CN102658061A - Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device - Google Patents
Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device Download PDFInfo
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- CN102658061A CN102658061A CN2012101151993A CN201210115199A CN102658061A CN 102658061 A CN102658061 A CN 102658061A CN 2012101151993 A CN2012101151993 A CN 2012101151993A CN 201210115199 A CN201210115199 A CN 201210115199A CN 102658061 A CN102658061 A CN 102658061A
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 132
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 132
- 239000010432 diamond Substances 0.000 title claims abstract description 49
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 48
- 238000001308 synthesis method Methods 0.000 title claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 66
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 64
- 238000003825 pressing Methods 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 238000004891 communication Methods 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 10
- 239000002131 composite material Substances 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a pressure-equalizing type diamond synthesis device and a diamond synthesis method based on the device. The pressure-equalizing type diamond synthesis device comprises a cubic apparatus, wherein the concave arc-shaped top pressing surface of each top hammer forms a spherical top pressing cavity; a pair of opposite top hammers is provided with a conductive electrode respectively; and the conductive electrode is isolated from the corresponding top hammer. The pressure-equalizing type diamond synthesis device further comprises a spherical raw material synthesis block made of graphite and a catalyst, wherein a spherical pyrophyllite synthesis bowl matched with the spherical top pressing cavity is arranged on the raw material synthesis block; a conductive communicating device corresponding to the conductive electrode and the raw material synthesis block are arranged on the pyrophyllite synthesis bowl; the raw material synthesis block and the pyrophyllite synthesis bowl are spherical and matched with each other; the top pressing surface of the top hammer has a concave arc shape matched with the top hammer; the top hammers apply pressure to the raw material synthesis block from six directions; the pressure in the spherical top pressing cavity is uniform; any angle of the raw material synthesis block is extruded uniformly; when the raw material synthesis block are electrified and heated, the raw material synthesis block has high resistance value and is heated quickly and uniformly; and the synthesis efficiency of the diamond is improved.
Description
Technical Field
The invention relates to a diamond synthesis device and a diamond synthesis method based on the synthesis device.
Background
Diamond is the most robust carbon structure, in which carbon atoms are arranged in a crystal structure, each carbon atom is tightly bonded with the other four carbon atoms, and diamond atoms are in a three-dimensional regular tetrahedron structure, are in a pyramid structure, form a spatial network structure, and finally form a solid with high hardness and poor activity; carbon atoms in graphite are bonded together in a planar layered structure, and the bonding between layers is weak, so that the layers are easily slid to be separated. Under the high-temperature and high-pressure state, covalent bonds can be formed among carbon atoms in different layers of the graphite, when the duration time of the high-temperature and high-pressure state reaches a certain time limit, a large number of carbon atoms in different layers of the graphite form covalent bonds with each other, the layered structure of the graphite is gradually converted into a net structure, and the graphite is converted into diamond. Therefore, under the action of the catalyst, the graphite can be used to synthesize the diamond under the high-temperature and high-pressure state.
At present, there are two main devices for synthesizing diamond single crystals: the first is the two-side roof in foreign countries; second, the domestic six-face top. The principle is to convert graphite catalyst into diamond at high temperature and high pressure.
At present, square pyrophyllite blocks (with the functions of heat preservation, pressure transmission, heat insulation and insulation), conductive steel rings (commonly called as 'plugs') and synthetic columns (catalyst columns for generating diamond) are adopted. After being assembled, the components are heated and then placed in a six-sided jack for synthesis. Since the entire assembly is square or planar circular, this structure affects the temperature and pressure equalization inside the chamber, and thus some characteristics of the produced diamond, such as grain size, morphology, hardness, etc., are not uniform. Similarly, because the traditional press anvil is square, and the cavity of the pyrophyllite assembly block is internally provided with a cylinder, the transmission of internal pressure and the trend of current are unbalanced, so that the temperature and the pressure of a synthesis column in the pyrophyllite assembly block are also unbalanced, and the synthesis efficiency of diamonds is influenced.
Disclosure of Invention
The invention aims to solve the first technical problem of providing a pressure-equalizing type diamond synthesis device which can ensure that a raw material synthesis block is uniformly pressed and heated, thereby improving the diamond synthesis efficiency.
