CN114318098A - Large-size fine-grained polycrystalline diamond composite material and preparation method thereof - Google Patents
Large-size fine-grained polycrystalline diamond composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a large-size fine-grained polycrystalline diamond composite material and a preparation method thereof, wherein the method comprises the following steps: dissolving metal salt, absolute ethyl alcohol and a dispersing agent in a solvent to obtain metal salt sol, and dispersing diamond micro powder in the metal salt sol to obtain a mixed solution; dispersing alkali liquor in the mixed solution for reaction to obtain white precipitate; heating the white precipitate in a reducing atmosphere to obtain a diamond binder mixture; dispersing an inhibitor into the diamond binder mixture, putting a tungsten carbide matrix material into the diamond binder mixture, performing vacuum heat treatment, and sintering by using high-temperature and high-pressure equipment to obtain the PCD composite material for the large-size fine-grained cutter. The method has strong practicability and good process stability. The method solves the problems that the PCD composite material for the large-size fine-grained cutter is difficult to sinter and has low synthesis yield under the existing conditions, and the PCD composite material for the large-size fine-grained cutter with low stress and high quality can be synthesized in batches by the method, and can realize higher yield.
Description
Technical Field
The invention belongs to the technical field of polycrystalline diamond, and particularly relates to a large-size fine-grained polycrystalline diamond composite material and a preparation method thereof.
Background
The polycrystalline diamond (PCD) composite material for the large-size fine-grained cutter is formed by sintering 0.05-1.5 mu m diamond micro powder, an organic metal salt treated binder and a WC/Co (tungsten carbide/cobalt) hard alloy substrate at high temperature and high pressure, is generally used in domestic high-precision machining, has the advantages of high smoothness of machined products, good machining size and the like, and has more obvious machining advantages of the PCD composite material for the fine-grained cutter along with the continuous progress of the domestic machining field and the higher and higher requirement of high-precision elements.
Due to plastic deformation and the existence of gaps under ultrahigh pressure in the preparation process, the diamond raw material is locally in a high-temperature low-pressure thermodynamically unstable state, so that the PCD composite material for the large-size fine-grained cutter has large internal stress and is easy to crack.
Therefore, the prior art is still subject to further improvement.
Disclosure of Invention
The invention aims to provide a preparation method of a polycrystalline diamond composite material, and aims to solve the problem that when the existing PCD composite material for a large-size fine-grained cutter is prepared, cracks are easily generated due to large polycrystalline stress sintered under the condition of high temperature and high pressure.
The invention adopts the technical scheme that the preparation method of the polycrystalline diamond composite material comprises the following operation steps:
dissolving metal salt, absolute ethyl alcohol and a dispersing agent in a solvent to obtain metal salt sol;
dispersing the diamond micro powder in the metal salt sol to obtain a mixed solution;
dispersing alkali liquor in the mixed solution for reaction to obtain white precipitate;
heating the white precipitate in a reducing atmosphere to obtain a diamond binder mixture;
dispersing an inhibitor in the diamond binder mixture, putting a tungsten carbide matrix material into the diamond binder mixture, carrying out vacuum heat treatment, and sintering by using high-temperature and high-pressure equipment to obtain the polycrystalline diamond composite material.
Optionally, the method for preparing the large-size fine-grained polycrystalline diamond composite material comprises a step of preparing an organic metal salt, wherein the organic metal salt is selected from one or more of butyl titanate, ferric citrate, nickel acetate, chromium acetate, cobalt isooctanoate, cobalt oxalate and nickel isooctanoate.
Optionally, in the preparation method of the large-size fine-grained polycrystalline diamond composite material, the mass ratio of the metal elements in the organic metal salt to the diamond micropowder is 0.05-20: 75-98.5.
Optionally, in the preparation method of the large-size fine-grained polycrystalline diamond composite material, the dispersant is polyethylene glycol or sodium metaphosphate; the solvent is methanol, ethanol, acetone or water.
Optionally, the preparation method of the large-size fine-grained polycrystalline diamond composite material comprises the step of preparing an alkali solution, wherein the alkali solution is one or more selected from the group consisting of an ammonia carbonate solution, an ammonia bicarbonate solution, a sodium hydroxide solution, a potassium hydroxide solution, a sodium carbonate solution, a potassium carbonate solution, a sodium bicarbonate solution, a potassium bicarbonate solution and ammonia water.
