CN114700494A - Preparation method of polycrystalline diamond compact - Google Patents
Preparation method of polycrystalline diamond compact Download PDFInfo
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- CN114700494A CN114700494A CN202111525281.9A CN202111525281A CN114700494A CN 114700494 A CN114700494 A CN 114700494A CN 202111525281 A CN202111525281 A CN 202111525281A CN 114700494 A CN114700494 A CN 114700494A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/10—Sintering only
- B22F3/1039—Sintering only by reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
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Abstract
The invention provides a preparation method of a polycrystalline diamond compact, which comprises the following steps: A) sequentially stacking titanium powder, diamond micro powder and tungsten carbide hard alloy; B) and B) sintering the assembly block obtained in the step A) at high temperature and high pressure to obtain the polycrystalline diamond compact. In the preparation process, metal titanium powder is added at the bottom and reacts with air in the inner core to generate TiO in the pressurizing and heating process2And TiN, so that the gas in the inner core is reduced, and the inner core achieves the purpose of removing the gas, thereby improving the wear resistance and the density of the polycrystalline diamond compact.
Description
Technical Field
The invention relates to the field of preparation of superhard composite materials, in particular to a preparation method of a polycrystalline diamond compact.
Background
Polycrystalline diamond compact is a superhard composite material, and micron-sized diamond particles and a hard alloy tungsten carbide substrate with the thickness of several millimeters are sintered together by using a static high-temperature high-pressure method (cubic press). Therefore, the polycrystalline diamond compact not only has the high hardness and the high wear resistance of polycrystalline diamond, but also has the impact toughness and the machinability of hard alloy, and is widely applied to the fields of petroleum geological drilling, mechanical processing and the like.
Polycrystalline diamond compacts, which are used as cutting teeth of petroleum geological drilling bits, are required to have extremely high wear resistance, impact resistance and thermal stability. Along with the continuous promotion of compound piece and compound piece drill bit performance in recent years, the use proportion of compound piece is constantly improving, and good development trend appears in the trade. However, compared with the domestic composite sheet, the domestic composite sheet has a large gap in performance, so that the domestic composite sheet is limited in selling price and application range, and the domestic composite sheet is difficult to enter in oil fields with complex geological conditions and in the world of the foreign composite sheet. Therefore, the performance of the polycrystalline diamond compact is improved, and the method has important significance.
In the synthesis process of the polycrystalline diamond compact, the inner surface of the metal cup cover, the diamond grains, the surface of the hard alloy and the like cannot reach a completely gasification-free state from the microscopic molecular structure of the interface reaction, namely the actual PDC sheet interface synthesis reaction is sintering and connection reaction on a solid interface under the influence of gas films included in different degrees. In this sense, it is necessary to try to improve the depth of the cleaning process at the interface so that the actual interface reactions can achieve a reaction bond as close as possible to the ideal clean interface. This has a significant impact on improving the performance and yield of polycrystalline diamond compacts.
The air-exhaust purification treatment process of the inner core in the manufacturing process of the polycrystalline diamond compact is characterized in that the inner core is pre-pressed when diamond micro powder is filled, so that the doping and mixing of an adsorbed gas film caused by powder filling can be reduced, but gas still exists in the inner core, the gas in the inner core can not be discharged during high-temperature and high-pressure sintering, gaps are left in the polycrystalline diamond compact, the more the gaps are, the weaker the bonding force of diamond-diamond bonds among grains is, the more Co is needed to be used to enable diamond to be fully bonded, but the strength of the compact after cobalt removal is reduced more, and the overall performance of the compact is influenced.
In summary, how to effectively reduce the amount of gas in the inner core during the manufacturing process is an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of a polycrystalline diamond compact, which can consume gas in an inner core and improve the wear resistance and density of the polycrystalline diamond compact.
In view of this, the present application provides a method for preparing a polycrystalline diamond compact, including the steps of:
A) sequentially stacking titanium powder, diamond micro powder and tungsten carbide hard alloy;
B) and B) sintering the assembly block obtained in the step A) at high temperature and high pressure to obtain the polycrystalline diamond compact.
Preferably, the diamond micro powder further comprises cobalt powder, and the mass ratio of the diamond micro powder to the cobalt powder is (90-95): (5-10).
Preferably, the granularity of the diamond micro powder is 20-30 μm, and the granularity of the cobalt powder is 1-5 μm.
