CN112495303B - Self-sharpening diamond and preparation method thereof - Google Patents
Self-sharpening diamond and preparation method thereof Download PDFInfo
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- CN112495303B CN112495303B CN202011336269.9A CN202011336269A CN112495303B CN 112495303 B CN112495303 B CN 112495303B CN 202011336269 A CN202011336269 A CN 202011336269A CN 112495303 B CN112495303 B CN 112495303B
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- 239000010432 diamond Substances 0.000 title claims abstract description 81
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 76
- 239000010439 graphite Substances 0.000 claims abstract description 76
- 239000002245 particle Substances 0.000 claims abstract description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005121 nitriding Methods 0.000 claims abstract description 25
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 20
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 19
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 18
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052796 boron Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims description 27
- 229910000831 Steel Inorganic materials 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000010959 steel Substances 0.000 claims description 23
- 239000000919 ceramic Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000462 isostatic pressing Methods 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 9
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000005087 graphitization Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000000465 moulding Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 16
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 4
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 239000013078 crystal Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000002194 synthesizing effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- -1 iron-chromium-aluminum Chemical compound 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- 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
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- 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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of diamonds, and particularly relates to a self-sharpening diamond and a preparation method thereof. The self-sharpening diamond provided by the invention is prepared by nitriding a graphite column; the graphite column comprises the following components in percentage by mass: 28-31% of cobalt, 9-12% of nickel, 1.8-2% of cerium, 0.8-1% of boron and 55-59% of graphite. In the invention, the surface of the self-sharpening diamond particles is rough due to the cerium with specific content, so that the self-sharpening diamond falls off in a micro-blade crushing mode in the grinding process to expose a new sharp surface, the self-sharpening diamond keeps a continuous sharp surface, and the utilization rate of the self-sharpening diamond is improved; meanwhile, the self-sharpening diamond provided by the invention is subjected to nitriding treatment in the preparation process, so that nitrogen atoms replace part of carbon atoms in the diamond in the synthesis process of the diamond, and the strength of the self-sharpening diamond is reduced.
Description
Technical Field
The invention belongs to the technical field of diamonds, and particularly relates to a self-sharpening diamond and a preparation method thereof.
Background
Diamond is the hardest substance in nature and is mainly used in the fields of cutting, grinding, polishing, drilling and the like. Along with the continuous development of science and technology, the application field of diamond is continuously expanded in recent years, and the diamond is related to various industries such as weapons, aerospace, stone building materials, semiconductors, photovoltaic industry, precious stones, mining, automobile machinery, electronic appliances and the like; the amount of diamond used has also increased year by year. However, when the diamond is applied to some hard materials (such as zirconia-related materials, hard alloy, stainless steel, etc.), the utilization rate is low, and resource waste is easily caused.
The technical problem that the diamond with higher utilization rate is prepared to reduce resource waste is urgently needed to be solved at present.
Disclosure of Invention
In view of the above, the present invention provides a self-sharpening diamond, which has a rough surface, and is broken by a micro blade during grinding to expose a new sharp surface, so that the self-sharpening diamond can maintain a continuous sharp surface, and the utilization rate of the diamond is improved.
The invention provides a self-sharpening diamond, which is prepared by nitriding a graphite column; the graphite column comprises the following components in percentage by mass:
the invention also provides a preparation method of the self-sharpening diamond in the technical scheme, which comprises the following steps:
mixing cobalt, nickel, cerium, boron and graphite according to the raw material ratio, and then pressing and forming to obtain a graphite column;
and nitriding and pressing the graphite column in sequence to synthesize the self-sharpening diamond.
Preferably, the cobalt, the nickel, the cerium, the boron and the graphite are powdery, and the particle sizes of the cobalt, the nickel, the cerium, the boron and the graphite are independently less than or equal to 48 mu m.
Preferably, the graphite is graphite subjected to graphitization treatment, the graphitization treatment temperature is 2800-3000 ℃, and the time is 25-30 days.
Preferably, the pressure of the nitriding treatment is 0.5-0.7 MPa, and the time is 23-25 h.
