CN115125537B - Method for removing cobalt in polycrystalline diamond compact - Google Patents
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- CN115125537B CN115125537B CN202210780771.1A CN202210780771A CN115125537B CN 115125537 B CN115125537 B CN 115125537B CN 202210780771 A CN202210780771 A CN 202210780771A CN 115125537 B CN115125537 B CN 115125537B
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 77
- 239000010941 cobalt Substances 0.000 title claims abstract description 77
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 65
- 239000010432 diamond Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000002841 Lewis acid Substances 0.000 claims abstract description 7
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 7
- 150000007517 lewis acids Chemical class 0.000 claims abstract description 7
- 239000010452 phosphate Substances 0.000 claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims description 19
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 5
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 5
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 5
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical group [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 238000004846 x-ray emission Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a method for removing cobalt in a polycrystalline diamond compact, which comprises the following steps: after an alloy substrate of the polycrystalline diamond compact is additionally provided with a protection tool, the alloy substrate is immersed in a cobalt-removing solution for soaking, and then is washed and dried to complete removal of cobalt in the polycrystalline diamond compact; wherein the cobalt-removing solution is prepared by the following method: adding Lewis acid and phosphate into sulfuric acid solution to prepare the cobalt-removing solvent. Compared with the prior art, the method for removing cobalt in the polycrystalline diamond compact shortens the cobalt removing period by half under the condition of reaching the same cobalt removing depth and cobalt removing content, greatly improves the cobalt removing efficiency, reduces the production cost, improves the processing capacity, improves the field working environment, reduces the safety risk of field workers, and has less environmental pollution.
Description
Technical Field
The invention relates to the technical field of nano composite material preparation, in particular to a method for removing cobalt in a polycrystalline diamond compact.
Background
Polycrystalline Diamond Compact (PDC) is a superhard composite material formed by mixing diamond micro powder and a small amount of binder cobalt powder and then sintering the mixture with a hard alloy substrate at high temperature and ultrahigh pressure, has the ultrahigh hardness and wear resistance of polycrystalline diamond and the weldability and toughness of hard alloy, and is widely applied to the fields of oil and gas drilling, geological exploration, mineral exploitation, hard material processing, metal material processing and the like.
The binder cobalt plays an important role in the synthesis, processing and use processes of the PDC, and the cobalt promotes the formation of D-D bonds among diamond grains through the dissolution-recrystallization process in the PDC synthesis process, but can also cause the failure of the PDC in the grinding process, wherein the failure is caused by the fact that the cobalt has strong affinity with carbon at high temperature and low pressure, and can convert diamond into graphite, so that the wear resistance of a PDC sample is correspondingly reduced; meanwhile, the difference between the thermal expansion coefficients of cobalt and diamond is large, so that stress is easily increased in the high-temperature processes of grinding, welding and drilling, cracks appear in the PDC, and failure modes such as abrasion, chipping and tooth breaking are caused. Therefore, after the PDC is synthesized, the cobalt in the diamond layer is removed, and the service performance of the PDC can be greatly improved. The PDC cobalt removal technology generally adopts corrosive strong acid or a mixed solution of a plurality of strong acids as a cobalt removal reagent, and achieves the cobalt removal effect by utilizing the strong corrosivity of the strong acid reagent, but the cobalt removal efficiency is low, the cobalt removal period is long, and meanwhile, the use of part of the strong acid reagents, namely nitric acid, hydrofluoric acid and hydrochloric acid, has high danger and causes pollution to the environment.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for removing cobalt in a polycrystalline diamond compact, so as to solve the problems that the cobalt removal efficiency of the polycrystalline diamond compact is low, the period is long and the used strong acid is dangerous in the prior art.
The technical scheme for solving the technical problems is as follows: a method of removing cobalt from a polycrystalline diamond compact is provided, comprising:
after an alloy substrate of the polycrystalline diamond compact is additionally provided with a protection tool, the alloy substrate is immersed in a cobalt-removing solution for soaking, and then is washed and dried to complete removal of cobalt in the polycrystalline diamond compact;
wherein the cobalt removal solution is prepared by the following method: adding Lewis acid and phosphate into sulfuric acid solution to prepare the cobalt-removed solution.