Preferably, the mass ratio of the titanium powder to the diamond micro powder is (0.03-0.05): 1.5.
preferably, the sintering temperature is 1200-1500 ℃, and the time is 2-10 min.
Preferably, the sintering pressure is 5-6 GPa.
Preferably, the step a) is preceded by: reduction treatment of titanium powder and impurity removal treatment of diamond micropowder.
Preferably, the preparation method of the polycrystalline diamond compact specifically comprises the following steps:
a1) purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the tungsten carbide hard alloy by using machining;
b1) mixing the diamond micro powder and the cobalt powder;
c1) putting Ti powder into the bottom of a metal cup, paving, then putting the mixed diamond micro powder, flattening, then putting hard alloy, and buckling a buckling cup;
d1) and (3) putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering.
The application provides a preparation method of a polycrystalline diamond compact, which is characterized in that metal titanium powder is added at the bottom and reacts with air in an inner core in the pressurizing and heating process to generate TiO2TiN, reduce the gas in the inner core, make the inner core reach the purpose of going gasification to improve polycrystalline diamond compact's wearability and density, and strong nitrogen compound TiN can form stable compound on the diamond surface, improve polycrystalline diamond compact's compactness and thermal stability.
Drawings
Fig. 1 is a schematic view of the structure of an inner core of a polycrystalline diamond compact during the manufacturing process of the present invention;
FIG. 2 is a photograph of an example of an off-specification polycrystalline diamond compact with excess Ti powder added;
FIG. 3 is a light load test chart of samples prepared with and without Ti powder added in accordance with the present invention;
FIG. 4 is a graph showing the heavy load test of the samples prepared with and without Ti powder according to the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the problem that gas exists in the inner core during the preparation of the polycrystalline diamond compact in the prior art, the application provides a preparation method of the polycrystalline diamond compact, which effectively consumes the gas in the inner core by introducing Ti powder and arranging the Ti powder at the bottom end of the compact, and finally improves the wear resistance and the density of the polycrystalline diamond compact. Specifically, the embodiment of the invention discloses a preparation method of a polycrystalline diamond compact, which comprises the following steps:
A) sequentially stacking titanium powder, diamond micro powder and tungsten carbide hard alloy;
B) and B) sintering the assembly block obtained in the step A) at high temperature and high pressure to obtain the polycrystalline diamond compact.
In polycrystalline diamond compact's preparation process, this application first looks stack titanium powder, diamond miropowder and tungsten carbide in proper order and place. In the process, the granularity of the diamond micro powder is 20-30 microns, and the diamond micro powder also comprises cobalt powder, wherein the granularity of the cobalt powder is 1-5 microns. The mass ratio of the diamond micro powder to the cobalt powder is (90-95): the polycrystalline diamond compact comprises (5-10) diamond powder and cobalt powder, wherein the mass ratio of the diamond powder to the cobalt powder is 94:6, the cobalt powder is used as a binder and exists in the diamond powder, the sources of the titanium powder, the diamond powder and tungsten carbide hard alloy are not particularly limited, the mass ratio of the titanium powder to the diamond powder is (0.05-0.05): 1.5, and the polycrystalline diamond compact has cracks at the bottom end due to the fact that the content of the titanium powder is too high, so that the yield of products is reduced.
The obtained assembly block is sintered at high temperature and high pressure to obtain a polycrystalline diamond compact; in the process, Ti powder reacts with air in the inner core to generate TiO2And TiN. The sintering temperature is 1200-1500 ℃, the time is 2-10 min, and the pressure is 5-6 GPa; more specifically, the sintering temperature is 1280-1460 ℃, the time is 3-8min, and the pressure is 5.2-5.6 GPa.
The process of preparing the polycrystalline diamond compact specifically comprises the following steps:
1) purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining;
2) mixing the micro powder and the binder cobalt in advance according to a proportion, and dry-mixing for 2 hours in a mixer;
3) baking and dehumidifying the pyrophyllite, steel rings, magnesium tubes, carbon tubes and other accessories;
4) putting Ti powder into the bottom of a metal cup, paving, then putting the mixed diamond micro powder, flattening, then putting hard alloy, and buckling a buckling cup;
5) putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, specifically selecting a 6 x 800 ton cubic press, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and releasing the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
The application provides a method for consuming gas in the process of sintering a polycrystalline diamond compact at high temperature and high pressure, which comprises the steps of adding metal Ti powder to the bottom end of a sample, and reacting with air in an inner core to generate TiO in the process of pressurizing and heating2TiN is used for reducing gas in the inner core, so that the inner core achieves the purpose of gasification removal, and the wear resistance and the density are improved; and the strong nitrogen compound TiN can form a stable compound on the surface of the diamond, so that the compactness and the thermal stability of the polycrystalline diamond compact are improved.