Preferably, the pressing synthesis is carried out in a press, the pressure of the pressing synthesis is 4.8-5 Gpa, the temperature is 1350-1400 ℃, and the time is 34-38 min.
Preferably, the press forming comprises the steps of:
carrying out isostatic pressing treatment on the mixed material obtained by mixing to obtain a high-density forming body;
and crushing the high-density forming body, and pressing into a graphite column.
Preferably, the pressure of the isostatic pressing treatment is 180-190 MPa, and the time is 10-15 min; the pressure of the first pressing is 60-65 MPa, and the time is 4-6 s.
Preferably, the nitriding-treated graphite columns are assembled before the press synthesis, and the assembling comprises the following steps:
putting the graphite column into a steel cup, and putting the steel cup with the graphite column into a ceramic insulating cup;
arranging a heating belt on the surface of the ceramic insulating cup, and then filling the heating belt into a pyrophyllite block to obtain a primary synthetic block;
and (3) additionally arranging heating sheets and steel caps at two ends of the primary synthetic block to obtain the synthetic block.
Preferably, before the synthetic block is pressed and synthesized, the synthetic block is baked at the temperature of 120-140 ℃ for 7.5-8.5 hours.
The invention provides a self-sharpening diamond, which is prepared by nitriding a graphite column; the graphite column comprises the following components in percentage by mass: 28-31% of cobalt, 9-12% of nickel, 1.8-2% of cerium, 0.8-1% of boron and 55-59% of graphite. In the invention, the cerium with a specific content mainly plays a role in doping in the synthesis process of the self-sharpening diamond, so that the crystal of the self-sharpening diamond is defective and incomplete, the surface roughness of the self-sharpening diamond particles is improved, the self-sharpening diamond falls off in a micro-blade breaking mode in the grinding process to expose a new sharp surface, the self-sharpening diamond keeps a continuous sharp surface, and the utilization rate of the self-sharpening diamond is improved; meanwhile, the self-sharpening diamond provided by the invention is subjected to nitriding treatment in the preparation process, so that nitrogen atoms replace part of carbon atoms in the diamond in the synthesis process of the diamond, and the strength of the self-sharpening diamond is reduced.
Detailed Description
The invention provides a self-sharpening diamond, which is prepared by nitriding a graphite column; the graphite column comprises the following components in percentage by mass:
in the present invention, all the above-mentioned raw materials are conventional commercially available products unless otherwise specified.
In the invention, the graphite column comprises 28-31% of cobalt by mass percentage, preferably 28.9-30.6%.
In the invention, the graphite column comprises 9-12% of nickel by mass percentage, and preferably 9.3-10.2%.
In the invention, the graphite column comprises 1.8-2% of cerium by mass percentage, and preferably 1.9-2%.
In the invention, the graphite column comprises 0.8-1% of boron by mass percentage, and preferably 0.9-1%. In the invention, the boron can enter the diamond crystal lattice to be bonded with carbon in the diamond in a B-C bond mode, so that the surface of the diamond crystal is rough, and the {111} plane is developed, thereby effectively preventing or delaying the oxidation of the self-sharpening diamond and leading the self-sharpening diamond to have thermal stability obviously superior to that of the conventional diamond. In the invention, the boron improves the high temperature resistance of the self-sharpening diamond by 150-200 ℃.
In the invention, the graphite column comprises 55-59% of graphite by mass percentage, and preferably 56.1-58.9%.
In the invention, the self-sharpening diamond is prepared by nitriding a graphite column. In the invention, the nitriding treatment enables nitrogen atoms to enter the graphite column, and the nitrogen atoms in the graphite column enter the self-sharpening diamond crystal lattice to partially replace carbon atoms in the process of synthesizing the diamond, so that the growth speed of the self-sharpening diamond is increased, and the strength of the self-sharpening diamond is reduced.