Optionally, the preparation method of the large-size fine-grained polycrystalline diamond composite material, wherein the step of heating the white precipitate in a reducing atmosphere to obtain a diamond binder mixture specifically includes:
drying the white precipitate at 50-100 ℃, and heating in a reducing atmosphere to obtain a diamond binder mixture;
the reducing gas in the reducing atmosphere is methane, ethane, hydrogen or carbon monoxide.
Optionally, the preparation method of the large-size fine-grained polycrystalline diamond composite material, wherein the step of mixing and adding the inhibitor into the diamond binder mixture, adding the tungsten carbide base material into the diamond binder mixture, and sintering the mixture to obtain the polycrystalline diamond composite material, specifically includes:
dispersing an inhibitor in the diamond binder mixture to obtain a precursor;
and putting the precursor into a metal cup, putting a tungsten carbide substrate material into the metal cup, and carrying out vacuum heat treatment and sintering treatment to obtain the polycrystalline diamond composite material.
Optionally, the method for preparing the large-size fine-grained polycrystalline diamond composite material comprises the following steps of selecting one or more of cubic boron nitride, boron carbide, tungsten carbide and titanium carbide; the mass ratio of the inhibitor to the metal elements in the organic metal salt to the diamond micro powder is 1-5: 0.05-20:75-98.5.
Optionally, the preparation method of the large-size fine-grained polycrystalline diamond composite material comprises the following steps: one or more methods of ball milling and mixing, mixer mixing, ultrasonic mixing and manual grinding and mixing are overlapped.
Optionally, the preparation method of the large-size fine-grained polycrystalline diamond composite material comprises the step of carrying out vacuum heat treatment, wherein the vacuum degree is 10-5the temperature of the torr is 300-750 ℃; the sintering temperature of the sintering treatment is 1200-1600 ℃ and the pressure is 6.0-8.0 GPa.
A polycrystalline diamond composite material is prepared by the preparation method of the polycrystalline diamond composite material; the finished product size of the large-size fine-grained polycrystalline diamond composite material is 40-75 mm.
Has the advantages that: the invention provides a preparation method of a polycrystalline diamond composite material, which has strong practicability and good process stability. . The method solves the problems that the PCD composite material for the large-size fine-grained cutter is difficult to sinter and has low synthesis yield under the existing conditions, and the PCD composite material for the large-size fine-grained cutter with low stress and high quality can be synthesized in batches by the method, and can realize higher yield.
Drawings
Fig. 1 is a flow diagram of a preferred embodiment of a method of making a polycrystalline diamond composite material according to the present invention;
FIG. 2 is a microstructure view of a large size fine particle size PCD composite produced in example 1;
FIG. 3 is a microstructure view of a large size fine particle size PCD composite produced in example 2;
fig. 4 is a microstructure view of a large-sized fine-grained PCD composite manufactured in example 3.
Detailed Description
The invention provides a large-size fine-grained polycrystalline diamond composite material 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. The specific embodiments described herein are merely illustrative and are not intended to be limiting.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the units indicating the content of the raw materials are all in parts by mass. Other raw materials and reagents not specifically mentioned in the present invention are those generally used in the art.
Specifically, as shown in fig. 1, the preparation method of the polycrystalline diamond composite material includes the following steps:
and S10, dissolving the metal salt, the absolute ethyl alcohol and the dispersing agent in the solvent to obtain the metal salt sol.
Specifically, a metal salt sol is prepared, and an organic metal salt, absolute ethyl alcohol and a dispersant are added into a solvent to obtain the metal salt sol. Wherein the organic metal salt may be any one or more of butyl titanate, ferric citrate, nickel acetate, chromium acetate, cobalt isooctanoate, cobalt oxalate and nickel isooctanoate. That is, the organic metal salt may be one or a mixture of several kinds, and when the organic metal salt is a mixture of several kinds, the kind and the ratio of the mixture are not limited herein, and may be adjusted according to the actual use situation. The dispersant can be polyethylene glycol or sodium metaphosphate, the solvent is methanol, ethanol, acetone or water, the organic metal salt and absolute ethanol can be mixed firstly, and then the mixture is added into the solvent containing the dispersant, so that the organic metal salt can be uniformly dispersed into the solvent to form metal salt sol.