In order to solve the technical problems, the technical scheme of the invention is as follows: the pressure-equalizing type diamond synthesis device comprises a six-sided jack, wherein a top hammer of the six-sided jack is provided with an inwards-concave arc-shaped top pressing surface, the inwards-concave arc-shaped top pressing surface forms a spherical top pressing cavity, a pair of opposite top hammers are respectively provided with a conductive electrode, and the conductive electrodes are insulated from the corresponding top hammers;
the graphite electrode is characterized by further comprising a spherical raw material synthesis block made of graphite and a catalyst, wherein a spherical pyrophyllite synthesis pot matched with the spherical jacking cavity is installed on the raw material synthesis block, and a conductive communication device corresponding to the conductive electrode and the raw material synthesis block is installed on the pyrophyllite synthesis pot.
As a preferred technical scheme, the six concave arc-shaped pressing surfaces have the same shape.
As a preferable technical solution, the conductive communication means includes a conductive cap corresponding to the conductive electrode and the raw material synthesis block, and the conductive cap is insulated from all of the hammers.
As a preferred technical scheme, the spherical pyrophyllite synthesis pot comprises two hemispherical pyrophyllite synthesis pots which are matched with each other.
By adopting the technical scheme, the voltage-sharing type diamond synthesis device comprises a six-face top, wherein the anvil of the six-face top is provided with an inwards concave arc-shaped top pressing surface which forms a spherical top pressing cavity, a pair of opposite anvil is respectively provided with a conductive electrode, and the conductive electrodes are insulated from the corresponding anvil; the device also comprises a spherical raw material synthesis block made of graphite and a catalyst, wherein a spherical pyrophyllite synthesis pot matched with the spherical jacking cavity is arranged on the raw material synthesis block, and a conductive communication device corresponding to the conductive electrode and the raw material synthesis block is arranged on the pyrophyllite synthesis pot; the raw material synthetic block and the pyrophyllite synthetic pot are mutually matched spheres, the top pressing surface of the top hammer is a concave arc matched with the top pressing surface, the top hammer presses the raw material synthetic block from six directions, the pressure in the spherical top pressing cavity is uniform, and the raw material synthetic block can be uniformly extruded at any angle; meanwhile, the raw material synthesis block is electrified and heated, and the temperature rise is rapid and uniform due to the high resistance of the raw material synthesis block; the synthesis efficiency of the diamond is improved.
The invention aims to solve the second technical problem of providing a diamond synthesis method based on a pressure equalizing type diamond synthesis device.
In order to solve the technical problems, the technical scheme of the invention is as follows: a diamond synthesis method based on a pressure-equalizing type diamond synthesis device comprises the following steps:
uniformly mixing graphite powder and a catalyst to prepare spherical raw material synthetic blocks;
manufacturing a spherical pyrophyllite synthesis pot, wherein the spherical pyrophyllite synthesis pot is provided with a cavity for accommodating the spherical raw material synthesis block, and mounting the raw material synthesis block into the spherical pyrophyllite synthesis pot; the pyrophyllite synthesis pot is provided with a conductive communicating device corresponding to the conductive electrode and the raw material synthesis block;
thirdly, placing the assembly of the pyrophyllite synthesis pot and the raw material synthesis block on a workbench with a six-surface top, wherein the anvil with the six-surface top is provided with an inwards concave arc-shaped top pressing surface which is formed into a spherical top pressing cavity, the assembly of the pyrophyllite synthesis pot and the raw material synthesis block is positioned in the spherical top pressing cavity, a pair of opposite anvils are respectively provided with a conductive electrode, and the conductive electrodes are insulated from the corresponding anvils; enabling the conductive communicating device on the pyrophyllite synthesis pot to correspond to the conductive electrode;
and fourthly, starting the six-side jack, extruding the pyrophyllite synthesis pot by the jack hammer, increasing the pressure in the pyrophyllite synthesis pot, when the pressure is increased to 2.1-5.8 Gpa, simultaneously switching on a conductive electrode and a power supply, electrifying and heating the raw material synthesis block, increasing the temperature to 1100-1500 ℃, keeping the temperature for 2-5 minutes, slowly cooling to below 80 ℃, slowly relieving the pressure to normal pressure, removing the pyrophyllite synthesis pot, and finally taking out the sintered body containing the diamond.