The existing single crystal diamond can fall off after being impacted or worn to remove edges and corners in the grinding process, and the utilization rate of the whole single crystal diamond is generally less than 25%. In the invention, the cerium with the specific content plays a doping role in the self-sharpening diamond synthesis process, so that self-sharpening diamond crystals are incomplete and generate defects, self-sharpening diamond particles with rough surfaces are obtained, the self-sharpening diamond falls off in a micro-blade breaking mode in the grinding process to expose new sharp surfaces, and the self-sharpening diamond keeps continuous sharp surfaces. In the invention, the micro-blade crushing mode is that each falling accounts for about 1% of the specific gravity of the whole diamond, so that the overall utilization rate of the diamond reaches more than 50%, and the utilization rate of the self-sharpening diamond is improved.
The invention also provides a preparation method of the self-sharpening diamond in the technical scheme, which comprises the following steps:
mixing cobalt, nickel, cerium, boron and graphite according to the raw material ratio, and then pressing and forming to obtain a graphite column;
and nitriding and pressing the graphite column in sequence to synthesize the self-sharpening diamond.
According to the invention, cobalt, nickel, cerium, boron and graphite are mixed according to the raw material ratio and then are pressed and formed to obtain the graphite column. In the invention, the cobalt is preferably cobalt powder, and the particle size of the cobalt powder is preferably less than or equal to 48 mu m, and more preferably 45-47.5 mu m. In the invention, the nickel is preferably nickel powder, and the particle size of the nickel powder is preferably less than or equal to 48 mu m, and more preferably 45-47.5 mu m. In the invention, the cerium is preferably cerium powder, and the particle size of the cerium powder is preferably less than or equal to 48 mu m, and more preferably 45-47.5 mu m. In the invention, the boron is preferably boron powder, and the particle size of the boron powder is preferably less than or equal to 48 μm, and more preferably 45-47.5 μm. In the invention, the purity of the graphite is preferably more than or equal to 99.999 percent; the graphite is preferably graphite powder, and the particle size of the graphite powder is preferably less than or equal to 48 mu m, and more preferably 40-47.5 mu m. In the invention, the graphite powder is preferably graphite subjected to graphitization treatment, and the graphitization treatment temperature is preferably 2800-3000 ℃, and more preferably 2850-2900 ℃; the time is preferably 25 to 30 days, and more preferably 26 to 28 days. In the present invention, the graphitization treatment can improve the purity of graphite.
The invention limits the particle size of each raw material, can uniformly mix the materials, and is beneficial to obtaining the self-sharpening diamond with higher structural consistency.
The invention has no special requirement on the mixing as long as the materials can be uniformly mixed, and in the embodiment of the invention, the mixing device is a three-dimensional mixer, the volume of the mixed materials is not more than 50% of the volume of a mixing barrel in the three-dimensional mixer, and the mixing time is 24 hours.
In the present invention, the press forming includes the steps of:
carrying out isostatic pressing treatment on the mixed material obtained by mixing to obtain a high-density forming body;
and crushing the high-density forming body, and pressing into a graphite column.
The invention carries out isostatic pressing treatment on the mixture obtained by mixing to obtain a high-density formed body. In the invention, the pressure of the isostatic pressing treatment is preferably 180-190 MPa, and more preferably 183-187 MPa; the time is preferably 10 to 15min, and more preferably 12 to 13 min. In the invention, the high-density forming body is preferably a cylinder, and the diameter of the cylinder is preferably 180-220 mm, and more preferably 200 mm; the height is preferably 480-520 mm, and more preferably 500 mm. In the invention, the isostatic pressing treatment can increase the density of the mixture, and is beneficial to the subsequent first pressing.
After the high-density forming body is obtained, the high-density forming body is crushed and then is firstly pressed into the graphite column. In the invention, the particle size of the crushed particles is preferably 2.8-3.3 mm, and more preferably 3-3.1 mm. The method of crushing is not particularly limited in the present invention as long as the desired particle diameter can be obtained. In the invention, the pressure of the first pressing is preferably 60-65 MPa, and more preferably 63-65 MPa; the time is preferably 4 to 6 seconds, and more preferably 4.5 to 5 seconds. In the invention, the diameter of the graphite column is preferably 46-50 mm, and more preferably 48 mm; the height of the graphite column is preferably 38-42 mm, and more preferably 40 mm. The device for the first pressing is not particularly limited, and a press conventional in the art may be used, and a four-column press is specifically selected in the embodiment of the present invention.