The beneficial effects of the invention are as follows: compared with the prior art, the method for removing cobalt in the polycrystalline diamond compact has the advantages that the cobalt in the polycrystalline diamond compact is removed, the cobalt removal period is shortened by half under the condition that the same cobalt removal depth and cobalt removal content requirements are met, the cobalt removal efficiency is greatly improved, the production cost is reduced, the treatment capacity is improved, the field working environment is improved, the safety risk of field workers is reduced, and the environmental pollution is less.
On the basis of the technical scheme, the invention can be further improved as follows:
further, the concentration of the sulfuric acid solution is 6-9mol/L, the concentration of Lewis acid in the sulfuric acid solution is 150-180g/L, and the concentration of phosphate is 5-15g/L.
Further, the Lewis acid is aluminum trichloride or ferric trichloride.
Further, the phosphate is sodium dihydrogen phosphate or potassium dihydrogen phosphate.
Further, the soaking temperature is 120-160 ℃.
Further, the soaking pressure is 0.8-1MPa.
Further, the soaking time is 5-15 days.
Furthermore, the thickness of the composite layer of the polycrystalline diamond compact is 1.2-3mm.
The invention has the following beneficial effects:
1. the method is adopted to remove cobalt in the polycrystalline diamond compact, when the thickness of the composite layer is 1.2mm, the cobalt removal period reaching the standard cobalt removal depth of 0.6mm is 5-7d; when the thickness of the composite layer is 3mm, the cobalt removal period reaching the standard cobalt removal depth of 1.2mm is 12-15d, and compared with the prior art, the cobalt removal period is shortened by half.
2. By adopting the method to remove the cobalt in the polycrystalline diamond compact, the cobalt content in the composite layer can be reduced from 4-7wt% to below 0.5 wt%.
3. The cobalt removing solution does not contain strong acid with high volatility and corrosivity such as nitric acid, hydrofluoric acid and the like, can improve the field working environment, reduces the safety risk of field workers, and has less environmental pollution.
Drawings
Fig. 1 is an XRF pattern of a polycrystalline diamond compact of example 1 after cobalt removal;
fig. 2 is an XRF pattern of the polycrystalline diamond compact of example 2 after cobalt removal;
fig. 3 is an XRF pattern of the polycrystalline diamond compact of example 3 after cobalt removal;
fig. 4 is an XRF pattern of the polycrystalline diamond compact of comparative example 1 after cobalt 15d removal;
fig. 5 is an XRF pattern of a polycrystalline diamond compact of comparative example 1 after cobalt 40d removal.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth to illustrate, but are not to be construed to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1:
a method for removing cobalt from a polycrystalline diamond compact comprises the following steps:
(1) Preparing 9mol/L sulfuric acid solution, and then adding 180g of aluminum trichloride and 15g of sodium dihydrogen phosphate into every 1L of sulfuric acid solution to prepare decobalt solution;
(2) Adding an anti-corrosion protection tool to an alloy substrate of a polycrystalline diamond composite sheet (the cobalt content is 4.8 wt%) with the composite layer thickness of 1.2mm, placing the alloy substrate into a pressure reaction kettle, adding the cobalt-removing solution prepared in the step (1), ensuring that the liquid level of the cobalt-removing solution soaks the polycrystalline diamond composite sheet, sealing the reaction kettle, quickly heating to 120 ℃, keeping the temperature constant, then automatically boosting to 0.8Mpa constant pressure, and soaking for 5d;
(3) And (3) decompressing the reaction kettle soaked in the step (2), reducing the temperature to room temperature, taking out the polycrystalline diamond compact, washing and drying to complete the removal of cobalt in the polycrystalline diamond compact.