For further understanding of the present invention, the method for preparing the polycrystalline diamond compact provided by the present invention is described in detail with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the pyrophyllite, steel rings, magnesium tubes, carbon tubes and other accessories; placing 0.50g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and buckling a metal buckle cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
Example 2
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the pyrophyllite, steel rings, magnesium tubes, carbon tubes and other accessories; placing 0.40g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and fastening a metal button cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
Example 3
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the assistant parts such as pyrophyllite, steel rings, magnesium pipes, carbon tubes and the like; placing 0.30g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and fastening a metal button cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
Example 4
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the assistant parts such as pyrophyllite, steel rings, magnesium tubes, carbon tubes and the like. Placing 0.20g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and fastening a metal button cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
Example 5
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the pyrophyllite, steel rings, magnesium tubes, carbon tubes and other accessories; placing 0.10g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and fastening a metal button cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
Example 6
Purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the hard alloy by using machining; mixing the micro powder and the binder cobalt in advance according to a certain proportion (the granularity of the diamond micro powder is 20-30 mu m, the granularity of the binder cobalt powder is 1 mu m, and the proportion of the diamond micro powder and the binder cobalt powder is 94:6), and dry-mixing for two hours in a mixer; baking and dehumidifying the pyrophyllite, steel rings, magnesium tubes, carbon tubes and other accessories; placing 0.03g of Ti powder (10 mu m) into the bottom of a metal cup, paving, then placing 1.5g of mixed diamond micro powder, flattening, finally placing tungsten carbide hard alloy, and buckling a metal buckle cup; putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering; adopting a conventional sintering process, selecting a 6 multiplied by 800 ton cubic press for experiments, increasing the pressure of the press to 5.6GPa, then heating and maintaining the pressure according to the preset heating power, sintering the synthesized block at high temperature and high pressure according to the heat preservation time, and beginning to release the pressure after the synthesized block is cooled for a period of time; wherein the sintering temperature range is 1280-1460 ℃, and the heat preservation time is 3-8 min.
In the embodiment, the polycrystalline diamond compact is synthesized into 20 pieces, the finished product is 7-10 pieces, and the rest are defective products or waste products, wherein the yield is 35-60%, and the yield is low; the polycrystalline diamond compact of examples 1-6 had a mass of 39.6 g.
Example 7
When the addition of Ti powder is excessive, the cup bottom containing the synthesized Ti powder has cracks, which are obvious, and the blocks are more dropped after sand blasting, as shown in figure 2. Therefore, when the amount of the filled micro powder is fixed, different amounts of Ti powder are required to be added for experiments so as to determine the optimal powder filling amount.
The other steps are the same as in example 1, except that: the mass of the filled powder (diamond micro powder and cobalt powder) is 1.5g, when 0.10-0.50 g of Ti powder is added, 20 pieces are synthesized, 7-10 finished products are obtained, and the rest are defective products or waste products, wherein the yield is 35-60%; when 0.03-0.05 g of Ti powder is added, 20 sheets are synthesized, 16-18 finished products are obtained, and other defective products or waste products are obtained, wherein the yield can reach 80-90%, and the yield is the highest.
