CN109706340A - A kind of fine-granularity diamond plycrystalline diamond and preparation method thereof - Google Patents
A kind of fine-granularity diamond plycrystalline diamond and preparation method thereof Download PDFInfo
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- CN109706340A CN109706340A CN201910064573.3A CN201910064573A CN109706340A CN 109706340 A CN109706340 A CN 109706340A CN 201910064573 A CN201910064573 A CN 201910064573A CN 109706340 A CN109706340 A CN 109706340A
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Abstract
The invention discloses a kind of fine-granularity diamond plycrystalline diamonds and preparation method thereof, wherein the method includes the steps: cobalt salt and dispersing agent are dissolved in solvent, diadust is added and mixes, obtains mixed liquor；It is complete to cobalt precipitating that alkaline solution is added dropwise into mixed liquor, filtering obtains solid mixture；Solid mixture is placed in oxygen-containing atmosphere and carries out calcination processing, then calcined product is placed in vacuum or reducing atmosphere to and is heated carry out redox reaction, obtain diadust containing cobalt；Diadust is fitted into metal cup and coats one layer of metallic cobalt on diadust surface layer, is then vacuum-treated, repressurization is sintered, and fine-granularity diamond plycrystalline diamond can be obtained.The present invention solves the problems, such as that the plycrystalline diamond stress being sintered out under high-temperature and high-pressure conditions in the prior art is larger and is easy to produce crackle.
Description
Technical field
The present invention relates to Diamond machining techniques field more particularly to a kind of fine-granularity diamond plycrystalline diamond and its preparation sides
Method.
Background technique
Fine-granularity diamond plycrystalline diamond is sintered under high temperature, condition of high voltage by 0-3 μm of diadust and metallic cobalt,
The sintered body that it is mainly made of diadust and cobalt has the characteristics that hardness is high, wearability is high, while due also to Buddha's warrior attendant
The small feature of sword out that stone crystal grain is small and has is the ideal material for manufacturing high quality cutting tool and wire drawing die.
It is easy to produce crackle since the plycrystalline diamond stress being sintered out under high-temperature and high-pressure conditions is larger, simultaneously because diadust
Partial size is thin and is easy to produce the phenomenon that crystal grain is grown up.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of fine-granularity diamond plycrystalline diamond and its systems
Preparation Method, it is intended to solve existing fine-granularity diamond plycrystalline diamond in the preparation since the plycrystalline diamond being sintered out under high-temperature and high-pressure conditions is answered
Power larger the problem of being easy to produce crackle.
Technical scheme is as follows:
A kind of preparation method of fine-granularity diamond plycrystalline diamond, wherein comprising steps of
Cobalt salt and dispersing agent are dissolved in solvent, diadust is added and mixed, mixed liquor is obtained；
It is complete to cobalt precipitating that alkaline solution is added dropwise into mixed liquor, filtering obtains solid mixture；
Solid mixture is placed in oxygen-containing atmosphere and carries out calcination processing, calcined product is then placed in vacuum or reproducibility gas
In atmosphere and carry out redox reaction is heated, obtains diadust containing cobalt；
Diadust is fitted into metal cup and coats one layer of metallic cobalt on diadust surface layer, is then carried out at vacuum
Reason, repressurization are sintered, and fine-granularity diamond plycrystalline diamond can be obtained.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein in the mixed liquor, the matter of cobalt element and diamond
Amount is than being 0.1 ~ 5:95 ~ 99.9.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the cobalt salt is cobalt chloride, cobalt chloride hydration chemical combination
Object, cobalt nitrate, cobalt nitrate hydrated compound, cobaltous sulfate, cobaltous sulfate hydrated compound, carboxylic acid cobalt, carboxylic acid cobalt hydrated compound, grass
One of sour cobalt and cobalt oxalate hydrated compound are a variety of.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the dispersing agent is polyethylene glycol.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the solvent is water, methanol, ethyl alcohol or acetone.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the alkaline solution is sodium hydroxide, hydroxide
One of potassium, sodium carbonate, potassium carbonate, sodium bicarbonate, saleratus, carbonic acid ammonia, ammonium hydrogencarbonate and ammonium hydroxide and a variety of combinations
Solution.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the diadust partial size is 0-3 μm.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the reducibility gas is hydrogen or carbon monoxide.