Example 2:
a method for removing cobalt from a polycrystalline diamond compact comprises the following steps:
(1) Preparing 6mol/L sulfuric acid solution, and then adding 150g of aluminum trichloride and 5g of sodium dihydrogen phosphate into every 1L of sulfuric acid solution to prepare decobalt solution;
(2) Adding an anti-corrosion protection tool to an alloy substrate of a polycrystalline diamond composite sheet (with the cobalt content being 6 wt%) with the composite layer thickness being 3mm, placing the alloy substrate in a pressure reaction kettle, adding the cobalt-removing solution prepared in the step (1), ensuring that the liquid level of the cobalt-removing solution soaks the polycrystalline diamond composite sheet, sealing the reaction kettle, rapidly heating to 160 ℃, keeping the temperature constant, then automatically boosting to 1Mpa and keeping the pressure constant, and soaking for 15d;
(3) And (3) decompressing the reaction kettle soaked in the step (2), reducing the temperature to room temperature, taking out the polycrystalline diamond compact, washing and drying to complete the removal of cobalt in the polycrystalline diamond compact.
Example 3:
a method of removing cobalt from a polycrystalline diamond compact, comprising the steps of:
(1) Preparing 8mol/L sulfuric acid solution, and then adding 165g of aluminum trichloride and 10g of sodium dihydrogen phosphate into every 1L of sulfuric acid solution to prepare decobalt solution;
(2) Adding an anti-corrosion protection tool to an alloy substrate of a polycrystalline diamond composite sheet (with the cobalt content being 6 wt%) with the composite layer thickness being 3mm, placing the alloy substrate in a pressure reaction kettle, adding the cobalt-removing solution prepared in the step (1), ensuring that the liquid level of the cobalt-removing solution soaks the polycrystalline diamond composite sheet, sealing the reaction kettle, quickly heating to 150 ℃, keeping the temperature constant, then automatically boosting to 0.9Mpa constant pressure, and soaking for 12d;
(3) And (3) decompressing the reaction kettle soaked in the step (2), reducing the temperature to room temperature, taking out the polycrystalline diamond compact, washing and drying to complete the removal of cobalt in the polycrystalline diamond compact.
Comparative example 1:
a method for removing cobalt from a polycrystalline diamond compact comprises the following steps:
(1) Adding a nitric acid solution with the concentration of 4mol/L into pure hydrofluoric acid to prepare a cobalt-removed solution; wherein the volume ratio of the pure hydrofluoric acid to the nitric acid solution is 4:6;
(2) Adding an anti-corrosion protection tool to an alloy substrate of a polycrystalline diamond compact (cobalt content is 6 wt%) with the thickness of a composite layer being 3mm, placing the alloy substrate in a pressure reaction kettle, adding the cobalt-removing solution prepared in the step (1), ensuring that the liquid level of the cobalt-removing solution is soaked in the polycrystalline diamond compact, sealing the reaction kettle, and soaking for 15 days at 50 ℃;
(3) After the soaking in the step (2) is finished, taking out the polycrystalline diamond compact, washing and drying to complete the removal of cobalt in the polycrystalline diamond compact;
(4) And (3) repeating the step (2) on the polycrystalline diamond compact obtained in the step (3), continuously soaking for 25d at 50 ℃, taking out the polycrystalline diamond compact after soaking is finished, washing and drying to finish the removal of cobalt in the final polycrystalline diamond compact.
Test examples
The polycrystalline diamond compacts obtained in examples 1 to 3 and comparative example 1 after cobalt removal were analyzed for cobalt removal depth by X-ray fluorescence spectroscopy, the test voltage was 40V, the results are shown in fig. 1 to 5, and the metal cobalt content in the compacts after cobalt removal was determined by energy spectroscopy, and the results are shown in table 1.
As can be seen from fig. 1 to 5, the light color region is a cobalt-removed region, the black color region is a region without cobalt removal because of the presence of metallic cobalt, the X-ray cannot completely penetrate the sample, and the cobalt-removed region has a cobalt-removed depth shown in table 1, so that by using the method of the present invention, only 7 days are required for achieving the standard cobalt-removed depth of 0.6mm for a polycrystalline diamond compact with a composite layer thickness of 1.2mm, and only 12-15 days are required for achieving the standard cobalt-removed depth of 1.2mm for a polycrystalline diamond compact with a composite layer thickness of 3 mm; and by adopting the method of the comparative example 1, for the polycrystalline diamond compact with the composite layer thickness of 3mm, the cobalt removal depth can only reach the unqualified cobalt removal depth of 0.886mm after 15d, and finally can only reach the cobalt removal depth of 1.16mm even if the cobalt removal depth is continued for 25d, and the standard cobalt removal depth can not reach 1.2 mm.
