CN107626262B - Synthesis process of high-holding-force diamond - Google Patents
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- 239000010432 diamond Substances 0.000 title claims abstract description 66
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 26
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000010419 fine particle Substances 0.000 claims abstract description 11
- 230000003068 static effect Effects 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000012938 design process Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000009461 vacuum packaging Methods 0.000 claims description 8
- 238000009489 vacuum treatment Methods 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims 5
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
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Abstract
The invention discloses a synthesis process of a high-holding-force diamond, which comprises the following steps: preparing 100 meshes of fine powder catalyst and 300 meshes of fine spherical graphite powder; mixing spherical graphite powder and a powder catalyst, carrying out static pressure, and crushing into fine particles to obtain a particle mixture; adding the particle mixture into a mold to obtain a core column; placing the obtained core column in a vacuum furnace for high-temperature deoxidization, cooling, then placing the core column into a synthesis block, and heating and pressurizing the synthesis block to synthesize the diamond with high holding power; according to the preparation process of the diamond with high holding power, the quality of the diamond in the early stage of synthesis can be ensured, the diamond with rough surface and scratches can be synthesized, the holding power of the diamond is improved, the cutting efficiency of a diamond die is increased, and the service life of the diamond die is prolonged; the diamond obtained by the preparation process has rough surface, the processed diamond mould has large binding force with the matrix, the diamond can not fall off too early, and the cutting efficiency and the service life of the diamond mould are improved.
Description
Technical Field
The invention relates to the technical field, in particular to a synthesis process of a diamond with high holding force.
Background
Diamond is widely applied to the fields of drilling, stone processing, mechanical processing, electronic industry, aerospace industry and the like due to excellent mechanical, physical and chemical properties, is an indispensable engineering material in modern industry, and is particularly used as a super abrasive to be introduced into grinding industry, so that the processing efficiency and the processing quality of parts are obviously improved, the service life of a grinding wheel is prolonged, and the dimensional stability of the processed parts is improved. Generally, the more regular the crystal form of diamond and the fewer surface defects, the higher the crystal quality, but the higher the wear resistance, the smoother the surface, less rough and the weaker the mechanical bond with the binder. During grinding, premature removal of the entire diamond particle often occurs. According to statistics, the diamond abrasive particles 2/3 in the common diamond grinding wheel fall off prematurely before the grinding effect is not fully exerted, and the service life is greatly shortened. The traditional abrasive diamond and a matrix are often low in bonding strength and poor in holding force, the diamond is prone to falling off prematurely in the using process, and the using efficiency of the diamond is seriously affected.
At present, no effective solution has been found to solve the above problems. At present, the surface coating method is mainly adopted to change the surface state of the abrasive, although the problem of low holding force can be partially solved. However, this method is expensive and technically difficult.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a synthesis process of a high-holding-force diamond.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a synthesis process of a high-holding-force diamond comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: adding the mixture into a three-dimensional mixer in a ratio of 3-6, mixing for 3-5 hours, and crushing into fine particles within 80 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80-3.00g/cm3；
Placing the core column obtained in the step III in a vacuum furnace, performing vacuum treatment for 8-10 hours at 1000-1050 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, discharging, performing vacuum packaging, then placing into a synthetic block, heating, performing pressure synthesis by using a cubic press, and heating for 1440-1800 seconds at high temperature of 1200-1300 ℃ and high pressure of 5.5-6.0 GPa by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at a speed of more than 1MPa, starting heating, stopping pressurizing, keeping for 250-300 seconds, continuing pressurizing, pressurizing to 78-80 MPa within 20 seconds, stopping pressurizing, keeping for 320-350 seconds, increasing the pressure to 87-92 MPa within 10 seconds, keeping for 900-960 seconds, and then reducing the pressure at a constant speed within 180-600 seconds until pressure relief is completed;
the power of the cubic press is set as follows: the initial power is 7000-7900W, the power is maintained for 380-410 seconds, then the power is reduced to 6000-6500W within 15 seconds, the power is maintained for 850-900 seconds, and then the power is reduced at a constant speed within 120-540 seconds until the heating is finished.
Preferably, in the step (II), the weight ratio of the spherical graphite powder to the powder catalyst is 7: 5.
preferably, in the second step, the uniformly mixed spherical graphite powder and the powder catalyst are subjected to static pressure and then crushed into fine particles of 40-50 meshes.
Preferably, the density of the core column is 2.80-2.85g/cm3。
Preferably, the pressure of the cubic press is set to: pressurizing a cubic press from 0 to 50MPa at the speed of 2MPa, stopping pressurizing, keeping for 280 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 90MPa within 10 seconds, keeping for 950 seconds, and then uniformly reducing the pressure within 480 seconds until pressure relief is finished.
