CN109706340B - Fine-grained diamond polycrystal and preparation method thereof - Google Patents
Fine-grained diamond polycrystal and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fine-grained diamond polycrystal and a preparation method thereof, wherein the method comprises the following steps: dissolving cobalt salt and a dispersing agent in a solvent, adding diamond micro powder and uniformly mixing to obtain a mixed solution; dropwise adding an alkaline solution into the mixed solution until cobalt is completely precipitated, and filtering to obtain a solid mixture; placing the solid mixture in an oxygen-containing atmosphere for calcination treatment, then placing the calcined product in vacuum or reducing atmosphere and heating for oxidation-reduction reaction to obtain cobalt-containing diamond micro powder; putting the diamond micro powder into a metal cup, coating a layer of metal cobalt on the surface layer of the diamond micro powder, then carrying out vacuum treatment, and then pressurizing and sintering to obtain the fine-grained diamond polycrystal. The invention solves the problem that the polycrystalline stress sintered under the conditions of high temperature and high pressure in the prior art is large and cracks are easy to generate.
Description
Technical Field
The invention relates to the technical field of diamond processing, in particular to a fine-grained diamond polycrystal and a preparation method thereof.
Background
The fine grain diamond polycrystal is made up by sintering diamond micropowder of 0-3 micrometers and metal cobalt under the condition of high temp. and high pressure, and is a sintered body mainly formed from diamond micropowder and cobalt, and possesses the characteristics of high hardness and high wear resistance, at the same time, because the diamond crystal grain is small, it has the characteristic of small edge, so that it is an ideal material for making high-quality cutting tool and wire-drawing die.
The polycrystalline stress sintered under the condition of high temperature and high pressure is large, so that cracks are easy to generate, and the grain growth phenomenon is easy to generate due to the fine grain size of the diamond micro powder.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a fine-grained diamond polycrystal and a preparation method thereof, and aims to solve the problem that the existing fine-grained diamond polycrystal is easy to crack due to large stress of the sintered polycrystal under high-temperature and high-pressure conditions during preparation.
The technical scheme of the invention is as follows:
a preparation method of fine-grained diamond polycrystal comprises the following steps:
dissolving cobalt salt and a dispersing agent in a solvent, adding diamond micro powder and uniformly mixing to obtain a mixed solution;
dropwise adding an alkaline solution into the mixed solution until cobalt is completely precipitated, and filtering to obtain a solid mixture;
placing the solid mixture in an oxygen-containing atmosphere for calcination treatment, then placing the calcined product in vacuum or reducing atmosphere and heating for oxidation-reduction reaction to obtain cobalt-containing diamond micro powder;
putting the diamond micro powder into a metal cup, coating a layer of metal cobalt on the surface layer of the diamond micro powder, then carrying out vacuum treatment, and then pressurizing and sintering to obtain the fine-grained diamond polycrystal.
The preparation method of the fine-grained diamond polycrystal comprises the step of mixing cobalt with diamond according to a mass ratio of 0.1-5: 95-99.9.
The preparation method of the fine-grained diamond polycrystal comprises the step of preparing a fine-grained diamond polycrystal by using a cobalt salt, wherein the cobalt salt is one or more of cobalt chloride, a cobalt chloride hydrate compound, cobalt nitrate, a cobalt nitrate hydrate compound, cobalt sulfate, a cobalt sulfate hydrate compound, cobalt carboxylate, a cobalt carboxylate hydrate compound, cobalt oxalate and a cobalt oxalate hydrate compound.
The preparation method of the fine-grained diamond polycrystal comprises the step of preparing a fine-grained diamond polycrystal, wherein the dispersant is polyethylene glycol.
The preparation method of the fine-grained diamond polycrystal comprises the step of preparing a fine-grained diamond polycrystal, wherein the solvent is water, methanol, ethanol or acetone.
The preparation method of the fine-grained diamond polycrystal comprises the step of preparing a polycrystalline silicon film by using a base solution, wherein the base solution is one or a combination solution of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonia carbonate, ammonium bicarbonate and ammonia water.
The preparation method of the fine-grained diamond polycrystal comprises the step of preparing a diamond fine powder with the grain size of 0-3 mu m.
The preparation method of the fine-grained diamond polycrystal is characterized in that the reducing gas is hydrogen or carbon monoxide.
The preparation method of the fine-grained diamond polycrystal comprises the steps of calcining at 400-700 ℃, heating at 400-1200 ℃, and pressurizing to sinter at 1200-1600 ℃ and 5.5-8.0 GPa.