The preparation method of the fine-granularity diamond plycrystalline diamond, wherein the temperature of calcination processing is 400 ~ 700 DEG C, heating
Temperature is 400 ~ 1200 DEG C, and the process conditions being sintered of pressurizeing are 1200 ~ 1600 DEG C of temperature, 5.5 ~ 8.0GPa of pressure.
A kind of fine-granularity diamond plycrystalline diamond, wherein be prepared by method as described above.
The utility model has the advantages that the present invention by first handling diadust, disperses doping metals cobalt wherein, then will
One layer of metallic cobalt is added in being fitted into metal cup and on surface layer doped with the diadust of metallic cobalt, in this way to carry out high temperature high
When pressure sintering, can uniformly it divide using between the metallic cobalt on the surface and the metallic cobalt catalysis diamond particles of internal doping simultaneously
Cloth generates D-D key, forms the higher dimond synneusis of bond strength, improves the wear-resisting property of product, solve the prior art
The plycrystalline diamond stress larger the problem of being easy to produce crackle being sintered out under high temperature condition of high voltage.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method preferred embodiment of fine-granularity diamond plycrystalline diamond of the present invention；
The SEM figure that Fig. 2 is dimond synneusis A obtained in embodiment 1；
The SEM figure that Fig. 3 is dimond synneusis B obtained in embodiment 2；
The SEM figure that Fig. 4 is dimond synneusis C obtained in embodiment 3.
Specific embodiment
The present invention provides a kind of fine-granularity diamond plycrystalline diamond and preparation method thereof, to make the purpose of the present invention, technical solution
And effect is clearer, clear, the present invention is described in more detail below.It should be appreciated that specific implementation described herein
Example is only used to explain the present invention, is not intended to limit the present invention.
The preparation method of fine-granularity diamond plycrystalline diamond of the present invention, as shown in Figure 1, comprising steps of
S1, cobalt salt and dispersing agent are dissolved in solvent, diadust is added and mixed, obtain mixed liquor；
S2, into mixed liquor, dropwise addition alkaline solution is complete to cobalt precipitating, and filtering obtains solid mixture；
S3, it solid mixture is placed in oxygen-containing atmosphere carries out calcination processing, calcined product is then placed in vacuum or reduction
In property atmosphere and carry out redox reaction is heated, obtains diadust containing cobalt；
S4, diadust is fitted into metal cup and coats one layer of metallic cobalt on diadust surface, then carry out vacuum
Processing, repressurization are sintered, and fine-granularity diamond plycrystalline diamond can be obtained.
The present invention is existed by a certain amount of metallic cobalt of Uniform Doped between diadust in advance to improve cobalt metal
The uniformity being distributed between diadust particle can make metallic cobalt be catalyzed diamond in the processing of subsequent high temperature high-pressure sinter
It is uniformly distributed between grain and generates D-D key, while before diadust carries out high temperature and pressure sintering, the table on diadust layer
Layer one layer of cobalt metal of deposition, such diadust is when high temperature and pressure is sintered, the cobalt metal molten on surface and the gold for making surface layer
Hard rock wetting is uniform, meanwhile, the metallic cobalt on surface can also permeate downwards, and the diadust of lubrication inside and lower layer is formed more
More D-D keys, further eliminating cobalt Metal Distribution unevenness causes to fail to be formed between interior diamond particles to combine to form D-D key
And there is a possibility that internal stress, the higher dimond synneusis of bond strength is formed, the wearability of diamond compact is improved
Can, it solves the problems, such as that the plycrystalline diamond stress being sintered out under high-temperature and high-pressure conditions is larger and is easy to produce crackle.In addition, the present invention passes through
The above method can also avoid diadust from being easy to produce the phenomenon that crystal grain is grown up since partial size is thin.