As a preferred technical scheme, the spherical pyrophyllite synthesis pot comprises two hemispherical pyrophyllite synthesis pots which are matched with each other.
As a preferable technical solution, the conductive communication means includes a conductive cap corresponding to the conductive electrode and the raw material synthesis block, and the conductive cap is insulated from all of the hammers.
As a preferred technical scheme, the six concave arc-shaped pressing surfaces have the same shape.
The pressure equalizing type diamond synthesis device can ensure that the raw material synthesis block is uniformly pressed and heated, namely, the pressure conduction is balanced and the current trend is balanced; the temperature in the cavity surrounded by the pyrophyllite synthesis pot is balanced, the efficiency of synthesizing the diamond can be improved, and the synthesized diamond has higher grade and more complete shape.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein,
FIG. 1 is a schematic view illustrating a pressing state according to an embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating a state to be pressed according to an embodiment of the present invention;
FIG. 3 is a schematic diagram showing an assembled state of a spherical pyrophyllite synthesis pot and a raw material synthesis block according to an embodiment of the present invention;
FIG. 4 is a schematic view showing a state in which a spherical pyrophyllite synthesis pot and a raw material synthesis block are disassembled according to an embodiment of the present invention;
in the figure: 1-top hammer; 11-an inner concave arc-shaped jacking surface; 2-a spherical jacking cavity; 3-a conductive electrode; 4-raw material synthesis block; 5-pyrophyllite synthesis pot; 61-a conductive cap; 62-an insulating layer; 63-electrode insertion hole.
Detailed Description
Exemplary embodiments according to the present invention are described in detail below with reference to the accompanying drawings. Here, it is to be noted that, in the drawings, the same reference numerals are given to the constituent elements having substantially the same structure and function, and redundant description about the substantially same constituent elements is omitted in order to make the description more concise.
As shown in fig. 1 and 2, the pressure equalizing type diamond synthesizer comprises a six-sided anvil including six anvils 1, only four anvils 1 sections in the upper, lower, left and right are shown in fig. 1 and 2, and two anvils 1 in the vertical section direction are not shown in the drawing; the anvil 1 with the six-sided anvil is provided with inner concave arc-shaped anvil surfaces 11, the six inner concave arc-shaped anvil surfaces 11 are the same in shape, the inner concave arc-shaped anvil surfaces 11 form a spherical anvil cavity 2, a pair of opposite anvil is respectively provided with a conductive electrode 3, and the conductive electrodes 3 are insulated from the corresponding anvil 1;
as shown in fig. 3 and 4, the graphite/catalyst composite block further comprises a spherical raw material composite block 4 made of graphite and a catalyst, wherein a spherical pyrophyllite composite bowl 5 matched with the spherical top pressing cavity 2 is mounted on the raw material composite block 4, and the spherical pyrophyllite composite bowl 5 comprises two hemispherical pyrophyllite composite bowls 5 matched with each other; install on the synthetic alms bowl 5 of hemisphere pyrophyllite of the synthetic alms bowl 5 of pyrophyllite with conductive electrode 3 with the conductive intercommunication device that the synthetic piece 4 of raw materials corresponds, conductive intercommunication device include with conductive electrode 3 with the conductive cap 61 that the synthetic piece 4 of raw materials corresponds, conductive cap 61 with all it is insulating between the top hammer 1, conductive cap 61 is adjacent towards be equipped with insulating layer 62 on the terminal surface of top hammer 1, be equipped with on the insulating layer 62 with the electrode jack 63 that conductive electrode 3 corresponds, conductive electrode 3's tip inserts electrode jack 63 with conductive cap 61 contacts. That is, the conductive electrodes 3 located in the two opposing hammers 1 are communicated with the raw material synthesizing block 4 through the corresponding conductive caps 61.
The raw material synthesis block 4 is prepared by mixing graphite powder and catalyst powder, and the catalyst can be Co, Ni and other materials.