A fine-grained diamond polycrystalline, wherein the fine-grained diamond polycrystalline is prepared by the method.
Has the advantages that: according to the invention, the diamond micro powder is treated firstly, metal cobalt is dispersed and doped in the diamond micro powder, then the diamond micro powder doped with the metal cobalt is filled into the metal cup, and a layer of metal cobalt is added on the surface layer, so that when high-temperature and high-pressure sintering is carried out, the metal cobalt on the surface and the metal cobalt doped in the diamond micro powder can be simultaneously utilized to catalyze the uniform distribution among diamond particles to generate D-D bonds, a diamond polycrystal with higher bonding strength is formed, the wear resistance of a product is improved, and the problem that the polycrystalline sintered under the high-temperature and high-pressure conditions in the prior art has larger stress and is easy to crack is solved.
Drawings
Fig. 1 is a flow chart of a preferred embodiment of the method for preparing fine-grained polycrystalline diamond according to the present invention;
fig. 2 is an SEM image of polycrystalline a diamond prepared in example 1;
fig. 3 is an SEM image of polycrystalline B diamond prepared in example 2;
fig. 4 is an SEM image of polycrystalline C diamond prepared in example 3.
Detailed Description
The invention provides a fine-grained diamond polycrystalline and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation method of the fine-grained diamond polycrystal, disclosed by the invention, as shown in figure 1, comprises the following steps of:
s1, dissolving cobalt salt and a dispersing agent in a solvent, adding diamond micro powder, and uniformly mixing to obtain a mixed solution;
s2, dropwise adding an alkaline solution into the mixed solution until cobalt is completely precipitated, and filtering to obtain a solid mixture;
s3, placing the solid mixture in an oxygen-containing atmosphere for calcination, then placing the calcined product in vacuum or reducing atmosphere and heating for oxidation-reduction reaction to obtain cobalt-containing diamond micropowder;
s4, putting the diamond micro powder into a metal cup, coating a layer of metal cobalt on the surface of the diamond micro powder, then carrying out vacuum treatment, and then pressurizing and sintering to obtain the fine-grained diamond polycrystal.
The invention uniformly dopes a certain amount of metal cobalt among the diamond micro-powder in advance so as to improve the uniformity of cobalt metal distribution among the diamond micro-powder particles, can ensure that the metal cobalt catalyzes the diamond particles to uniformly distribute and generate D-D bonds during the subsequent high-temperature high-pressure sintering treatment, and simultaneously, before the diamond micro-powder is sintered at high temperature and high pressure, a layer of cobalt metal is deposited on the upper surface layer of the diamond micro-powder layer, so that the cobalt metal on the surface is melted and the diamond on the surface layer is uniformly wetted during the high-temperature high-pressure sintering of the diamond micro-powder, meanwhile, the metal cobalt on the surface can also permeate downwards to lubricate the diamond micro-powder inside and under the diamond micro-powder to form more D-D bonds, further eliminate the possibility that the D-D bonds cannot be formed among the diamond particles inside due to uneven distribution of the cobalt metal to generate internal, the wear resistance of the diamond compact is improved, and the problem that the sintered polycrystalline stress is large and cracks are easy to generate under the high-temperature and high-pressure condition is solved. In addition, the method can avoid the phenomenon that the diamond micro powder is easy to grow because of fine particle size.
Preferably, before step S1, the diamond fine powder is purified (e.g., acid-base purification) to an impurity content of less than 100ppm, and more preferably to an impurity content of less than 50ppm, such as Fe, Ni, Mn, Cr, Al, Ca, Mg, Si, etc. And removing impurities on the surface and in the internal gaps of the diamond micropowder to realize better polycrystalline effect and avoid the adverse effect of the impurities on the performance of a final product.
In the step S1, the cobalt salt and the dispersant are dissolved in the solvent, the cobalt salt is fully dispersed by the action of the dispersant, and then the diamond micro powder is added under the action of ultrasonic stirring to uniformly mix the diamond micro powder and the cobalt salt, so as to obtain a mixed solution. Preferably, the diamond micro powder in the invention has a particle size in the range of 0-3 microns (for example, 0-0.7 μm, 0.5-1 μm, 0.9-1.5 μm or 2-3 μm) to ensure the fine particle size of the prepared product. In the mixed liquid, the mass ratio of cobalt element to diamond is 0.1-5: 95-99.9 by controlling the adjustment ratio of cobalt salt to diamond micro powder, if the content of metal cobalt in the content range is too low, the requirement of catalyzing formation of a D-D bond structure between the diamond micro powder can not be met, and if the content of metal cobalt is too high, a large thermal residual stress can be formed due to the difference of the thermal expansion coefficients of the cobalt metal and the diamond, so that the diamond composite sheet has the phenomena of non-wear resistance, sheet breakage and the like in the working process.