Preferably, the power of the cubic press is set as follows: the power was initially 7500W, held for 400 seconds, then adjusted down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 420 seconds.
A further preferred synthesis process comprises the steps of:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 5, adding the mixture into a three-dimensional mixer in proportion, mixing for 3-5 hours, and crushing into fine particles within 50 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80g/cm3；
Putting the core column obtained in the step (III) into a vacuum furnace, carrying out vacuum treatment for 9 hours at 1040 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, then putting into a synthetic block, heating the synthetic block, carrying out pressurization synthesis by using a cubic press, and heating for 1700 seconds at 1250 ℃ and 5.8GPa under high pressure by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at the speed of 2MPa, starting heating, stopping pressurizing, keeping for 280 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 90MPa within 10 seconds, keeping for 950 seconds, and then reducing the pressure at a constant speed within 480 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the power was initially 7500W, held for 400 seconds, then adjusted down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 420 seconds.
Compared with the prior art, the invention has the following advantages:
the invention relates to a preparation process of a high-holding-force diamond, which comprises the following steps: the primary power reduction power curve and the secondary overpressure pressure curve can stabilize the early-stage temperature and pressure of the diamond in a stable diamond growth area and ensure the quality of the diamond in the early stage of synthesis, and the last step of constant-speed pressure relief and constant-speed power reduction in the synthesis step not only ensures the stable growth area in the later stage of the synthesis of the diamond and ensures the quality of the diamond, but also can synthesize the diamond with rough surface and scratches, improve the holding force of the diamond, and increase the cutting efficiency and the service life of a diamond die; the diamond obtained by the preparation process has rough surface, the processed diamond mould has large binding force with the matrix, the diamond can not fall off too early, and the cutting efficiency and the service life of the diamond mould are improved.
The preparation process is adjusted on the basis of the traditional process, has the advantages of stable process, high conversion rate, regular crystal form, high impact index and rough surface, can meet the requirements of high control and wear resistance of diamond on the market, and greatly improves the use efficiency of tools. The diamond obtained by the preparation process is a product which is in short supply in markets at home and abroad, can obtain good economic benefit for enterprises, and compared with the traditional process, the process can control the synthesis of the diamond with high holding power, and is an innovation for the synthetic process of the artificial diamond.
Drawings
FIG. 1 is a diagram of a diamond with high holding force;
fig. 2 is an enlarged view of a single diamond with high holding force.
Detailed Description
The four-column press is also called a four-column oil press.
The invention is further described with reference to specific examples.
Example 1
A synthesis process of a high-holding-force diamond comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 3, adding the mixture into a three-dimensional mixer for mixing for 3 hours, and crushing the mixture into fine particles within 80 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80g/cm3；
Putting the core column obtained in the step (III) into a vacuum furnace, carrying out vacuum treatment for 8 hours at 1000 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, vacuum-packaging after discharging, then putting into a synthetic block, heating the synthetic block, carrying out pressurization synthesis by using a cubic press, and heating for 1440 seconds at high temperature of 1200 ℃ and high pressure of 5.5GPa by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at a speed of more than 1MPa, starting heating, stopping pressurizing, keeping for 250 seconds, continuing pressurizing, pressurizing to 78MPa within 20 seconds, stopping pressurizing, keeping for 320 seconds, increasing the pressure to 87MPa within 10 seconds, keeping for 900 seconds, and then reducing the pressure at a constant speed within 180 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the power was initially 7000W for 380 seconds, then the power was ramped down to 6000W for 15 seconds, 850 seconds, and then ramped down to the end of heating for 120 seconds.
Example 2
A synthesis process of a high-holding-force diamond comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 6, adding the mixture into a three-dimensional mixer for mixing for 5 hours, and crushing the mixture into fine particles within 80 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 3.00g/cm3；
Fourthly, placing the core column obtained in the third step into a vacuum furnace, carrying out vacuum treatment for 10 hours at 1050 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, then placing into a synthetic block, heating the synthetic block, carrying out pressurization synthesis by using a cubic press, and heating for 1800 seconds at 1300 ℃ of high temperature and 6.0GPa of high pressure by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at a speed of more than 1MPa, starting heating, stopping pressurizing, keeping for 300 seconds, continuing pressurizing, pressurizing to 80MPa within 20 seconds, stopping pressurizing, keeping for 350 seconds, increasing the pressure to 92MPa within 10 seconds, keeping for 960 seconds, and then reducing the pressure at a constant speed within 600 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the starting power was 7900W, held for 410 seconds, then the power was ramped down to 6500W for 15 seconds, held for 900 seconds, and then ramped down to the end of heating for 540 seconds.
