CN112158835A - Synthesis method of carbon material with super-strong hardness - Google Patents
Synthesis method of carbon material with super-strong hardness Download PDFInfo
- Publication number
- CN112158835A CN112158835A CN202011005000.2A CN202011005000A CN112158835A CN 112158835 A CN112158835 A CN 112158835A CN 202011005000 A CN202011005000 A CN 202011005000A CN 112158835 A CN112158835 A CN 112158835A
- Authority
- CN
- China
- Prior art keywords
- pressure
- sample
- carbon material
- fullerene
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses a synthesis method of a carbon material with super-strong hardness, and belongs to the technical field of preparation of superhard materials. The method comprises the following specific steps: and dispersing fullerene in the nano diamond powder, uniformly mixing, putting into a high-pressure device, sintering for 1 hour under the temperature and pressure conditions of 13GPa and 2100k, quenching a sample, relieving the pressure to normal pressure, grinding, polishing and cleaning to obtain the pure composite superhard carbon material. The composite superhard carbon material is prepared by doping a small amount of fullerene and sintering at high temperature and high pressure, and the prepared composite superhard carbon material has great application potential and value in the fields of aerospace, geological survey, machine tool tools and the like.
Description
Technical Field
The invention belongs to the technical field of superhard material preparation. In particular to a superhard carbon material with excellent performance prepared by a high-temperature and high-pressure means of a large-cavity press.
Background
Generally, a material with the Vickers hardness of more than 40GPa is defined as a superhard material, and the superhard material is a novel functional material, has excellent mechanical properties and is widely applied to the fields of metallurgy, geology, national defense, military industry and the like. Diamond and cubic boron nitride are well known superhard materials, and the diamond is the hardest natural material (with the Vickers hardness of 70GPa-100 GPa), has high bulk modulus (442GPa), high melting point (3730 ℃) and high thermal conductivity (20W/cmK), but the single crystal diamond has poor thermal stability and chemical inertness, is easy to brittle fracture along a 111 cleavage plane, and has low compressive strength and insufficient toughness. Cubic boron nitride has excellent thermal stability and chemical inertness, but has a vickers hardness of only half that of diamond. How to further improve the hardness of the superhard material becomes a research direction for researchers to make continuous efforts. Recently, research shows that the mechanical properties such as hardness and the like of the polycrystalline diamond block can be greatly improved by introducing a nanometer twin structure, but the synthesis conditions are harsh, the pressure and the temperature are respectively higher than 18GPa and 1850 ℃, and a special onion-shaped nanometer structure is required to be used as a precursor, so that the requirement of large-scale industrial preparation cannot be met. How to prepare the superhard material with mechanical properties, particularly hardness superior to that of diamond, and the preparation under the condition of milder temperature and pressure is still an important scientific problem in the field.
Disclosure of Invention
In order to overcome the defects in the background art, the invention aims to provide a method for synthesizing a composite superhard carbon material by doping nano diamond powder, solve the problem of synthesizing the superhard carbon material with good mechanical property, and further provide a method for regulating and controlling the hardness and toughness of the superhard carbon material by changing the doping amount of fullerene.
The specific technical scheme of the invention is as follows:
a method for synthesizing a carbon material with super-strong hardness comprises the following steps:
the method comprises the following steps: dispersing fullerene in nano diamond powder, and grinding for 4-5 hours by using a mortar with the diameter of 50mm to uniformly mix an initial sample; according to the mass percent, the fullerene accounts for 4-6% of the mixture;
step two: putting the uniformly mixed initial sample into a high-pressure device, setting the temperature and pressure conditions of 13GPa and 2100k for sintering, keeping the temperature and pressure for 1 hour, immediately quenching the sample to room temperature, slowly releasing the pressure to normal pressure, and taking out the sample;
step three: and grinding and polishing the obtained sample, then respectively soaking and cleaning the sample by using acetone, and carrying out ultrasonic treatment by using ethanol to obtain the pure composite superhard carbon material.
Preferably, in step one, the fullerene comprises 5% of the mixture.
Preferably, the nano diamond powder has a particle size of 30 nm.