The raw material synthesis block 4 is spherical, the top pressing surface of the top hammer 1 is concave arc matched with the top pressing surface, after six-sided jacking is started, the top hammer 1 presses the raw material synthesis block 4 from six directions, the pressure in the spherical top pressing cavity 2 is uniform, the pressure in the synthesis cavity enclosed by the pyrophyllite synthesis pot 5 is also uniform, and any angle of the raw material synthesis block 4 can be uniformly extruded; the conductive electrodes 3 on the two opposite top hammers 1 are connected into a circuit, current passes through one conductive electrode 3, a conductive cap 61 corresponding to the electrode, the raw material synthesis block 4, the other conductive cap and the other conductive electrode 3 to electrify and heat the raw material synthesis block 4, and the resistance of the raw material synthesis block 4 is high, so that much heat is generated, and the temperature rise is rapid and uniform; the uniformly balanced pressure and uniformly balanced temperature improve the synthesis efficiency of the diamond.
A diamond synthesis method based on a pressure-equalizing type diamond synthesis device comprises the following steps:
uniformly mixing graphite powder and a catalyst to prepare a spherical raw material synthetic block 4;
manufacturing a spherical pyrophyllite synthesis pot 2, wherein the spherical pyrophyllite synthesis pot 2 comprises two hemispherical pyrophyllite synthesis pots 2 which are matched with each other; the spherical pyrophyllite synthesis pot 2 is provided with a cavity for accommodating the spherical raw material synthesis block 4, and the raw material synthesis block 4 is installed in the spherical pyrophyllite synthesis pot 2; the pyrophyllite synthesis pot 2 is provided with a conductive communication device corresponding to the conductive electrode 3 and the raw material synthesis block 4, the conductive communication device comprises a conductive cap 61 corresponding to the conductive electrode 3 and the raw material synthesis block 4, and the conductive cap 61 is insulated from all the top hammers 1;
thirdly, placing the assembly of the pyrophyllite synthesis pot 2 and the raw material synthesis block 4 on a six-cubic-top workbench, wherein the top hammer 1 of the six cubic top is provided with concave arc-shaped top pressing surfaces 11, and the six concave arc-shaped top pressing surfaces 11 are identical in shape; the concave arc-shaped jacking surface 11 forms a spherical jacking cavity 2, an assembly of the pyrophyllite synthesis bowl 2 and the raw material synthesis block 4 is positioned in the spherical jacking cavity 2, a pair of opposite jacking hammers 1 are respectively provided with a conductive electrode 3, and the conductive electrodes 3 are insulated from the corresponding jacking hammers 1; the conductive cap 61 on the pyrophyllite synthesis pot 2 corresponds to the conductive electrode 3;
the six-side top is started, the top hammer 1 extrudes the pyrophyllite synthesis pot 2, the pressure in the pyrophyllite synthesis pot 2 rises, when the pressure rises to 2.1-5.8 Gpa, the conductive electrode 3 is connected with a power supply, the raw material synthesis block 4 is electrified and heated, the temperature rises to 1100-1500 ℃, the temperature is kept for 2-5 minutes, the temperature is slowly cooled to be below 80 ℃, then the pressure is slowly relieved to the normal pressure, the pyrophyllite synthesis pot 2 is removed, and finally the sintered body containing the diamond is taken out.
The pressure equalizing type diamond synthesis device can ensure that the raw material synthesis block 4 is uniformly pressed and heated, namely, the pressure conduction is balanced, and the current trend is balanced; the temperature in the cavity surrounded by the pyrophyllite synthesis bowl 5 is balanced, the efficiency of synthesizing the diamond can be improved, and the synthesized diamond has higher grade and more complete shape.
As described above, the embodiments of the present invention have been specifically described above, but the present invention is not limited thereto. It should be understood by those skilled in the art that various modifications, combinations, sub-combinations, or substitutions may be made in accordance with design requirements or other factors while remaining within the scope of the appended claims and their equivalents.
Claims (8)
1. Pressure-equalizing type diamond synthesizer, its characterized in that: the conductive electrode is insulated from the corresponding anvil;
the graphite electrode is characterized by further comprising a spherical raw material synthesis block made of graphite and a catalyst, wherein a spherical pyrophyllite synthesis pot matched with the spherical jacking cavity is installed on the raw material synthesis block, and a conductive communication device corresponding to the conductive electrode and the raw material synthesis block is installed on the pyrophyllite synthesis pot.