After the graphite column is obtained, the self-sharpening diamond is obtained by sequentially carrying out nitriding treatment and pressing synthesis on the graphite column. Before the nitriding treatment is carried out, the container for nitriding treatment is preferably vacuumized to remove air in the container, and then nitrogen is filled for nitriding treatment. In the invention, the pressure of the nitriding treatment is preferably 0.5-0.7 MPa, and more preferably 0.6 MPa; the time is preferably 23-25 h, and more preferably 24 h.
According to the invention, the nitrided graphite columns are preferably assembled before the press synthesis. In the present invention, the assembling preferably comprises the steps of:
putting the graphite column into a steel cup, and putting the steel cup with the graphite column into a ceramic insulating cup;
arranging a heating belt on the surface of the ceramic insulating cup, and then filling the heating belt into a pyrophyllite block to obtain a primary synthetic block;
and (3) additionally arranging heating sheets and steel caps at two ends of the primary synthetic block to obtain the synthetic block.
The invention is to put the graphite column into the steel cup, and put the steel cup with the graphite column into the ceramic insulation cup. The size of the steel cup is not specially limited, as long as the graphite column can be filled. In the invention, the thickness of the steel cup is preferably 0.28-0.32 mm, and more preferably 0.3 mm. The size of the ceramic insulating cup is not particularly limited, and the ceramic insulating cup can be filled into a steel cup. In the invention, the thickness of the ceramic insulating cup is preferably 1.1-1.2 mm.
The surface of the ceramic insulating cup is provided with a heating belt and then is filled into a pyrophyllite block to obtain a primary synthetic block. In the invention, the heating belt is preferably an iron-chromium-aluminum heating belt, and the thickness of the heating belt is preferably 0.18-0.22 mm, and more preferably 0.2 mm. In the present invention, in the case of the present invention,
after the primary synthetic block is obtained, heating sheets and steel caps are additionally arranged at two ends of the primary synthetic block to obtain the synthetic block. In the present invention, the heat patch is preferably 1.9 or 2.0 mm. The invention has no special limitation on the mode of adding the heating sheet and the steel cap, and can be realized by adopting the conventional mode in the field.
After the synthetic block is obtained, the synthetic block is preferably baked at the baking temperature of preferably 120-140 ℃, more preferably 125-130 ℃; the time is preferably 7.5 to 8.5 hours, and more preferably 8 hours. In the present invention, the baking can remove moisture from the pyrophyllite block and graphite columns in the composite block while increasing the temperature of the composite block.
In the invention, the assembly can provide a high-temperature and high-pressure reaction environment for the graphite column, and the pressure can reach 5GPa in the pressing process in the assembled closed environment; the leaf wax plays roles in heat preservation, pressure transmission, insulation and sealing; the steel cap plays a role in pressure transmission and electric conduction.
In the invention, the pressing synthesis is preferably carried out in a press, and the upper cylinder diameter of the press is preferably 680-720 mm, and more preferably 700 mm. In the invention, the pressure of the pressing synthesis is preferably 4.5-5 GPa, and more preferably 4.8-4.9 GPa; the temperature is preferably 1350-1400 ℃, and more preferably 1380-1390 ℃; the time is preferably 34 to 38min, and more preferably 35 to 36 min.
In the present invention, the temperature of the press synthesis is preferably achieved by heating with a heating belt.
In the present invention, the post-press synthesis product is preferably post-treated after the completion of the press synthesis, and in the present invention, the post-treatment preferably comprises the steps of:
and taking out the product after the pressing synthesis from the synthesis block, and sequentially crushing, soaking and collecting to obtain the self-sharpening diamond.
In the invention, the particle size of the crushed particles is preferably 0.8-1.2 cm, and more preferably 0.9-1 cm. The present invention does not require any special way of breaking as is conventional in the art.