Preferably, before carrying out step S1, purification process (such as soda acid purifying) first is carried out to impurity to diadust
Content is lower than 100ppm, more preferably, is purified to impurity content lower than 50ppm, impurity therein such as Fe, Ni, Mn, Cr, Al, Ca,
Mg, Si etc..The impurity of diadust surface and internal clearance is removed, to realize preferably plycrystalline diamond effect, while avoiding impurity
To the adverse effect of final product performance.
In the step S1, cobalt salt and dispersing agent are dissolved in solvent, it is using the effect of dispersing agent that cobalt salt is fully dispersed,
Then diadust is added under ultrasonic agitation effect, diadust and cobalt salt is mixed, mixed liquor is obtained.It is preferred that
Ground, the present invention in diadust, it is desirable that granularity (may be, for example, 0-0.7 μm, 0.5-1 μm, 0.9- in 0 ~ 3 micron range
1.5 μm or 2-3 μm), to guarantee that the fine granularity of product is made.In the mixed liquor, pass through control cobalt salt and diadust
Adjusting ratio, so that the mass ratio of cobalt element and diamond is 0.1 ~ 5:95 ~ 99.9, the metallic cobalt in this content range, gold
It is too low to belong to cobalt content, is unable to reach between catalysis diadust and forms the requirement of D-D bond structure, and metallic cobalt content is too high, then
Understand because of cobalt metal with diamond coefficient of thermal expansion differences abnormity into biggish thermal residual strain, makes diamond compact in the course of work
It is middle phenomena such as not wear-resisting, disintegrating tablet occur.
Wherein, the cobalt salt is cobalt chloride, cobalt chloride water and compound, cobalt nitrate, cobalt nitrate hydrated compound, sulfuric acid
One of cobalt, cobaltous sulfate hydrated compound, carboxylic acid cobalt, carboxylic acid cobalt hydrated compound, cobalt oxalate and cobalt oxalate hydrated compound
Or it is a variety of.The dispersing agent is preferably polyethylene glycol, by cobalt salt dispersion effect it is further preferred that；More preferably, the molecular weight of polyethylene glycol
For 400-6000, the ratio of the volume (mL) of the quality (g) and solvent of the polyethylene glycol of addition is 0-5:100.The solvent can
Think water, methanol, ethyl alcohol or acetone.
In the step S2, alkaline solution is added dropwise into mixed liquor under ultrasonic agitation, using alkaline solution by cobalt ions
The Precipitation in the form of cobalt hydroxide, until after being filtered, washed after continuing ultrasonic treatment stirring a period of time after cobalt precipitating is complete
And it is dry with the Temperature Vacuum no more than 60 DEG C, to remove because the other impurities that cobalt plating process is brought into, realize better plycrystalline diamond
Effect obtains the solid mixture that main ingredient is cobalt hydroxide and diadust.
In the step S3, solid mixture is placed in oxygen-containing atmosphere (such as oxygen or air) and carries out calcination processing, is made
The impurity such as the dispersing agent, the solvent that mix in solid mixture are oxidized to gas removal, meanwhile, the impurity in diadust
It can be removed under the action of calcining, and cobalt hydroxide is sintered into cobalt oxide, to obtain by pure cobalt oxide and Buddha's warrior attendant
The calcined product of stone micro mist mixing；Preferably, the temperature of the calcination processing in step S3 is 400 ~ 700 DEG C, which can
By dispersing agent, solvent it is fully calcined be gaseous state, temperature is too low to cannot achieve calcining purpose, and temperature is excessively high that it will cause diamonds
The loss of micro mist, while also resulting in unnecessary energy consumption；More preferably, the calcination processing time is 1-5h, it can by dispersing agent, molten
The abundant after-flame such as agent.
In the step S3, the calcined product mixed by pure cobalt oxide with diadust is placed in vacuum or reduction
Property gas atmosphere in, by heating so that the cobalt oxide in calcined product is reduced into metallic cobalt, obtain the pure gold containing metallic cobalt
Hard rock micro mist, in the diadust, cobalt content 0.1-5%, preferably 1.5-3%, cobalt content is too low to be filled in sintering
Sub-dip moistens diamond particles and forms D-D key, and solid content is excessively high, can be poly- because of the less diamond made of diamond content
Brilliant intensity is lower.Wherein, heating temperature, which is 400 ~ 1200 DEG C, can be reduced into zirconium oxide metallic cobalt, the too low nothing of heating temperature
Method reaches reduction temperature, and temperature is excessively high, equally will cause the loss of diadust；Preferably, heating treatment time 1-
6h, the time is too short to be sufficiently reduced to metallic cobalt for zirconium oxide.Wherein, the reducibility gas is hydrogen or carbon monoxide.