The cobalt salt is one or more of cobalt chloride, cobalt chloride hydrate compound, cobalt nitrate hydrate compound, cobalt sulfate hydrate compound, cobalt carboxylate hydrate compound, cobalt oxalate and cobalt oxalate hydrate compound. The dispersant is preferably polyethylene glycol, and the cobalt salt is particularly well dispersed; more preferably, the molecular weight of the polyethylene glycol is 400-: 100. the solvent may be water, methanol, ethanol or acetone.
In the step S2, an alkaline solution is added dropwise to the mixed solution under ultrasonic stirring, cobalt ions are precipitated and separated out in the form of cobalt hydroxide by using the alkaline solution, and after the cobalt precipitation is completed, the cobalt ions are continuously subjected to ultrasonic treatment and stirred for a period of time, filtered, washed and dried in vacuum at a temperature not exceeding 60 ℃, so as to remove other impurities brought in by the cobalt plating process, realize a better polycrystalline effect and obtain a solid mixture with the main components of cobalt hydroxide and diamond micropowder.
In step S3, the solid mixture is calcined in an oxygen-containing atmosphere (such as oxygen or air), so that impurities such as dispersants and solvents doped in the solid mixture are oxidized into gas to be removed, meanwhile, impurities in the diamond micro powder can also be removed under the action of calcination, and cobalt hydroxide is calcined into cobalt oxide, thereby obtaining a calcined product formed by mixing pure cobalt oxide and diamond micro powder; preferably, the calcining temperature in the step S3 is 400 to 700 ℃, the dispersant and the solvent can be fully calcined into a gas state at the temperature, the calcining purpose cannot be realized at too low temperature, and the loss of the diamond micropowder and unnecessary energy consumption are caused at too high temperature; more preferably, the calcination treatment time is 1-5h, i.e. the dispersant, the solvent and the like can be fully burnt out.
In the step S3, the calcined product obtained by mixing pure cobalt oxide with the diamond fine powder is placed in a vacuum or reducing gas atmosphere, and the cobalt oxide in the calcined product is reduced to metallic cobalt by heating, so as to obtain pure diamond fine powder containing metallic cobalt, wherein the cobalt content in the diamond fine powder is 0.1 to 5%, preferably 1.5 to 3%, the cobalt content is too low to fully infiltrate diamond particles during sintering to form D-D bonds, and the diamond polycrystalline strength is lowered due to the fact that the content of diamond is too high. The zirconium oxide can be reduced into metal cobalt at the heating temperature of 400-1200 ℃, the reduction temperature cannot be reached at too low heating temperature, and the loss of diamond micropowder can be caused at too high temperature; preferably, the heat treatment time is 1 to 6 hours, which is too short to sufficiently reduce the zirconia to metallic cobalt. Wherein the reducing gas is hydrogen or carbon monoxide.
In the step S4, the diamond micro powder is put into a metal cup, a layer of metal cobalt is coated on the surface of the diamond micro powder, then vacuum treatment is performed to exhaust air, and then the metal cobalt is put into a high-pressure device to be pressurized to be sintered, because the metal cobalt is melted into liquid and permeates among diamond particles under the high-pressure and high-temperature environment, the diamond particles are partially dissolved in the melted cobalt metal under the high-temperature and high-pressure environment, when the solubility of diamond in the liquid-phase cobalt metal reaches saturation, diamond crystals are re-precipitated, so that the diamond particles are connected with each other to generate D-D bonds, and diamond polycrystalline crystals are formed. Because metal cobalt is doped and dispersed in the diamond micro powder and a layer of metal cobalt is added on the surface layer of the diamond micro powder, the combined action of the metal cobalt and the metal cobalt can enable more uniform D-D bonds to be formed in the diamond micro powder, eliminate the internal stress caused by uneven distribution of the D-D bonds and avoid cracks; the more and more the D-D bonds are formed, the more uniform the strength, impact toughness and wear resistance of the polycrystalline diamond are, and the fine-grained polycrystalline diamond can be obtained.