Example 3
A synthesis process of a high-holding-force diamond comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 4, adding the mixture into a three-dimensional mixer in proportion, mixing for 3-5 hours, and crushing into fine particles within 80 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.85g/cm3；
Putting the core column obtained in the step (III) into a vacuum furnace, carrying out vacuum treatment for 9 hours at 1020 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, then putting into a synthetic block, heating the synthetic block, carrying out pressure synthesis on the synthetic block by using a cubic press, and heating for 1600 seconds at 1250 ℃ and 5.8GPa under high pressure by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at a speed of more than 1MPa, starting heating, stopping pressurizing, keeping for 270 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 88MPa within 10 seconds, keeping for 920 seconds, and then reducing the pressure at a constant speed within 300 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the power was initially 7400W and held for 400 seconds, then the power was ramped down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 340 seconds.
Example 4
A synthesis process of a high-holding-force diamond comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 5, adding the mixture into a three-dimensional mixer in proportion, mixing for 3-5 hours, and crushing into fine particles within 50 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80g/cm3；
Putting the core column obtained in the step (III) into a vacuum furnace, carrying out vacuum treatment for 9 hours at 1040 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, then putting into a synthetic block, heating the synthetic block, carrying out pressurization synthesis by using a cubic press, and heating for 1700 seconds at 1250 ℃ and 5.8GPa under high pressure by matching with a design process to obtain the diamond with high holding power; the picture of the diamond with high holding power is shown in figure 1, the enlarged view of a single diamond is shown in figure 2, and it can be seen from figures 1 and 2 that the diamond particles obtained by the method are complete, high in crystallinity, uniform in particle size, rough in surface and high in holding power.
The pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at the speed of 2MPa, starting heating, stopping pressurizing, keeping for 280 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 90MPa within 10 seconds, keeping for 950 seconds, and then reducing the pressure at a constant speed within 480 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the power was initially 7500W, held for 400 seconds, then adjusted down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 420 seconds.
The high-holding-force diamonds obtained in the embodiments 1 to 4 have high content, a yield per unit of 280t or more and the properties shown in Table 1;
Claims (6)
1. a synthetic process of a high-holding-force diamond is characterized by comprising the following steps: the method comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: adding the mixture into a three-dimensional mixer in a ratio of 3-6, mixing for 3-5 hours, and crushing into fine particles within 80 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80-3.00g/cm3；
Placing the core column obtained in the step III in a vacuum furnace, carrying out vacuum treatment for 8-10 hours at 1000-1050 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, loading into a synthetic block, heating, carrying out pressurization synthesis by using a cubic press, and heating for 1440-1800 seconds at high temperature of 1200-1300 ℃ and high pressure of 5.5-6.0 GPa by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at the speed of 2MPa, starting heating, stopping pressurizing, keeping for 280 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 90MPa within 10 seconds, keeping for 950 seconds, and then reducing the pressure at a constant speed within 480 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the initial power is 7000-7900W, the power is maintained for 380-410 seconds, then the power is reduced to 6000-6500W within 15 seconds, the power is maintained for 850-900 seconds, and then the power is reduced at a constant speed within 120-540 seconds until the heating is finished.
2. The process for synthesizing a high holding force diamond according to claim 1, wherein: in the second step, the weight ratio of the spherical graphite powder to the powder catalyst is 7: 5.
3. the process for synthesizing a high holding force diamond according to claim 1, wherein: and step two, uniformly mixing the spherical graphite powder and the powder catalyst, and crushing the mixture into fine particles of 40-50 meshes after static pressure.
4. The process for synthesizing a high holding force diamond according to claim 1, wherein: the density of the core column is 2.80-2.85g/cm3。
5. The process for synthesizing a high holding force diamond according to claim 1, wherein: the power of the cubic press is set as follows: the power was initially 7500W, held for 400 seconds, then adjusted down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 420 seconds.