Has the advantages that:
because the doped fullerene can be subjected to carbon-carbon bond fracture and reconstruction under the conditions of high temperature and high pressure and finally converted into amorphous carbon or nano-diamond, on one hand, the welding with the nano-diamond grains in the precursor is realized, and on the other hand, the stress between the diamond grains under the conditions of high temperature and high pressure is relieved and absorbed, so that a stronger grain boundary effect is formed between the diamond grains, the hardness of the formed polycrystalline block is improved greatly, and particularly the composite superhard carbon material doped with a small amount of fullerene. The prepared composite superhard carbon material has great application potential and value in the fields of aerospace, geological survey, machine tool tools and the like.
Drawings
FIG. 1: TEM photograph of nanodiamond.
FIG. 2: and the doping proportion of the fullerene is 5 percent of the Raman spectrum of the nano-diamond.
FIG. 3: XRD of nanodiamond with fullerene doping ratio of 5%.
FIG. 4: normal temperature and normal pressure infrared spectrum of the nano-diamond before and after the high temperature annealing of the tube furnace.
FIG. 5: and (3) carrying out high-temperature and high-pressure treatment on the pure nano-diamond sample by using a large-cavity press to obtain an optical photo.
FIG. 6: and (3) an optical photo of the nano-diamond with the fullerene doping ratio of 5% after the high-temperature and high-pressure treatment of the large-cavity press.
FIG. 7: and (3) an optical photo of the nano-diamond with the fullerene doping ratio of 10% after the high-temperature and high-pressure treatment of the large-cavity press.
FIG. 8: SEM photograph of pure nano-diamond sample after high temperature and high pressure treatment by large cavity press.
FIG. 9: SEM photograph of the nano diamond with the fullerene doping ratio of 5% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 10: SEM photograph of nano diamond with fullerene doping ratio of 10% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 11: TEM photograph of pure nano-diamond sample after high temperature and high pressure treatment by large cavity press.
FIG. 12: and (3) TEM (transmission electron microscope) photos of the nano-diamond with the fullerene doping ratio of 5% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 13: TEM photograph of nano-diamond with fullerene doping ratio of 10% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 14: HRTEM picture of pure nano-diamond sample after high temperature and high pressure treatment by large cavity press.
FIG. 15: HRTEM photograph of the nano-diamond with the fullerene doping ratio of 5% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 16: HRTEM photograph of the nano-diamond with the fullerene doping ratio of 5% after high-temperature and high-pressure treatment by a large-cavity press.
FIG. 17: raman spectra of three different composite superhard carbon materials processed by a large-cavity press at high temperature and high pressure.
FIG. 18: XRD diffraction spectra of three different composite superhard carbon materials processed by a large-cavity press at high temperature and high pressure.
FIG. 19: the relationship graph of the Vickers hardness fracture indentation graph and the hardness value and the load of three different composite superhard carbon materials processed by a large-cavity press at high temperature and high pressure.
FIG. 20: fracture indentation patterns of three different composite superhard carbon materials subjected to high-temperature high-pressure treatment by a large-cavity press.
FIG. 21 is a graph showing fracture toughness of other superhard carbon materials such as diamond.
FIG. 22 is a schematic view of a large chamber press assembly.
The specific implementation mode is as follows:
the invention will be further illustrated with reference to specific examples.
Example 1:
10mg of nanodiamond powder (30nm) was weighed out, annealed at 550 ℃ for 1h in a tube furnace under argon atmosphere at a temperature rise rate of 10 ℃ per minute, and then cooled to room temperature. The samples before and after stress relief annealing were subjected to infrared testing (fig. 4) to see if some of the defects were removed. And (4) carrying out XRD (X-ray diffraction) test and Raman test on the sample before and after annealing, and observing whether the sample has a deterioration phenomenon. The obtained sample is put into a Max Voggenzeitez, LPR1000-400/50 type sixty-eight large-size high-pressure device without deterioration phenomenon for assembly (as shown in figure 22), wherein in a figure, 1 is magnesium oxide; 2 is rhenium sheet; 3 is boron nitride; 4 is lanthanum chromate; 5 is four-hole alumina; 6 is a thermocouple; 7 is an aluminum oxide sheet; 8 is a sample; 9 is zirconium dioxide; 10 is magnesium oxide. And b and c are diagrams of the assembly mode of the thermocouple, then the assembly block is placed in a large-cavity press to carry out a high-temperature high-pressure experiment, the temperature and pressure conditions of 13GPa and 2100k are set for sintering, the heat preservation and pressure maintaining time is about 1h, the sample is immediately quenched to the room temperature, and the pressure is slowly released to the normal pressure to take out the sample (as shown in figure 5). And grinding and polishing the obtained sample by using an electroplating diamond grinding disc, then respectively soaking and cleaning the sample by using acetone for 30min, then carrying out ultrasonic treatment by using ethanol for 30min to obtain a pure composite superhard carbon material, and then carrying out scanning test (as shown in figure 8) to ensure that the pure superhard carbon material is finally obtained.