The step S20, which is included after the step S10, is to disperse the diamond fine powder in the metal salt sol to obtain a mixed solution.
The diamond fine powder may have a particle size of 0.05 to 0.1 μm, 0.1 to 0.15 μm, 0.15 to 0.2 μm, 0.2 to 0.3 μm, 0.3 to 0.4 μm, 0.4 to 0.5 μm, 0.5 to 0.6 μm, 0.6 to 0.8 μm, 0.8 to 1.0 μm, 1.0 to 1.2 μm, 1.2 to 1.5 μm.
In this embodiment, the mass ratio of the metal element in the organic metal salt to the diamond fine powder may be 0.01 to 4:15, 0.01 to 4:19.9,0.01:15 to 19.9,4:15 to 19.9, or the like. By reasonably adjusting the adding proportion of the organic metal salt and the diamond micro powder, the obtained final product has stronger hardness and is not easy to crack during sintering.
The step S30, which is included after the step S20, is to disperse the diamond fine powder in the metal salt sol to obtain a mixed solution.
Specifically, a certain amount of alkali liquor can be added into the mixed liquor containing the diamond micropowder under the conditions of ultrasonic oscillation and stirring, white flocculent precipitate can be generated through reaction after the alkali liquor is added, and then solid-liquid separation is carried out, so that the white precipitate can be obtained. Wherein the alkali liquor is strong alkali solution, and can be one or more of ammonia carbonate solution, ammonium bicarbonate solution, sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, potassium carbonate solution, sodium bicarbonate solution, potassium bicarbonate solution and ammonia water. The ratio of the alkali liquor to the mixed liquor is 1:1, 2: 3 and 1: 4, and the ratio is based on that the white precipitate is not generated in the mixed liquor.
The step S40 of heating the white precipitate in a reducing atmosphere is included after the step S30, resulting in a diamond binder mixture.
Specifically, the white precipitate obtained in step S30 is dried at a temperature of 50 to 70 ℃, 70 to 80 ℃, or 80 to 100 ℃. The dried white precipitate (oxide or hydroxide of diamond and metal binder) is treated in a reducing atmosphere at the temperature of 900-1200 ℃ to obtain a mixture of diamond and metal binder (Ni, Co, Fe, Cr, Ti), because the metal binder 1 coated on the diamond exists in a liquid phase mode under the conditions of high temperature and high pressure, the metal binder 2 in the matrix material generates infiltration effect among diamond particles, and when the solubility of the diamond and the metal binder 1 and the metal binder 2 in the liquid phase reaches saturation, new diamond crystals are generated and original diamond particles are connected together to generate D-D bonds. In the sintering process, because the micro powder is fine, pores in the diamond are not uniform in the compaction density generated in a high-temperature and high-pressure environment, and the pores also exist in a non-directional manner, so that the metal bond 2 is not uniformly distributed when penetrating into the diamond in the synthesis process, the D-D bond is also not uniformly distributed, meanwhile, the metal bond 2 is not uniformly distributed, the difference of the thermal expansion coefficients of the metal bond 2 and the diamond indirectly generates stress difference, and the larger stress can cause cracks to be generated in the polycrystalline diamond. The method for adding the metal binder 1 on the diamond mainly comprises the steps that a layer of metal binder 1 is wrapped around the diamond in advance, a liquid-phase capillary passage can be formed in powder under the condition of high temperature and high pressure, the metal binder 2 in the matrix material can be infiltrated through the uniformly-distributed capillary holes to be uniformly distributed around the diamond, and therefore D-D bonds generated in a polycrystalline layer are uniformly distributed, meanwhile, the metal binder 2 can be prevented from being non-uniformly distributed, and the polycrystalline diamond (PCD) composite material for the large-size fine-grained cutter with excellent performance is obtained. Wherein the reducing gas may be methane, ethane, hydrogen or carbon monoxide.
And step S50 of dispersing an inhibitor in the diamond binder mixture, putting a tungsten carbide base material into the diamond binder mixture, and sintering the tungsten carbide base material to obtain the polycrystalline diamond composite material after the step S40.