2. The apparatus of claim 1 wherein: the six concave arc-shaped jacking surface shapes are the same.
3. The apparatus of claim 1 wherein: the conductive communication device comprises a conductive cap corresponding to the conductive electrode and the raw material synthesis block, and the conductive cap is insulated from all the top hammers.
4. A pressure grading diamond synthesis apparatus according to claim 1, 2 or 3, in which: the spherical pyrophyllite synthesizing pot comprises two hemispherical pyrophyllite synthesizing pots which are matched with each other.
5. A diamond synthesis method based on a pressure-equalizing type diamond synthesis device is characterized by comprising the following steps:
uniformly mixing graphite powder and a catalyst to prepare spherical raw material synthetic blocks;
manufacturing a spherical pyrophyllite synthesis pot, wherein the spherical pyrophyllite synthesis pot is provided with a cavity for accommodating the spherical raw material synthesis block, and mounting the raw material synthesis block into the spherical pyrophyllite synthesis pot; the pyrophyllite synthesis pot is provided with a conductive communicating device corresponding to the conductive electrode and the raw material synthesis block;
thirdly, placing the assembly of the pyrophyllite synthesis pot and the raw material synthesis block on a workbench with a six-surface top, wherein the anvil with the six-surface top is provided with an inwards concave arc-shaped top pressing surface which is formed into a spherical top pressing cavity, the assembly of the pyrophyllite synthesis pot and the raw material synthesis block is positioned in the spherical top pressing cavity, a pair of opposite anvils are respectively provided with a conductive electrode, and the conductive electrodes are insulated from the corresponding anvils; enabling the conductive communicating device on the pyrophyllite synthesis pot to correspond to the conductive electrode;
and fourthly, starting the six-side jack, extruding the pyrophyllite synthesis pot by the jack hammer, increasing the pressure in the pyrophyllite synthesis pot, when the pressure is increased to 2.1-5.8 Gpa, simultaneously switching on a conductive electrode and a power supply, electrifying and heating the raw material synthesis block, increasing the temperature to 1100-1500 ℃, keeping the temperature for 2-5 minutes, slowly cooling to below 80 ℃, slowly relieving the pressure to normal pressure, removing the pyrophyllite synthesis pot, and finally taking out the sintered body containing the diamond.
6. The diamond synthesis method according to claim 5, wherein: the spherical pyrophyllite synthesizing pot comprises two hemispherical pyrophyllite synthesizing pots which are matched with each other.
7. The diamond synthesis method according to claim 5, wherein: the conductive communication device comprises a conductive cap corresponding to the conductive electrode and the raw material synthesis block, and the conductive cap is insulated from all the top hammers.
8. A method of diamond synthesis as claimed in claim 5, 6 or 7 wherein: the six concave arc-shaped jacking surface shapes are the same.
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| CN201210115199.3A CN102658061B (en) | 2012-04-19 | 2012-04-19 | Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device |
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| CN201210115199.3A CN102658061B (en) | 2012-04-19 | 2012-04-19 | Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device |
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Cited By (5)
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| CN103521134A (en) * | 2013-10-29 | 2014-01-22 | 河南晶锐超硬材料有限公司 | Assembly for super-hard material synthesis |
| CN106422983A (en) * | 2016-11-10 | 2017-02-22 | 郑州磨料磨具磨削研究所有限公司 | Ultrahigh-pressure pressurizing and heating device |
| CN111167377A (en) * | 2020-01-14 | 2020-05-19 | 燕山大学 | Arc top hammer type four-side top ultrahigh-pressure device |
| CN113290926A (en) * | 2021-04-26 | 2021-08-24 | 杭州超然金刚石有限公司 | Preparation device and preparation process of diamond semiconductor |
| CN117138692A (en) * | 2023-10-21 | 2023-12-01 | 河南恒达超硬材料有限公司 | Diamond press with preheating structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117138692B (en) * | 2023-10-21 | 2024-06-07 | 河南恒达超硬材料有限公司 | Diamond press with preheating structure |
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| CN102658061B (en) | 2014-06-25 |
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