6. The process for synthesizing a high holding force diamond according to claim 1, wherein: the method comprises the following steps:
preparing 100-mesh fine powder catalyst and 300-mesh fine spherical graphite powder, wherein the powder catalyst is an iron-based alloy, and the impurity content of the spherical graphite powder is below 30 ppm;
secondly, mixing the spherical graphite powder and the powder catalyst according to a weight ratio of 7: 5, adding the mixture into a three-dimensional mixer in proportion, mixing for 3-5 hours, and crushing into fine particles within 50 meshes after static pressure to obtain a particle mixture;
thirdly, adding the particle mixture obtained in the second step into a mould, and pressing by a four-column press to obtain a core column, wherein the size of the core column is phi 56mm multiplied by 46.5mm, and the density of the core column is 2.80g/cm3；
Putting the core column obtained in the step (III) into a vacuum furnace, carrying out vacuum treatment for 9 hours at 1040 ℃, fully removing oxygen by using a hydrogen reduction method, naturally cooling to room temperature under the protection of nitrogen, carrying out vacuum packaging after discharging, then putting into a synthetic block, heating the synthetic block, carrying out pressurization synthesis by using a cubic press, and heating for 1700 seconds at 1250 ℃ and 5.8GPa under high pressure by matching with a design process to obtain the diamond with high holding power;
the pressure of the cubic press is set as follows: pressurizing a cubic press from 0 to 50MPa at the speed of 2MPa, starting heating, stopping pressurizing, keeping for 280 seconds, continuing pressurizing, pressurizing to 79MPa within 20 seconds, stopping pressurizing, keeping for 340 seconds, increasing the pressure to 90MPa within 10 seconds, keeping for 950 seconds, and then reducing the pressure at a constant speed within 480 seconds until pressure relief is finished;
the power of the cubic press is set as follows: the power was initially 7500W, held for 400 seconds, then adjusted down to 6200W for 15 seconds, held for 880 seconds, and then ramped down to the end of heating for 420 seconds.
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| CN108579615B (en) * | 2018-05-17 | 2020-11-03 | 长沙石立超硬材料有限公司 | Synthesis process for improving yield per unit of single crystal diamond by prokaryotic implantation method |
| CN109078581B (en) * | 2018-08-29 | 2020-07-07 | 中南钻石有限公司 | Catalyst alloy powder, surface groove-shaped diamond prepared from catalyst alloy powder, preparation method and application |
| CN115382465A (en) * | 2022-09-23 | 2022-11-25 | 中南钻石有限公司 | Surface frosted diamond and synthesis process thereof |
| CN117123143B (en) * | 2023-07-14 | 2024-02-23 | 山东中科润晶新材料有限公司 | Method for synthesizing special-shaped dodecahedron diamond |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5190734A (en) * | 1991-02-22 | 1993-03-02 | Frushour Robert H | Modified end assembly for high pressure, high temperature reaction vessels |
| CN102935346A (en) * | 2012-11-23 | 2013-02-20 | 山东昌润钻石股份有限公司 | Micron-level fine particle diamond synthesis process |
| CN103566830A (en) * | 2013-03-11 | 2014-02-12 | 河南省力量新材料有限公司 | Synthesis method of octahedron diamond |
| CN103846058A (en) * | 2012-11-28 | 2014-06-11 | 周存文 | Synthesis process of ultrafine-grade diamond |
| CN103949187A (en) * | 2014-05-14 | 2014-07-30 | 河南飞孟金刚石工业有限公司 | Coarse particle polycrystalline diamond synthesizing technology |
| CN104907003A (en) * | 2015-06-24 | 2015-09-16 | 河南黄河旋风股份有限公司 | Manufacturing method ofdiamond with rough surface |
| CN106824002A (en) * | 2015-12-03 | 2017-06-13 | 郑州华晶金刚石股份有限公司 | A kind of synthesis technique of gem grade diamond |
-
2017
- 2017-11-14 CN CN201711122291.1A patent/CN107626262B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5190734A (en) * | 1991-02-22 | 1993-03-02 | Frushour Robert H | Modified end assembly for high pressure, high temperature reaction vessels |
| CN102935346A (en) * | 2012-11-23 | 2013-02-20 | 山东昌润钻石股份有限公司 | Micron-level fine particle diamond synthesis process |
| CN103846058A (en) * | 2012-11-28 | 2014-06-11 | 周存文 | Synthesis process of ultrafine-grade diamond |
| CN103566830A (en) * | 2013-03-11 | 2014-02-12 | 河南省力量新材料有限公司 | Synthesis method of octahedron diamond |
| CN103949187A (en) * | 2014-05-14 | 2014-07-30 | 河南飞孟金刚石工业有限公司 | Coarse particle polycrystalline diamond synthesizing technology |
| CN104907003A (en) * | 2015-06-24 | 2015-09-16 | 河南黄河旋风股份有限公司 | Manufacturing method ofdiamond with rough surface |
| CN106824002A (en) * | 2015-12-03 | 2017-06-13 | 郑州华晶金刚石股份有限公司 | A kind of synthesis technique of gem grade diamond |
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| CN107626262A (en) | 2018-01-26 |
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