Specifically, the inhibitor and the product obtained in the step S30 are mixed, the mixture is placed into a metal cup, a tungsten carbide base material is placed into the metal cup, the kit is assembled, vacuum treatment is performed, sintering treatment is performed by using high-temperature high-pressure equipment after vacuum treatment, and the polycrystalline diamond composite material is obtained after high-temperature high-pressure sintering. Wherein the vacuum degree during vacuum treatment may be 10-5torr, temperature 300 ℃ to 500 ℃, 500 ℃ to 600 ℃, 600 ℃ to 750 ℃; the sintering temperature of the sintering treatment is 1200-1600 ℃, and the pressure is 6-7 GPa, 7-8.0 GPa. The matching degree of the temperature and the pressure in the sintering process plays an important role in the performance of the polycrystalline diamond (PCD) composite material for the large-size fine-grained cutter, and if the synthesis pressure is low, the product is easy to be graphitized, and the wear resistance is poor. The sintering temperature is lower or the sintering time is shorter, the generated D-D is less or weaker, and the strength and the wear resistance of the product are poorer, so that the product fails.
In this embodiment, the inhibitor refers to an agent for inhibiting crystal growth, and the inhibitor is added to prevent abnormal growth of diamond in the synthesis process of diamond micropowder, wherein the main reason is that the larger the product size is, the larger the temperature gradient existing inside the cavity is, and in the synthesis of polycrystalline diamond, the surface energy can be reduced due to the growth of crystal grains, so that the diamond is in a more stable state with lower free energy, and the growth of part of diamond with high free energy is promoted by the temperature difference, so that the growth of crystal grains is a spontaneous change trend. To prevent this change tendency, it is necessary to reduce the surface free energy of diamond by adding a grain growth inhibitor, thereby reducing abnormal growth of diamond particles due to a difference in temperature gradient. The problem of unstable product quality caused by abnormal growth is avoided. Wherein the inhibitor may be one or more of cubic boron nitride, boron carbide, tungsten carbide and titanium carbide. The mass ratio of the inhibitor to the metal elements in the organic metal salt to the diamond micro powder is 1-5: 0.05-20:75-98.5. By controlling the addition proportion of the raw materials, the prepared polycrystalline diamond composite material has high hardness and does not crack.
Based on the same inventive concept, the invention also provides a polycrystalline diamond composite material, which is prepared by adopting the preparation method of the polycrystalline diamond composite material.
The present invention is further illustrated by the following specific examples.
Example 1
Dissolving 3.0g of organic metal salt ferric citrate in 50ml of absolute ethyl alcohol, then adding into 250ml of purified water, adding 2g of sodium metaphosphate into the purified water, stirring to prepare ferric citrate sol, adding 30g of 0.5 micron diamond micro powder after the sol is fully mixed, and uniformly mixing to obtain mixed solution;
adding 20ml of NaOH solution into the sol by adopting an ultrasonic oscillation and stirring mode to form white flocculent precipitates, then carrying out solid-liquid separation to obtain precipitates, drying the precipitates in an environment at 100 ℃, taking out the dried precipitates, and carrying out high-temperature carbon monoxide atmosphere treatment to obtain a required diamond binder mixture; then the mixture is mixed with a grain growth inhibitor WC and the like according to the weight ratio of 95: 5, mixing.
Putting the mixed micro powder into a metal cup, putting a tungsten carbide substrate material into the metal cup, assembling a kit, and performing vacuum treatment (the vacuum degree is 10)-5torr) and sintering by using high-temperature and high-pressure equipment, wherein the pressure is 6GPa, the temperature is 1500 ℃, and then the needed PCD composite material for the large-size fine-grained cutter is obtained. The microstructure is shown in FIG. 2.
Example 2
Dissolving 2.5g of organic metal salt nickel acetate in 40ml of absolute ethyl alcohol, then adding into 260ml of purified water, adding 1g of sodium metaphosphate into the purified water, stirring to prepare nickel acetate sol, adding 35g of 0.7 micron diamond micro powder after the sol is fully mixed, and uniformly mixing to obtain mixed solution;
adding 30ml of KOH solution into the sol by adopting an ultrasonic oscillation and stirring mode to form white flocculent precipitates, then carrying out solid-liquid separation to obtain precipitates, drying the precipitates in an environment at 80 ℃, taking out the dried precipitates, and carrying out high-temperature ethane atmosphere treatment to obtain a required diamond binder mixture; then the mixture is mixed with a grain growth inhibitor WC and the like according to the proportion of 99: 1, and mixing.