In the present invention, the solvent for immersion is a mixture of sulfuric acid and nitric acid, the sulfuric acid is preferably sulfuric acid having a mass concentration of 98%, and the nitric acid is preferably nitric acid having a mass concentration of 50%. In the invention, the volume ratio of the sulfuric acid to the nitric acid is preferably 4-6: 5, more preferably 5 to 5.5: 5. in the present invention, the soaking preferably further includes washing, and the solvent for washing is preferably water. In the invention, the soaking can separate impurities such as graphite from self-sharpening diamond particles, and the impurities such as graphite, sulfuric acid and nitric acid can be removed by cleaning with water, thus being beneficial to obtaining high-purity self-sharpening diamond.
In the invention, the collection is preferably diamond washing, and specifically, the washed product is put into a tool similar to a dustpan and shaken in water, and the sediment in the tool is taken out. In the present invention, the collection process resembles the gold washing process.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
30Kg of cobalt powder with the particle size of 48 microns, 10Kg of nickel powder with the particle size of 48 microns, 2Kg of cerium powder with the particle size of 48 microns, 1Kg of boron powder with the particle size of 48 microns and 55Kg of graphite powder with the particle size of 48 microns and the purity of 99.999 percent (graphitizing for 26 days at 2900 ℃) are mixed for 24 hours in a three-dimensional mixer to obtain a mixture;
performing isostatic pressing on the mixture for 15min at 190MPa to obtain a cylinder with the diameter of 200mm and the height of 500 mm; crushing the cylinder into particles with the particle size of about 3 mm; pressing 200g of crushed particles on a four-column press (60MPa,5s) to obtain a graphite column with the diameter of 48mm and the height of 40 mm;
putting the graphite column into a nitriding container, vacuumizing, filling nitrogen, and nitriding for 24 hours under the pressure of 0.6 MPa; filling the nitrided graphite column into a steel cup with the thickness of 0.3mm, and filling the steel cup with the nitrided graphite column into a ceramic insulating cup with the thickness of 1.1 mm; arranging an iron-chromium-aluminum heating belt with the thickness of 0.2mm on the surface of the ceramic insulating cup, then loading the heating belt into the pyrophyllite block, and additionally installing heating sheets and steel caps at two ends of the pyrophyllite block to obtain a synthetic block.
Baking the synthetic block at 130 ℃ for 8h, pressing and synthesizing the block in a press (the upper cylinder diameter is 700mm) (the pressure is 5GPa, the temperature is 1350 ℃) for 36min, taking out the product after pressing and synthesizing from the synthetic block, and sequentially crushing (the particle size is 3mm after crushing), soaking (the soaking solution is a mixture of sulfuric acid and nitric acid with the volume ratio of 5: 5), washing and collecting (manually washing diamond) to obtain the self-sharpening diamond.
And preparing the obtained self-sharpening diamond into the self-sharpening diamond resin grinding wheel according to a conventional preparation method.
Example 2
Mixing 28Kg of cobalt powder with the particle size of 48 microns, 9Kg of nickel powder with the particle size of 48 microns, 1.9Kg of cerium powder with the particle size of 48 microns, 0.9Kg of boron powder with the particle size of 48 microns and 57Kg of graphite powder with the particle size of 48 microns and the purity of 99.999 percent (graphitizing for 28 days at 2900 ℃) in a three-dimensional mixer for 24 hours to obtain a mixture;
carrying out isostatic pressing on the mixture for 15 minutes at 190MPa to obtain a cylinder with the diameter of 200mm and the height of 500 mm; crushing the cylinder into particles with the particle size of about 3 mm; pressing 200g of crushed particles on a four-column press (60MPa,5s) to obtain a graphite column with the diameter of 48mm and the height of 40 mm;
putting the graphite column into a nitriding container, vacuumizing, filling nitrogen, and nitriding for 24 hours under the pressure of 0.6 MPa; filling the nitrided graphite column into a steel cup with the thickness of 0.3mm, and filling the steel cup with the nitrided graphite column into a ceramic insulating cup with the thickness of 1.2 mm; arranging an iron-chromium-aluminum heating belt with the thickness of 0.2mm on the surface of the ceramic insulating cup, then loading the heating belt into the pyrophyllite block, and additionally installing heating sheets and steel caps at two ends of the pyrophyllite block to obtain a synthetic block.