Example 8
The other steps are the same as in example 1, except that: adding 0.03-0.05 g of Ti powder, and testing the porosity of the diamond layer after the experiment, which shows that the Ti powder can enable the diamond layer to be more compact;
Ti+O2→TiO2；2Ti+N2→2TiN
porosity test method: the method comprises the following steps of (1) sampling, a constant-temperature drying box, a balance, experimental reagent distilled water and a beaker;
step 1: the determination of the porosity is based on the Archimedes principle, and the porosity is determined by adopting a boiling method in the test; firstly, weighing the required dry weight of a sample, and recording the dry weight as m 0;
step 2: putting the weighed sample into a clean beaker, and injecting distilled water into the beaker until the sample is submerged;
and step 3: then, placing the beaker in a constant-temperature drying oven, heating to boil, and keeping the boiling state for 2 hours to ensure that the distilled water completely permeates into the gap;
and 4, step 4: the heating was then stopped and allowed to cool to room temperature. Then, quickly taking out the sample, putting the sample into a small basket prepared for weighing in advance, hanging the small basket on a lifting hook of a balance to enable the sample to be continuously immersed in water, and weighing the suspended weight of the saturated sample in the water, wherein the suspended weight is recorded as m 1;
and 5: the saturated sample was taken out, the surface of the saturated sample was carefully wiped off with a moist wipe, and the mass of the saturated sample was quickly weighed and recorded as m 2.
Step 6: the porosity of the electrode was calculated by the formula: p ═ m2-m0)/(m2-m 1);
table 1 table of porosity data for samples prepared with and without Ti powder addition
| Sample number | Porosity of the material |
| Adding Ti powder sample | 3.20-3.30％ |
| Normal process sample | 3.45-3.55％ |
As can be seen from table 1, the porosity of the added Ti powder is lower than that of the normal process, which indicates that the diamond layer can be more dense by adding the Ti powder;
example 9
The other steps are the same as in example 1, except that: and adding 0.03-0.05 g of Ti powder, and placing the prepared polycrystalline diamond compact on a vertical lathe clamp to start stone grinding to test the abrasion ratio.
Table 2 light load test data table of samples prepared with and without Ti powder addition
Table 3 table of heavy load test data of samples prepared with and without Ti powder addition
Note: in the table, the abrasion ratio of light load and heavy load fluctuates between +/-10% of lower data.
As can be seen from the light load test results in table 2 and fig. 3, the test wear surface is smooth and higher than the normal formulation without Ti powder under the same conditions, which indicates that the diamond is tightly bonded and the diamond-diamond bond bonding strength is high, so that the service life of the polycrystalline diamond compact can be prolonged in the use process; when the composite sheet is subjected to cobalt removal and the cobalt removal depth is 500 mu m, a vertical lathe is used for testing heavy load, and as can be seen from table 3 and fig. 4, the wear resistance of the composite sheet added with Ti powder is improved by nearly 40% compared with that of the composite sheet added with Ti powder in a normal process.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of a polycrystalline diamond compact comprises the following steps:
A) sequentially stacking titanium powder, diamond micro powder and tungsten carbide hard alloy;
B) and B) sintering the assembly block obtained in the step A) at high temperature and high pressure to obtain the polycrystalline diamond compact.
2. The preparation method according to claim 1, wherein the diamond micro powder further comprises cobalt powder, and the mass ratio of the diamond micro powder to the cobalt powder is (90-95): (5-10).
3. The method according to claim 2, wherein the diamond fine powder has a particle size of 20 to 30 μm, and the cobalt powder has a particle size of 1 to 5 μm.
4. The production method according to claim 1 or 2, wherein the mass ratio of the titanium powder to the diamond micro powder is (0.03-0.05): 1.5.
5. the method according to claim 1 or 2, wherein the sintering temperature is 1200 to 1500 ℃ and the sintering time is 2 to 10 min.
6. The production method according to claim 1 or 2, wherein the sintering pressure is 5 to 6 GPa.
7. The method of claim 1 or 2, wherein step a) is preceded by: reduction treatment of titanium powder and impurity removal treatment of diamond micropowder.
8. The method according to any one of claims 1 to 7, wherein the polycrystalline diamond compact is prepared by a method comprising:
a1) purifying the metal cup by using a vacuum furnace, removing impurities from the diamond micro powder, reducing the Ti powder, and removing oil and rust from the tungsten carbide hard alloy by using machining;
b1) mixing the diamond micro powder and the cobalt powder;
c1) putting Ti powder into the bottom of a metal cup, paving, then putting the mixed diamond micro powder, flattening, then putting hard alloy, and buckling a buckling cup;
d1) and (3) putting the assembled inner core into a pyrophyllite block for assembly, and finally putting the assembled synthetic block into a cavity of a cubic press for high-temperature high-pressure sintering.
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| CN115740456A (en) * | 2022-12-12 | 2023-03-07 | 富耐克超硬材料股份有限公司 | Polycrystalline diamond compact and preparation method thereof |
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