Putting the mixed micro powder into a metal cup, putting a tungsten carbide substrate material into the metal cup, assembling a kit, and performing vacuum treatment (the vacuum degree is 10)-5torr) and sintering by using high-temperature and high-pressure equipment, wherein the pressure is 6GPa, and the temperature is 1550 ℃, and then the needed PCD composite material for the large-size fine-grained cutter is obtained. The microstructure is shown in FIG. 3.
Example 3
Dissolving 3.5g of organic metal salt cobalt oxalate in 100ml of absolute ethyl alcohol, then adding into 200ml of methanol, adding 2g of sodium metaphosphate into the methanol, stirring to prepare cobalt oxalate sol, adding 40 parts of 0.8 micron diamond micro powder after the sol is fully mixed, and uniformly mixing to obtain a mixed solution;
adding 30ml of KOH solution into the sol by adopting an ultrasonic oscillation and stirring mode to form white flocculent precipitates, then carrying out solid-liquid separation to obtain precipitates, drying the precipitates at 90 ℃, taking out the dried precipitates, and carrying out high-temperature ethane treatment to obtain a required diamond binder mixture; then the mixture and a grain growth inhibitor WC and the like are mixed according to the weight ratio of 98: 2, and mixing.
Putting the mixed micro powder into a metal cup, putting a tungsten carbide substrate material into the metal cup, assembling a kit, and performing vacuum treatment (the vacuum degree is 10)-5torr) and sintering by using high-temperature and high-pressure equipment, wherein the pressure is 6GPa, the temperature is 1530 ℃, and then the needed PCD composite material for the large-size fine-grained cutter is obtained. The microstructure is shown in FIG. 4.
Example 4
Dissolving 3.6g of organic metal salt nickel acetate in 80ml of absolute ethyl alcohol, then adding 220ml of the organic metal salt nickel acetate into acetone, adding 2g of sodium metaphosphate into the acetone, stirring to prepare nickel acetate sol, adding 30g of 1.0 micron diamond micro powder after the sol is fully mixed, and uniformly mixing to obtain mixed solution;
adding 30ml of ammonium bicarbonate solution into the sol by adopting an ultrasonic oscillation and stirring mode to form white flocculent precipitate, separating solid from liquid to obtain precipitate, drying the precipitate in an environment at 100 ℃, taking out the dried precipitate, and treating the dried precipitate in a high-temperature ethane atmosphere to obtain a required diamond binder mixture; then the mixture and a grain growth inhibitor WC and the like are mixed according to the weight ratio of 98: 2, and mixing.
Putting the mixed micro powder into a metal cup, putting a tungsten carbide substrate material into the metal cup, assembling a kit, and performing vacuum treatment (the vacuum degree is 10)-5torr) and sintering by using high-temperature and high-pressure equipment, wherein the pressure is 7GPa, the temperature is 1600 ℃, and then the needed PCD composite material for the large-size fine-grained cutter is obtained.
Example 5
Dissolving 3g of organic metal salt nickel acetate and 2g of nickel isooctanoate in 100ml of absolute ethyl alcohol, then adding the mixture into acetone by 200ml, adding 2g of sodium metaphosphate into the acetone, stirring to prepare nickel acetate sol, adding 35g of 1.0 micron diamond micropowder after the sol is fully mixed, and uniformly mixing to obtain mixed solution;
adding 15ml of ammonium bicarbonate solution into the sol by adopting an ultrasonic oscillation and stirring mode to form white flocculent precipitate, performing solid-liquid separation to obtain precipitate, drying the precipitate at the temperature of 100 ℃, taking out the dried precipitate, and performing high-temperature ethane treatment to obtain a required diamond binder mixture; then the mixture and a grain growth inhibitor WC and the like are mixed according to the weight ratio of 98: 2, and mixing.
Putting the mixed micro powder into a metal cup, putting a tungsten carbide substrate material into the metal cup, assembling a kit, and performing vacuum treatment (the vacuum degree is 10)-5torr) and sintering by using high-temperature and high-pressure equipment, wherein the pressure is 8GPa, the temperature is 1600 ℃, and then the needed PCD composite material for the large-size fine-grained cutter is obtained.