Baking the synthetic block at 130 ℃ for 8h, pressing and synthesizing the block in a press (the upper cylinder diameter is 700mm) (the pressure is 5GPa, the temperature is 1400 ℃) for 36min, taking out the product after pressing and synthesizing from the synthetic block, and sequentially crushing (the particle size is 3mm after crushing), soaking (the soaking solution is a mixture of sulfuric acid and nitric acid with the volume ratio of 5: 5), washing and collecting (manually washing diamond) to obtain the self-sharpening diamond.
Comparative example 1
A No. 1 single crystal resin grinding wheel (cerium is not contained in the raw materials for preparation) purchased from a domestic model SM3001 was used as a comparison.
Comparative example 2
A No. 2 single crystal resin grinding wheel from imported American company model No. GB3001 was used for comparison.
The grinding performance of the self-sharpening diamond resin grinding wheel prepared in example 1 and the single crystal resin grinding wheels of comparative examples 1 and 2 was measured, and the results are shown in table 1.
TABLE 1 Properties of resin grinding wheels in example 1, comparative examples 1 and 2
As can be seen from the data in table 1, the resin grinding wheel produced using the self-sharpening diamond provided by the present invention consumed less of the available portion to perform more grinding, indicating that the self-sharpening diamond provided by the present invention has a higher utilization and grinding rate.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. A self-sharpening diamond is prepared by nitriding a graphite column; the pressure of the nitriding treatment is 0.5-0.7 MPa, and the time is 23-25 h; the graphite column comprises the following components in percentage by mass:
2. a method of making a self-sharpening diamond as recited in claim 1, comprising the steps of:
mixing cobalt, nickel, cerium, boron and graphite according to the raw material ratio, and then pressing and forming to obtain a graphite column;
and nitriding and pressing the graphite column in sequence to synthesize the self-sharpening diamond.
3. The method according to claim 2, wherein the cobalt, nickel, cerium, boron and graphite are in a powdery form, and the particle diameters of the cobalt, nickel, cerium, boron and graphite are independently 48 μm or less.
4. The preparation method according to claim 2, wherein the graphite is graphite subjected to graphitization treatment, and the graphitization treatment temperature is 2800-3000 ℃ for 25-30 days.
5. The preparation method according to claim 2, wherein the nitriding treatment is carried out under a pressure of 0.5 to 0.7MPa for 23 to 25 hours.
6. The preparation method according to claim 2, wherein the press synthesis is carried out in a press, the pressure of the press synthesis is 4.8-5 GPa, the temperature is 1350-1400 ℃, and the time is 34-38 min.
7. The production method according to claim 2, wherein the press-molding includes the steps of:
carrying out isostatic pressing treatment on the mixed material obtained by mixing to obtain a high-density forming body;
and crushing the high-density forming body, and pressing into a graphite column.
8. The preparation method according to claim 7, wherein the isostatic pressing treatment is carried out at a pressure of 180 to 190MPa for 10 to 15 min; the pressure of the first pressing is 60-65 MPa, and the time is 4-6 s.
9. The method of claim 2, wherein the nitrided graphite columns are assembled prior to the press synthesis, the assembly including the steps of:
putting the graphite column into a steel cup, and putting the steel cup with the graphite column into a ceramic insulating cup;
arranging a heating belt on the surface of the ceramic insulating cup, and then filling the heating belt into a pyrophyllite block to obtain a primary synthetic block;
and (3) additionally arranging heating sheets and steel caps at two ends of the primary synthetic block to obtain the synthetic block.
10. The preparation method of claim 9, wherein before the synthetic block is pressed and synthesized, the synthetic block is baked at 120-140 ℃ for 7.5-8.5 hours.
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