Preferably, the sintering treatment is carried out under the pressure at 1200-1600 ℃ and 5.5-8.0 GPa. Preferably, the sintering temperature is 1350-1450 ℃, the sintering pressure is 6.0-8.0 GPa, and the sintering time is 300-380 s. The sintering temperature and the sintering pressure can obtain a good sintering reaction effect, the sintering purpose cannot be realized when the temperature is too low and the pressure is too low, diamond graphitization can be caused when the temperature is too high, and damage can be caused to the diamond when the sintering pressure is too high; the sintering time also influences the performance of the finally prepared diamond compact, the sintering time is too short, the diamond and metal cobalt cannot fully react, the formed D-D bonds are insufficient, the strength of the prepared diamond compact is insufficient, the diamond can be graphitized if the sintering time is too long, the strength of the diamond compact is reduced, and meanwhile, the bonding interface between a diamond polycrystalline layer formed by diamond micropowder and a hard alloy substrate is broken due to too long sintering time, so that the product is damaged and scrapped.
Based on the method, the invention also provides a fine-grained diamond polycrystal, wherein the diamond polycrystal is prepared by the method, the distribution uniformity of metal cobalt in the diamond polycrystal is excellent, D-D bonds among diamond particles are fully and reasonably distributed, the internal stress is extremely small, the diamond polycrystal has higher bonding strength, and the strength, the impact toughness and the wear resistance of the diamond polycrystal are excellent. The mass fraction of diamond in the fine-grained diamond polycrystal is 70-90%, and the mass fraction of cobalt is 10-30%.
The present invention will be described in detail below with reference to examples.
Example 1
(1) 2.42g of cobalt chloride hexahydrate and 1.50g of polyethylene glycol 2000 were dissolved in 300ml of absolute ethanol;
(2) 30g of 0.9-1.5 mu m diamond micro powder is poured into the solution in the step (1) under the condition of ultrasonic stirring, and the ultrasonic stirring is continued for 30min, wherein the stirring speed is 200 r/min;
(3) dropwise adding 7ml of 5-5.6% ammonia water into the solution in the step (2) under the ultrasonic stirring condition, continuing ultrasonic stirring for 40min after the dropwise adding is finished, keeping the stirring speed unchanged, filtering, washing with deionized water for multiple times, and drying;
(4) calcining the dried micro powder at 700 ℃ for 1h, and then reducing the micro powder at 400 ℃ for 5h in a hydrogen atmosphere;
(5) filling the treated micro powder into an internal package, and carrying out vacuum treatment for 3h at 600 ℃; and (3) after the outer package is finished, sintering the polycrystalline diamond A at the temperature of 1450 ℃ for 5min under the pressure of 6GPa to obtain a product of polycrystalline diamond A, taking out the sintered polycrystalline diamond A, and performing electron microscope scanning, wherein the result is shown in figure 2, and the grain size of the polycrystalline diamond A is uniform and does not grow, and no crack exists.
Example 2
(1) 2.70g of cobalt acetate and 3.00g of polyethylene glycol 2000 were dissolved in 300ml of absolute ethanol;
(2) 30g of 0.5-1.0 mu m diamond micro powder is poured into the solution in the step (1) under the condition of ultrasonic stirring, and the ultrasonic stirring is continued for 30min, wherein the stirring speed is 300 r/min;
(3) 15.5ml of 1mol/L sodium hydroxide solution is dripped into the solution in the step (2) under the condition of ultrasonic stirring, ultrasonic stirring is continued for 40min after the dripping is finished, the stirring speed is unchanged, and then the solution is filtered, washed by deionized water for multiple times and dried;
(4) calcining the dried micro powder at 400 ℃ for 5h, and then treating the micro powder at 1200 ℃ for 2h under the condition of vacuumizing;
(5) filling the treated micro powder into an internal package, and carrying out vacuum treatment for 3h at 600 ℃; and (3) after the outer packaging, sintering the outer packaging at the pressure of 6GPa and the temperature of 1400 ℃ for 6min to obtain a product of the polycrystalline B, taking out the sintered polycrystalline B, and performing electron microscope scanning, wherein the result is shown in figure 3, and the grain size of the polycrystalline B is uniform and does not grow up, and no crack exists.