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 method for preparing a large-size fine-grained polycrystalline diamond composite material, the method comprising:
dissolving metal salt, absolute ethyl alcohol and a dispersing agent in a solvent to obtain metal salt sol;
dispersing the diamond micro powder in the metal salt sol to obtain a mixed solution;
dispersing alkali liquor in the mixed solution for reaction to obtain white precipitate;
heating the white precipitate in a reducing atmosphere to obtain a diamond binder mixture;
and dispersing an inhibitor in the diamond binder mixture, adding a tungsten carbide matrix material, and sintering to obtain the polycrystalline diamond composite material.
2. The method of preparing a large size fine grain polycrystalline diamond composite according to claim 1, wherein the organic metal salt is selected from one or more of butyl titanate, ferric citrate, nickel acetate, chromium acetate, cobalt isooctanoate, cobalt oxalate and nickel isooctanoate.
3. The method of preparing a large-sized fine-grained polycrystalline diamond composite according to claim 1, wherein the mass ratio of the metal elements in the organic metal salt to the diamond micro powder is (0.01-4): 15-19.9.
4. The method of preparing a large-sized fine-grained polycrystalline diamond composite according to claim 1, wherein the dispersant is polyethylene glycol or sodium metaphosphate; the solvent is methanol, ethanol, acetone or water.
5. The method of preparing a large-sized fine-grained polycrystalline diamond composite according to claim 1, wherein the alkali solution is selected from one or more of an ammonia carbonate solution, an ammonia bicarbonate solution, a sodium hydroxide solution, a potassium hydroxide solution, a sodium carbonate solution, a potassium carbonate solution, a sodium bicarbonate solution, a potassium bicarbonate solution, and ammonia water.
6. The method for preparing a large-size fine-grained polycrystalline diamond composite material according to claim 1, wherein the step of heating the white precipitate in a reducing atmosphere to obtain a diamond binder mixture comprises:
drying the white precipitate at 50-100 ℃, and heating in a reducing atmosphere to obtain a diamond binder mixture;
the reducing gas in the reducing atmosphere is methane, ethane, hydrogen or carbon monoxide.
7. The method for preparing a large-size fine-grained polycrystalline diamond composite material according to claim 1, wherein the step of dispersing an inhibitor in the diamond binder mixture, placing a tungsten carbide matrix material in the diamond binder mixture, and sintering the tungsten carbide matrix material to obtain the polycrystalline diamond composite material specifically comprises the following steps:
mixing and adding an inhibitor into the diamond binder mixture to obtain a precursor;
and putting the precursor into a metal cup, putting a tungsten carbide substrate material into the metal cup, and carrying out vacuum heat treatment and sintering treatment to obtain the polycrystalline diamond composite material.
8. The method of preparing a large size fine grain polycrystalline diamond composite according to claim 1, wherein the inhibitor is selected from one or more of cubic boron nitride, boron carbide, tungsten carbide, and titanium carbide; the mass ratio of the metal elements in the inhibitor and the organic metal salt to the diamond micro powder is (1-5): (0.05-20):(75-98.5).
9. The method of preparing a large size fine grain polycrystalline diamond composite according to claim 7, wherein the vacuum heat treatment is performed in a degree of vacuum of 10-5the temperature of the torr is 300-750 ℃; the sintering temperature of the sintering treatment is 1200-1600 ℃, and the pressure is6.0-8.0GPa。
10. A large-size fine-grained polycrystalline diamond composite material, which is prepared by the preparation method of the polycrystalline diamond composite material according to any one of claims 1 to 9;
the finished product size of the large-size fine-grained polycrystalline diamond composite material is 40-75 mm.
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| CN108115142A (en) * | 2017-12-25 | 2018-06-05 | 富耐克超硬材料股份有限公司 | Diamond compact and preparation method thereof |
| CN109706340A (en) * | 2019-01-23 | 2019-05-03 | 深圳市海明润超硬材料股份有限公司 | A kind of fine-granularity diamond plycrystalline diamond and preparation method thereof |
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| CN108115142A (en) * | 2017-12-25 | 2018-06-05 | 富耐克超硬材料股份有限公司 | Diamond compact and preparation method thereof |
| CN109706340A (en) * | 2019-01-23 | 2019-05-03 | 深圳市海明润超硬材料股份有限公司 | A kind of fine-granularity diamond plycrystalline diamond and preparation method thereof |
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