The obtained carbon material was subjected to XRD test (fig. 18) and Raman test (fig. 17), respectively, and it was found that the sample still maintained the diamond structure and had good crystallinity, and it was observed under a transmission electron microscope that significant "rounding" and "thinning" occurred in the diamond particles in the polycrystalline body after the high-temperature and high-pressure treatment (see fig. 11), i.e., the portions with edges and corners at the boundaries were ground flat, and a phenomenon where many small diamond particles filled the gaps between the diamond particles occurred.
Example 2:
and dispersing the weighed 1mg of fullerene in 19mg of nano-diamond powder (30nm), and slowly grinding the fullerene by using a mortar with the diameter of 50mm, wherein the time is controlled to be 4-5 hours, so that the initial sample is uniformly mixed. And putting the mixed sample into a tube furnace, annealing the sample at high temperature at 550 ℃ at the heating rate of 10 ℃/min under the argon atmosphere, and then cooling to room temperature. The initial samples are respectively subjected to characterization such as XRD test (shown in figure 2), Raman test (shown in figure 3) and the like, and further the initial samples are well mixed and are not degenerated under high-temperature treatment.
Putting the obtained uniformly mixed initial sample into a Max Voggenzeitez, LPR1000-400/50 type sixty-eight large-size high-pressure device, assembling (as shown in figure 22), and performing high-temperature high-pressure experiment in the same way as in example 1, then putting the assembled block into a large-cavity press, performing sintering under the temperature and pressure conditions of 13GPa and 2100k, keeping the temperature and pressure for about 1h, immediately quenching the sample to room temperature, and slowly releasing the pressure to the normal pressure to take out the sample (as shown in figure 6). And grinding and polishing the obtained sample by using an electroplating diamond grinding disc, then respectively soaking and cleaning the sample by using acetone for 30min, then carrying out ultrasonic treatment by using ethanol for 30min to obtain a pure composite superhard carbon material, and then carrying out scanning test (as shown in figure 9) to ensure that the pure composite superhard carbon material is finally obtained.
The obtained composite superhard carbon material is subjected to XRD test (shown in figure 18) and Raman test (shown in figure 17), the sample sintered at high temperature and high pressure still keeps the structure of diamond and has good crystallinity, and the doped fullerene is converted into amorphous carbon after being sintered at high temperature and high pressure. Comparing the electron microscope image of diamond (as shown in fig. 11) with the electron microscope image of the composite superhard carbon material doped with 10% fullerene (as shown in fig. 13), the ultrafine grains formed by the diamond crushing are greatly reduced, and part of the boundaries of the diamond grains have amorphous carbon-like substances, namely, the doped fullerene is converted into amorphous carbon at high temperature and high pressure to bond the diamond grains, so that the superhard composite carbon structure is formed. The above characterization proves that the sample obtained by the synthesis method is the composite superhard carbon material doped with amorphous carbon.
Example 3:
and dispersing the weighed 1mg of fullerene in 9mg of nano-diamond powder (30nm), and slowly grinding the fullerene by using a mortar with the diameter of 50mm, wherein the time is controlled to be 4-5 hours, so that the initial sample is uniformly mixed. And putting the mixed sample into an argon atmosphere, annealing the sample at a high temperature of 550 ℃ at a heating rate of 10 ℃/min, and then cooling to room temperature. Respectively carrying out characterization such as XRD (X-ray diffraction) test and Raman test on the initial sample, and further verifying that the initial sample is uniformly mixed and does not deteriorate under high-temperature treatment.
Putting the obtained uniformly mixed initial sample into a Max Voggenzeitez, LPR1000-400/50 type sixty-eight large-size high-pressure device, assembling (as shown in figure 22), performing high-temperature high-pressure experiment in the same way as in example 1, putting the assembled block into a large-cavity press, performing sintering under the temperature and pressure conditions of 13GPa and 2000k, keeping the temperature and pressure for about 1h, immediately quenching the sample to room temperature, and slowly releasing the pressure to the normal pressure to take out the sample (as shown in figure 7). And grinding and polishing the obtained sample by using an electroplating diamond grinding disc, then respectively soaking and cleaning the sample by using acetone for 30min, then carrying out ultrasonic treatment by using ethanol for 30min to obtain a pure composite superhard carbon material, and then carrying out scanning test (as shown in figure 10) to ensure that the pure composite superhard carbon material is finally obtained.