Example 3
(1) 2.42g of cobalt chloride hexahydrate is dissolved in 300ml of absolute ethyl alcohol;
(2) 30g of diamond micro powder with the particle size of 2-3 mu m is poured into the solution in the step (1) under the condition of ultrasonic stirring, and the ultrasonic stirring is continued for 30 min;
(3) dropwise adding 7ml of 5-5.6% ammonia water into the solution in the step (2) under the ultrasonic stirring condition, continuing ultrasonic stirring for 40min after dropwise adding is finished, filtering, washing with deionized water for multiple times, and drying;
(4) calcining the dried micro powder at 600 ℃ for 3h, and reducing carbon monoxide at 900 ℃ for 2 h;
(5) filling the treated micro powder into an internal package, and carrying out vacuum treatment for 3h at 600 ℃; and (3) after the outer packaging, sintering the outer packaging at the temperature of 1450 ℃ for 5min under the pressure of 6GPa to obtain a product of the polycrystalline C of the diamond, taking out the sintered polycrystalline C of the diamond, and scanning the sintered polycrystalline C of the diamond by an electron microscope, wherein the result is shown in figure 4, and the grains of the polycrystalline B of the diamond have uniform granularity and do not grow up and have any cracks.
In addition, the hardness and wear resistance of the polycrystalline diamond A, the polycrystalline diamond B and the polycrystalline diamond C prepared in the embodiments 1 to 3 are tested, and the results show that the polycrystalline diamond A, the polycrystalline diamond B and the polycrystalline diamond C have extremely high hardness and excellent wear resistance. The test result shows that the hardness of the three polycrystalline is 6500-8000(Hv), and the abrasion ratio of the grinding wheel is 150-300 ten thousand.
In summary, the preparation method of fine-grained diamond polycrystalline provided by the invention comprises the steps of firstly processing diamond micro powder, dispersing and doping metal cobalt in the diamond micro powder, then putting the diamond micro powder doped with the metal cobalt into a metal cup, and adding a layer of metal cobalt on the surface layer, so that when high-temperature and high-pressure sintering is carried out, the metal cobalt on the surface and the metal cobalt doped in the interior can be simultaneously utilized to catalyze the diamond particles to uniformly distribute and generate D-D bonds, the diamond polycrystalline with higher bonding strength is formed, the wear resistance of the product is improved, and the problem that the polycrystalline sintered under the condition of high temperature and high pressure in the prior art is large in stress and easy to generate cracks is solved.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of fine-grained diamond polycrystal is characterized by comprising the following steps:
dissolving cobalt salt and a dispersing agent in a solvent, adding diamond micro powder and uniformly mixing to obtain a mixed solution;
dropwise adding an alkaline solution into the mixed solution until cobalt is completely precipitated, and filtering to obtain a solid mixture;
placing the solid mixture in an oxygen-containing atmosphere for calcination treatment, then placing the calcined product in vacuum or reducing atmosphere and heating for oxidation-reduction reaction to obtain cobalt-containing diamond micro powder;
putting the diamond micro powder into a metal cup, coating a layer of metal cobalt on the surface layer of the diamond micro powder, then carrying out vacuum treatment, and then pressurizing and sintering to obtain the fine-grained diamond polycrystal with uniform D-D bonds inside.
2. The method for preparing a fine-grained diamond polycrystal according to claim 1, wherein the mass ratio of cobalt element to diamond in the mixed solution is 0.1-5: 95-99.9.
3. The method of preparing a fine grain diamond polycrystal according to claim 1, wherein the cobalt salt is one or more of cobalt chloride, a cobalt chloride hydrate compound, cobalt nitrate, a cobalt nitrate hydrate compound, cobalt sulfate, a cobalt sulfate hydrate compound, cobalt carboxylate, a cobalt carboxylate hydrate compound, cobalt oxalate and a cobalt oxalate hydrate compound.
4. The method of making fine-grained diamond polycrystallmes according to claim 1, wherein the dispersing agent is polyethylene glycol.
5. The method of preparing fine-grained diamond polycrystals according to claim 1, wherein the solvent is water, methanol, ethanol, or acetone.
6. The method for preparing fine-grained diamond polycrystal according to claim 1, wherein the alkaline solution is one or a combination solution of more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonia carbonate, ammonium bicarbonate and ammonia water.
7. The method of preparing a fine-grained diamond polycrystal according to claim 1, wherein the grain size of the diamond micropowder is 0 to 3 μm.
8. The method of making a fine-grained diamond polycrystalline according to claim 1, wherein the reducing gas is hydrogen or carbon monoxide.
9. The method for preparing fine-grained diamond polycrystal according to claim 1, wherein the calcination treatment temperature is 400-700 ℃, the heating temperature is 400-1200 ℃, and the sintering treatment under pressurization is carried out under the process conditions of 1200-1600 ℃ and 5.5-8.0 GPa.
10. A fine-grained diamond polycrystalline prepared by the method of any one of claims 1 to 9.
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