TABLE 1 depth of cobalt removal and cobalt content of the cobalt-removed polycrystalline diamond compact
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for removing cobalt from a polycrystalline diamond compact is characterized by comprising the following steps: after an alloy substrate of the polycrystalline diamond compact is additionally provided with a protection tool, the alloy substrate is immersed in a cobalt-removing solution for soaking, and then is washed and dried to complete removal of cobalt in the polycrystalline diamond compact;
wherein the cobalt-removing solution is prepared by the following method: adding Lewis acid and phosphate into a sulfuric acid solution to prepare a cobalt-removed solution;
the concentration of the sulfuric acid solution is 6-9mol/L, the concentration of Lewis acid in the sulfuric acid solution is 150-180g/L, and the concentration of phosphate is 5-15g/L;
the soaking temperature is 120-160 ℃;
the soaking pressure is 0.8-1MPa.
2. The method of removing cobalt from a polycrystalline diamond compact of claim 1, wherein the lewis acid is aluminum trichloride or ferric trichloride.
3. The method of removing cobalt from a polycrystalline diamond compact of claim 1, wherein the phosphate is sodium dihydrogen phosphate or potassium dihydrogen phosphate.
4. The method of removing cobalt from a polycrystalline diamond compact of claim 1, wherein the soaking time is between 5 days and 15 days.
5. The method of removing cobalt from a polycrystalline diamond compact of claim 1, wherein the thickness of the composite layer of the polycrystalline diamond compact is 1.2mm to 3mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104532016A (en) * | 2014-12-23 | 2015-04-22 | 西安石油大学 | Cobalt leaching method of cobalt-leached composite acid based on synthetic polycrystalline diamond composite sheet |
| CN110144618A (en) * | 2019-06-03 | 2019-08-20 | 河南四方达超硬材料股份有限公司 | Method for removing metallic cobalt in polycrystalline diamond compact |
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| EP1738773A1 (en) * | 2005-06-29 | 2007-01-03 | Schering AG | Composition comprising magnetic iron oxide particles and use thereof in medical imaging |
| US20100011673A1 (en) * | 2008-07-18 | 2010-01-21 | James Shamburger | Method and apparatus for selectively leaching portions of PDC cutters through templates formed in mechanical shields placed over the cutters |
| JP2013096778A (en) * | 2011-10-31 | 2013-05-20 | Vision Development Co Ltd | Treatment method of waste liquid containing metal atom, and adsorbent |
| CN202417313U (en) * | 2011-12-01 | 2012-09-05 | 西南石油大学 | Single cone bit with PDC (Polycrystalline Diamond Compact) teeth |
| US8961630B2 (en) * | 2012-05-04 | 2015-02-24 | Baker Hughes Incorporated | Methods of forming cutting elements by removing metal from interstitial spaces in polycrystalline diamond |
| US10246335B2 (en) * | 2016-05-27 | 2019-04-02 | Baker Hughes, A Ge Company, Llc | Methods of modifying surfaces of diamond particles, and related diamond particles and earth-boring tools |
| CN109576701A (en) * | 2019-01-28 | 2019-04-05 | 深圳市海明润超硬材料股份有限公司 | The process for surface preparation and diamond compact preparation method of hard alloy substrate |
| CN111911082B (en) * | 2020-07-11 | 2022-03-22 | 长江大学 | Method for strengthening polycrystalline diamond compact |
| CN112915922A (en) * | 2021-01-27 | 2021-06-08 | 山东昌润钻石股份有限公司 | Primary synthesis method of superfine diamond |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104532016A (en) * | 2014-12-23 | 2015-04-22 | 西安石油大学 | Cobalt leaching method of cobalt-leached composite acid based on synthetic polycrystalline diamond composite sheet |
| CN110144618A (en) * | 2019-06-03 | 2019-08-20 | 河南四方达超硬材料股份有限公司 | Method for removing metallic cobalt in polycrystalline diamond compact |
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