In the step S4, diadust is fitted into metal cup and coats one layer of metal on diadust surface
Then cobalt is vacuum-treated, to drain air, be then placed in high-tension apparatus pressurization and be sintered, because in high pressure height
Under warm environment, metallic cobalt is fused into liquid and is permeating between diamond particles, diamond particles then portion at high temperature under high pressure
Divide and be dissolved in the cobalt metal of fusing, when solubility of the diamond in liquid phase cobalt metal reaches saturation, will be precipitated again
Diamond crystal generates D-D key to interconnect between making diamond particles, forms dimond synneusis.Because previously
Doping has dispersed metallic cobalt and has been added to one layer of metallic cobalt on diadust surface layer in diadust, both common
Effect can to form more D-D keys more evenly inside diadust, eliminate because in caused by D-D key is unevenly distributed
Stress avoids the occurrence of crackle；And much more uniform, intensity, toughness and the wearability of dimond synneusis that D-D key is formed
Can be also better, fine-granularity diamond plycrystalline diamond can be obtained.
Preferably, the process conditions being sintered of pressurizeing are 1200 ~ 1600 DEG C of temperature, 5.5 ~ 8.0GPa of pressure.Compared with
Goodly, sintering temperature is 1350 ~ 1450 DEG C, sintering pressure is 6.0 ~ 8.0GPa, sintering time is 300 ~ 380s.Above-mentioned sintering temperature
Degree and pressure can obtain preferable sintering reaction effect, and temperature is too low, pressure is too small cannot achieve sintering purpose, and temperature
Excessive to will cause diamond graphitization, sintering pressure is excessive equally to damage diamond；Sintering time also influences finally
The performance of the diamond compact of preparation, sintering time is too short, and diamond is unable to fully react with metallic cobalt, the D-D key of formation
It is insufficient, cause the diamond compact intensity being prepared inadequate, and if sintering time is too long, it can make diamond that stone occur
Mo Hua reduces its intensity, while the too long dimond synneusis layer for also resulting in diadust formation of sintering time and hard close
The combination interface of auri body is broken, and product damage is caused to be scrapped.
Based on the above method, the present invention also provides a kind of fine-granularity diamond plycrystalline diamonds, wherein by method as described above
It being prepared, metallic cobalt distributing homogeneity is splendid in the dimond synneusis, and the distribution of D-D key is sufficiently reasonable between diamond particles,
Internal stress is minimum, has the higher dimond synneusis of bond strength, intensity, toughness and wear-resisting property are splendid.It is described
The mass fraction of diamond is 70-90% in fine-granularity diamond plycrystalline diamond, and the mass fraction of the cobalt is 10-30%.
Below by embodiment, the present invention is described in detail.
Embodiment 1
(1) 2.42g CoCL2 6H2O and 1.50g polyethylene glycol 2000 are dissolved in 300ml dehydrated alcohol；
(2) diadust of 30g 0.9-1.5 μm is poured into (1) in solution under conditions of ultrasonic agitation and continues ultrasound
Stir 30min, stirring rate 200r/min；
(3) it takes the ammonium hydroxide of 7ml 5-5.6% to be added drop-wise in the solution in (2) under conditions of ultrasonic agitation, continues after being added dropwise to complete
40min is stirred by ultrasonic, stirring rate is constant, then filters and is repeatedly washed with deionized water, dries；
(4) micro mist after drying is calcined at 700 DEG C 1h, then restores 5h at 400 DEG C in hydrogen atmosphere；
(5) micro mist handled well is packed into interior assembling kit, is vacuum-treated 3h at 600 DEG C；In pressure 6GPa, temperature after exterior
It is sintered 5min at 1450 DEG C, product dimond synneusis A can be obtained, takes out the dimond synneusis A sintered, Electronic Speculum is carried out and sweeps
It retouches, as a result as shown in Figure 2, it can be seen that dimond synneusis A crystallite size is not grown up uniformly, and any crackle is also not present.
