containing impurities. Subsequent processing will remove the contaminated diamond surface layer 70 and the portion of the polycrystalline diamond working layer adjacent thereto.
After the cobalt liquid fills the gap, the diamond crystals in the whole polycrystalline diamond working layer have the same pressure as the cobalt liquid, and the cobalt liquid can permeate into the diamond crystal face which is originally in close contact with the cobalt liquid. The whole crystal face of the diamond particle is accelerated to graphitize under the action of cobalt. The cobalt solution will then dissolve the graphite on the diamond surface. When the graphite in the cobalt solution is supersaturated, the graphite starts to generate the recrystallized diamond 80 between the crystal faces of the diamond 30 and the diamond 40 under the action of the catalyst of the cobalt. After the synthesis is completed, most of the crystal faces of the primary diamond grain size particles 30 and the secondary diamond grain size particles 40 in the polycrystalline diamond working layer 10 form diamond bonding bonds as shown in fig. 3.
This application adopts 35 microns to 275 microns's diamond major diameter, in the synthetic sintering, can form wide cobalt seepage line, and the resistance that wide cobalt seepage line oozed cobalt is little, oozes cobalt fast, and the ability of taking away getter in the space and impurity is big to make diamond recrystallization's graphite purity high, the environmental cleaning, the good quality of recrystallization diamond, the quantity of recrystallization diamond is many, and the bonding ability of formation is strong. Thereby making the diamond compact of the present application have high chipping resistance, high impact strength, high wear resistance, and a finished surface finish.
The invention is described above with reference to the accompanying drawings as an example, in so far as it is a insubstantial improvement in the method concept and technical solutions of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.
Claims (8)
1. The utility model provides a polycrystalline diamond compact, polycrystalline diamond compact comprises polycrystalline diamond working layer and carbide base layer, its characterized in that: the polycrystalline diamond working layer is prepared from a mixture of a degassing agent and diamond particles with certain surface cleanliness, and the porosity of the polycrystalline diamond working layer is 30% -45% at room temperature; the diamond particles consist of diamond primary particle size particles and diamond secondary particle size particles, and the particle size of the diamond primary particle size particles is 35-275 microns; the grain diameter of the diamond auxiliary grain size particles is less than or equal to 1/4 grain diameter of the diamond main grain size particles, and the weight percentage of the diamond main grain size particles in the diamond grains is 70-100%; the degassing agent accounts for 0.1-3.0% of the weight of the diamond particles; the hard alloy base layer is made of tungsten carbide containing cobalt.
2. The polycrystalline diamond compact of claim 1, wherein: the degassing agent is one or more of metal zirconium powder, zirconium copper alloy, zirconium aluminum alloy, zirconium nickel alloy, zirconium carbide, metal titanium powder, titanium alloy and titanium carbide.
3. A polycrystalline diamond compact according to claim 1 or claim 2, wherein: the cobalt content of the cemented carbide substrate layer is 12-16 wt%.
4. A polycrystalline diamond compact according to claim 3, wherein: the surface cleanliness of the diamond particles was: the grain diameter of the diamond particles is less than 3 microns, and the surface impurity content of the diamond particles is less than 55 ppm; the grain diameter of the diamond particles is 3-40 microns, and the surface impurity content of the diamond particles is less than 40 ppm; the grain diameter of the diamond particles is 40-60 microns, and the surface impurity content of the diamond particles is less than 27 ppm; the diamond particles have a particle size of greater than 60 microns and a surface impurity level of less than 15 ppm.
5. A method of making a polycrystalline diamond compact according to any one of claims 1 to 4, wherein: placing the raw materials of the polycrystalline diamond working layer on a hard alloy substrate layer, and sintering and synthesizing the polycrystalline diamond working layer through two sections of high temperature and high pressure;
high temperature and high pressure in the first stage: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1173.15-1373.15K, and the synthesis heating time is 3.5-6 minutes;
second-stage high-temperature high-pressure: the synthesis pressure is 6500-7500MPa, the synthesis temperature is 1723.15-1823.15K, and the synthesis heating time is 8-16 minutes.
6. The method of making a polycrystalline diamond compact of claim 5, wherein: the diamond particles are divided into a plurality of granularity sections according to the average particle size, the main granularity of the diamond particles is selected from one granularity section or the mixture of two to three adjacent granularity sections, and the auxiliary granularity of the diamond particles is selected from one granularity section or the mixture of a plurality of finer granularity sections.
7. The method of making a polycrystalline diamond compact of claim 6, wherein: the raw material of the polycrystalline diamond working layer and the hard alloy basal layer are placed in a high-temperature resistant metal cup during sintering synthesis.
8. The method of making a polycrystalline diamond compact of claim 7, wherein: the high-temperature resistant metal cup is made of one or a combination of more of tantalum, molybdenum, niobium and zirconium.
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