The obtained composite superhard carbon material is subjected to XRD test (shown in figure 18) and Raman test (shown in figure 17), the sample sintered at high temperature and high pressure still keeps the structure of diamond and has good crystallinity, and the doped fullerene is converted into amorphous carbon or nano-diamond after being sintered at high temperature and high pressure. Comparing an electron microscope image (as shown in fig. 12) of a product obtained by directly sintering diamond nanocrystals with an electron microscope image (as shown in fig. 12) of a composite superhard carbon material doped with 5% fullerene, a sample obtained by high-temperature and high-pressure sintering in the case has good crystallinity, and the sample has the defects that diamond particle boundaries are adhered by amorphous carbon in most regions and some small nano diamonds are also present. In other words, 10% of the doped fullerene is partially converted into amorphous carbon at high temperature and high pressure and appears at the grain boundary of the nano-diamond, so as to play a role of 'bonding' grains, and meanwhile, the excessive fullerene is converted into nano-diamond particles at high temperature and high pressure and appears in the composite block. The above characterization proves that the sample obtained by the synthesis method is the composite superhard carbon material doped with amorphous carbon.
The above embodiments 1 and 3 are comparative examples, which do not fall within the scope of the present invention, and embodiment 2 is the most preferable embodiment of the technical solution of the present invention.
Example 4:
and (5) testing mechanical properties.
(1) And polishing the three samples sintered at high temperature and high pressure by using a diamond grinding sheet and diamond powder polishing solution.
(2) And when the polished surface reaches the mirror surface degree, washing away the residual polishing solution on the surface of the sample by using ethanol.
(3) The hardness of the sintered samples was tested using a vickers microhardness tester, the hardness values of the three samples were tested under loads of 1.96N, 2.94N, 4.9N, 9.8N, 19.6N, 29.4N, respectively, at least five hardness values were tested under each load, and the average value was found to reduce the error. The vickers hardness values versus load are shown in fig. 19, which is a photograph of an indentation of three materials under a load of 9.8N.
(4) And (3) carrying out fracture toughness test on the sintered sample by using a Vickers microhardness tester, respectively testing fracture toughness values of the three samples under 29.4N load, testing at least five hardness values under the load, and calculating an average value to reduce errors. The impression picture under a load of 29.4N is shown in fig. 20.
Analysis of Experimental results
By adding fullerene with different proportions in the process of sintering the nano-diamond at high temperature and high pressure, the hardness of the obtained nano-polycrystalline composite material can be effectively improved, and the fracture toughness of the nano-polycrystalline composite material is improved. In the nano polycrystalline diamond obtained by sintering, a sample has good crystallinity, and an amorphous carbon grain boundary structure appears among partial diamond grains, namely when a proper amount of the nano polycrystalline diamond is added, fullerene is converted into amorphous carbon at high temperature and high pressure to adhere the diamond nano grains, so that the high-performance polycrystalline composite block is formed.
The superhard carbon material synthesized under the high-temperature and high-pressure conditions has a better hardness value, the convergence value of the hardness under the load of 29.4N is more than 110Gpa, and the hardness value of the material doped with 5% of the superhard carbon material is more than 140GPa and is higher than that of single crystal diamond. As shown in FIG. 21, the incorporation of fullerenes of different percentages has a control effect on mechanical properties such as Vickers hardness and fracture toughness of the synthesized samples. As can be seen from the transmission electron microscope picture, the addition of a proper amount of fullerene can form an amorphous carbon structure at the boundary of diamond grains, on one hand, the diamond nanocrystals are adhered, on the other hand, the stress between the diamond grains at high temperature and high pressure is relieved and absorbed, so that a stronger grain boundary effect is formed between the diamond grains, the hardness of the formed polycrystalline block is greatly improved, and the hardness is 20% higher than that of the block sintered without the addition of the fullerene. Along with the increase of the addition percentage of the fullerene, the fracture toughness of the synthesized novel superhard material is also improved, which shows that the fracture toughness of the superhard material can be indirectly adjusted by adjusting the content of the fullerene. The fracture toughness of the single crystal diamond is 5-13.5 MPa ^1/2, and the fracture toughness of the twin crystal diamond is 10-15 MPa ^ 1/2. Comparing with fig. 21, the superhard carbon material formed by sintering the doped fullerene under the conditions of high temperature and high pressure has more excellent hardness and fracture toughness. In conclusion, the composite superhard carbon material formed by the fullerene doped diamond synthesized by the invention has higher hardness and better fracture toughness than single crystal diamond.