Embodiment 2
(1) 2.70g cobalt acetate and 3.00g polyethylene glycol 2000 are dissolved in 300ml dehydrated alcohol；
(2) diadust of 30g 0.5-1.0 μm is poured into (1) in solution under conditions of ultrasonic agitation and continues ultrasound
Stir 30min, stirring rate 300r/min；
(3) it takes the sodium hydroxide solution of 15.5ml 1mol/L to be added drop-wise in the solution in (2) under conditions of ultrasonic agitation, drips
Continue that 40min is stirred by ultrasonic after adding into, stirring rate is constant, then filters and is repeatedly washed with deionized water, dries；
(4) micro mist after drying is calcined at 400 DEG C 5h, then handles 2h at 1200 DEG C under vacuum-pumping conditions；
(5) micro mist handled well is packed into interior assembling kit, is vacuum-treated 3h at 600 DEG C；In pressure 6GPa, temperature after exterior
It is sintered 6min at 1400 DEG C, product dimond synneusis B can be obtained, takes out the dimond synneusis B sintered, Electronic Speculum is carried out and sweeps
It retouches, as a result as shown in Figure 3, it can be seen that dimond synneusis B crystallite size is not grown up uniformly, and any crackle is also not present.
Embodiment 3
(1) 2.42g CoCL2 6H2O is dissolved in 300ml dehydrated alcohol；
(2) diadust of 30g 2-3 μm is poured into (1) in solution under conditions of ultrasonic agitation and continues to be stirred by ultrasonic
30min；
(3) it takes the ammonium hydroxide of 7ml 5-5.6% to be added drop-wise in the solution in (2) under conditions of ultrasonic agitation, continues after being added dropwise to complete
40min is stirred by ultrasonic, then filter and is repeatedly washed with deionized water, dries；
(4) micro mist after drying is calcined into 3h at 600 DEG C, the carbon monoxide reductase 12 h at 900 DEG C；
(5) micro mist handled well is packed into interior assembling kit, is vacuum-treated 3h at 600 DEG C；In pressure 6GPa, temperature after exterior
It is sintered 5min at 1450 DEG C, product dimond synneusis C can be obtained, takes out the dimond synneusis C sintered, and carries out Electronic Speculum and sweeps
It retouches, as a result as shown in Figure 4, it can be seen that dimond synneusis B crystallite size is not grown up uniformly, and any crackle is also not present.
In addition, the present invention is also poly- by product dimond synneusis A, dimond synneusis B obtained by embodiment 1 ~ 3 and diamond
Brilliant C carries out hardness and wear-resisting property test, the results showed that dimond synneusis A, dimond synneusis B and dimond synneusis C all have
High hardness and excellent wear-resisting property.Test result is the hardness of three kinds of plycrystalline diamonds in 6500-8000 (Hv), grinding wheel wear resistance ratio
In 150-300 ten thousand.
In conclusion the present invention provides fine-granularity diamond plycrystalline diamond preparation method, by first to diadust
Handled, wherein disperse doping metals cobalt, then by doped with the diadust of metallic cobalt in being fitted into metal cup simultaneously
One layer of metallic cobalt is added on surface layer, in this way when carrying out high temperature and pressure sintering, the metallic cobalt on the surface and interior can be utilized simultaneously
It is uniformly distributed between the metallic cobalt catalysis diamond particles of portion's doping and generates D-D key, it is poly- to form the higher diamond of bond strength
Crystalline substance improves the wear-resisting property of product, and it is larger to solve the plycrystalline diamond stress being sintered out under high-temperature and high-pressure conditions in the prior art
The problem of being easy to produce crackle.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of fine-granularity diamond plycrystalline diamond, which is characterized in that comprising steps of
Cobalt salt and dispersing agent are dissolved in solvent, diadust is added and mixed, mixed liquor is obtained；
It is complete to cobalt precipitating that alkaline solution is added dropwise into mixed liquor, filtering obtains solid mixture；
Solid mixture is placed in oxygen-containing atmosphere and carries out calcination processing, calcined product is then placed in vacuum or reproducibility gas
In atmosphere and carry out redox reaction is heated, obtains diadust containing cobalt；
Diadust is fitted into metal cup and coats one layer of metallic cobalt on diadust surface layer, is then carried out at vacuum
Reason, repressurization are sintered, and fine-granularity diamond plycrystalline diamond can be obtained.
2. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that in the mixed liquor,
The mass ratio of cobalt element and diamond is 0.1 ~ 5:95 ~ 99.9.
3. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the cobalt salt is chlorination
Cobalt, cobalt chloride hydrated compound, cobalt nitrate, cobalt nitrate hydrated compound, cobaltous sulfate, cobaltous sulfate hydrated compound, carboxylic acid cobalt, carboxylic
One of sour cobalt hydrated compound, cobalt oxalate and cobalt oxalate hydrated compound are a variety of.
4. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the dispersing agent is poly-
Ethylene glycol.
5. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the solvent be water,
Methanol, ethyl alcohol or acetone.
6. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the alkaline solution is
One in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, saleratus, carbonic acid ammonia, ammonium hydrogencarbonate and ammonium hydroxide
Kind and a variety of combination solutions.
7. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the diadust
Partial size is 0-3 μm.
8. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the reducibility gas
For hydrogen or carbon monoxide.
9. the preparation method of fine-granularity diamond plycrystalline diamond according to claim 1, which is characterized in that the temperature of calcination processing
Be 400 ~ 700 DEG C, heating temperature is 400 ~ 1200 DEG C, the process conditions that are sintered of pressurizeing be 1200 ~ 1600 DEG C of temperature,
5.5 ~ 8.0GPa of pressure.
10. a kind of fine-granularity diamond plycrystalline diamond, which is characterized in that be prepared by the method as described in claim 1 ~ 9 is any.
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| CN110560678A (en) * | 2019-07-26 | 2019-12-13 | 郑州中南杰特超硬材料有限公司 | Polycrystalline tube and preparation method thereof |
| CN111974310A (en) * | 2020-09-07 | 2020-11-24 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing polycrystalline diamond compact from cobalt catalyst-loaded diamond micro powder |
| CN114318098A (en) * | 2021-12-09 | 2022-04-12 | 深圳市海明润超硬材料股份有限公司 | Large-size fine-grained polycrystalline diamond composite material and preparation method thereof |
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| CN103072332A (en) * | 2012-12-27 | 2013-05-01 | 深圳市海明润实业有限公司 | Polycrystalline diamond compact and preparation method thereof |
| CN104114722A (en) * | 2011-12-21 | 2014-10-22 | 六号元素磨料股份有限公司 | Methods of forming a superhard structure or body comprising a body of polycrystalline diamond containing material |
| CN104350027A (en) * | 2012-03-30 | 2015-02-11 | 第六元素研磨剂股份有限公司 | Polycrystalline diamond material and method of forming |
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| CN104114722A (en) * | 2011-12-21 | 2014-10-22 | 六号元素磨料股份有限公司 | Methods of forming a superhard structure or body comprising a body of polycrystalline diamond containing material |
| CN104350027A (en) * | 2012-03-30 | 2015-02-11 | 第六元素研磨剂股份有限公司 | Polycrystalline diamond material and method of forming |
| CN103072332A (en) * | 2012-12-27 | 2013-05-01 | 深圳市海明润实业有限公司 | Polycrystalline diamond compact and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110560678A (en) * | 2019-07-26 | 2019-12-13 | 郑州中南杰特超硬材料有限公司 | Polycrystalline tube and preparation method thereof |
| CN111974310A (en) * | 2020-09-07 | 2020-11-24 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing polycrystalline diamond compact from cobalt catalyst-loaded diamond micro powder |
| CN114318098A (en) * | 2021-12-09 | 2022-04-12 | 深圳市海明润超硬材料股份有限公司 | Large-size fine-grained polycrystalline diamond composite material and preparation method thereof |
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