Fullerene is a good basic carbon material, atoms are alternately combined through single bonds and double bonds, double bonds of fullerene molecules are opened under certain conditions, and stable covalent bonds can be formed with adjacent molecules through cycloaddition forms such as [ 2+2 ], [ 3+3 ], [ 4+4 ] and the like at high temperature and high pressure, so that different polymers are obtained. The embodiment shows that the invention synthesizes the superhard carbon material with ultrahigh hardness by taking the powder mixed by fullerene and nano-diamond as a precursor through high-temperature and high-pressure means, and opens up a new way for preparing novel composite superhard materials.
Claims (3)
1. A method for synthesizing a carbon material with super-strong hardness comprises the following steps:
the method comprises the following steps: dispersing fullerene in nano diamond powder, and grinding for 4-5 hours by using a mortar with the diameter of 50mm to uniformly mix an initial sample; according to the mass percent, the fullerene accounts for 4-6% of the mixture;
step two: putting the uniformly mixed initial sample into a high-pressure device, setting the temperature and pressure conditions of 13GPa and 2100k for sintering, keeping the temperature and pressure for 1 hour, immediately quenching the sample to room temperature, slowly releasing the pressure to normal pressure, and taking out the sample;
step three: and grinding and polishing the obtained sample, then respectively soaking and cleaning the sample by using acetone, and carrying out ultrasonic treatment by using ethanol to obtain the pure composite superhard carbon material.
2. The method as claimed in claim 1, wherein the fullerene is 5% of the mixture in the first step.
3. The method as claimed in claim 1 or 2, wherein the nano-diamond powder has a particle size of 30 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011005000.2A CN112158835A (en) | 2020-09-23 | 2020-09-23 | Synthesis method of carbon material with super-strong hardness |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011005000.2A CN112158835A (en) | 2020-09-23 | 2020-09-23 | Synthesis method of carbon material with super-strong hardness |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112158835A true CN112158835A (en) | 2021-01-01 |
Family
ID=73864345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011005000.2A Pending CN112158835A (en) | 2020-09-23 | 2020-09-23 | Synthesis method of carbon material with super-strong hardness |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112158835A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896533A (en) * | 2021-09-26 | 2022-01-07 | 吉林大学 | Millimeter-scale sp3Amorphous carbon block and preparation method thereof |
| CN114763307A (en) * | 2021-01-15 | 2022-07-19 | 燕山大学 | Layered carbon grain boundary phase toughened diamond composite phase material and preparation method thereof |
| CN114855021A (en) * | 2022-05-26 | 2022-08-05 | 山东省科学院新材料研究所 | Preparation method of fullerene raw ash modified diamond/aluminum composite material |
| CN116143518A (en) * | 2021-11-23 | 2023-05-23 | 燕山大学 | Conductive high-strength diamond/amorphous carbon composite material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070187153A1 (en) * | 2006-02-10 | 2007-08-16 | Us Synthetic Corporation | Polycrystalline diamond apparatuses and methods of manufacture |
| CN105401034A (en) * | 2015-12-12 | 2016-03-16 | 河南广度超硬材料有限公司 | High-density polycrystalline superhard material and preparation method thereof |
| CN106518077A (en) * | 2016-10-19 | 2017-03-22 | 四川大学 | Method for preparing high-purity polycrystalline diamond |
| CN108786659A (en) * | 2018-07-09 | 2018-11-13 | 吉林大学 | A kind of synthetic method of the composite superhard material with high-fracture toughness |
| CN109400160A (en) * | 2018-12-25 | 2019-03-01 | 吉林大学 | A kind of composite superhard material and its synthetic method |
| CN111233476A (en) * | 2020-01-17 | 2020-06-05 | 成都东为科技有限公司 | Binder-free polycrystalline diamond material and preparation method thereof |
-
2020
- 2020-09-23 CN CN202011005000.2A patent/CN112158835A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070187153A1 (en) * | 2006-02-10 | 2007-08-16 | Us Synthetic Corporation | Polycrystalline diamond apparatuses and methods of manufacture |
| CN105401034A (en) * | 2015-12-12 | 2016-03-16 | 河南广度超硬材料有限公司 | High-density polycrystalline superhard material and preparation method thereof |
| CN106518077A (en) * | 2016-10-19 | 2017-03-22 | 四川大学 | Method for preparing high-purity polycrystalline diamond |
| CN108786659A (en) * | 2018-07-09 | 2018-11-13 | 吉林大学 | A kind of synthetic method of the composite superhard material with high-fracture toughness |
| CN109400160A (en) * | 2018-12-25 | 2019-03-01 | 吉林大学 | A kind of composite superhard material and its synthetic method |
| CN111233476A (en) * | 2020-01-17 | 2020-06-05 | 成都东为科技有限公司 | Binder-free polycrystalline diamond material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114763307A (en) * | 2021-01-15 | 2022-07-19 | 燕山大学 | Layered carbon grain boundary phase toughened diamond composite phase material and preparation method thereof |
| CN113896533A (en) * | 2021-09-26 | 2022-01-07 | 吉林大学 | Millimeter-scale sp3Amorphous carbon block and preparation method thereof |
| CN113896533B (en) * | 2021-09-26 | 2023-04-14 | 吉林大学 | Millimeter-scale sp 3 Amorphous carbon block and method for producing same |
| CN116143518A (en) * | 2021-11-23 | 2023-05-23 | 燕山大学 | Conductive high-strength diamond/amorphous carbon composite material and preparation method thereof |
| CN114855021A (en) * | 2022-05-26 | 2022-08-05 | 山东省科学院新材料研究所 | Preparation method of fullerene raw ash modified diamond/aluminum composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112158835A (en) | Synthesis method of carbon material with super-strong hardness | |
| CN109252081A (en) | A kind of high-entropy alloy Binder Phase ultrafine tungsten carbide hard alloy and preparation method thereof | |
| US6395214B1 (en) | High pressure and low temperature sintering of nanophase ceramic powders | |
| JP2005514300A (en) | Low oxygen cubic boron nitride and its products | |
| CN109437920B (en) | Nanometer/submicron structure wBN superhard material, wBN-cBN superhard composite material, preparation method and cutter | |
| JP2008517868A (en) | Cubic boron nitride compact | |
| JP2015529611A (en) | Ultra-hard nano-twinned boron nitride bulk material and synthesis method thereof | |
| US20180009716A1 (en) | Friable ceramic-bonded diamond composite particles and methods to produce same | |
| CN109400160A (en) | A kind of composite superhard material and its synthetic method | |
| WO2020186752A1 (en) | Method for preparing superfine grain wc-co hard alloy by means of plasma ball milling | |
| CN112299861B (en) | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic | |
| RU2312844C2 (en) | Heat-resistant composite diamond sintered article and the method of its production | |
| CN110436928A (en) | High-performance nano twin boron carbide ceramics block materials and preparation method thereof | |
| CN110342943A (en) | The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses | |
| Ekimov et al. | Mechanical properties and microstructure of diamond–SiC nanocomposites | |
| CN111116206A (en) | Preparation method of compact MoAlB ceramic material, product thereof and preparation method of high-purity MoAlB ceramic powder | |
| US10541064B2 (en) | SiC powder, SiC sintered body, SiC slurry and manufacturing method of the same | |
| CN112678817A (en) | Preparation method of millimeter polycrystalline diamond | |
| CN111172443A (en) | High-comprehensive-performance hard alloy cutter material and preparation method thereof | |
| CN108786659A (en) | A kind of synthetic method of the composite superhard material with high-fracture toughness | |
| JP4106590B2 (en) | Cubic boron nitride sintered body and manufacturing method thereof | |
| Ovsyannikov et al. | High-hardness ceramics based on boron carbide fullerite derivatives | |
| CN113149658B (en) | Titanium nitride-based composite ceramic material and preparation method thereof | |
| CN115010503A (en) | Use method of sintering aid for transparent oxide ceramic material | |
| JP4061374B2 (en) | Method for producing ultrafine particle cBN sintered body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210101 |