CN111659318B - Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method - Google Patents
Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method Download PDFInfo
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- CN111659318B CN111659318B CN202010541379.2A CN202010541379A CN111659318B CN 111659318 B CN111659318 B CN 111659318B CN 202010541379 A CN202010541379 A CN 202010541379A CN 111659318 B CN111659318 B CN 111659318B
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- heating
- heat preservation
- pipe
- diamond
- modification
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- 239000010432 diamond Substances 0.000 title claims abstract description 39
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 38
- 238000012986 modification Methods 0.000 title claims abstract description 20
- 230000004048 modification Effects 0.000 title claims abstract description 20
- 238000002715 modification method Methods 0.000 title claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 74
- 238000004321 preservation Methods 0.000 claims abstract description 49
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 4
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000009434 installation Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 17
- 239000000919 ceramic Substances 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000010459 dolomite Substances 0.000 description 5
- 229910000514 dolomite Inorganic materials 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000001668 ameliorated effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 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
- B01J3/065—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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application discloses an assembly block for high-temperature and high-pressure modification of CVD cultivated diamond and a modification method, and mainly relates to the technical field of superhard material synthesis. Including being located outer pyrophyllite piece, be equipped with the installation cavity that runs through it in the pyrophyllite piece, the both ends in installation cavity all set up rather than the conductive cap that the cross-section corresponds, be equipped with on the inboard terminal surface of conductive cap rather than the heating piece that contacts, two be equipped with the heating pipe between the heating piece, the axial vertical heating piece of heating pipe, just the annular terminal surface in both ends of heating pipe contacts with the heating piece of homonymy respectively, the outside of heating pipe has cup jointed first heat preservation pipe, be equipped with two heat preservation posts in the heating pipe, two be used for placing the diamond between the heat preservation post. The application has the beneficial effects that: can conduct ultrahigh pressure and generate heat to modify CVD cultivated diamond, improve the crystallization quality and improve the color and the purity grade.
Description
Technical Field
The application relates to the technical field of superhard material synthesis, in particular to an assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and a modification method.
Background
Laboratory grown diamond, which is created and manufactured by artificial means simulating the crystallization characteristics of natural diamond, is truly diamond in every respect: chemical, physical, atomic and light, all of which are identical to natural diamond. The CVD method is a main method for producing large-particle diamond, in the metastable zone of diamond, using low-temperature high-pressure condition, about 900 deg.c, heating the gas containing C-methane (CH 4) and hydrogen gas in vacuum reaction chamber with microwave to generate plasma, decomposing C from the gas compound state into individual free atomic state, and through diffusion and convection, finally the diamond structure is deposited on the substrate or seed crystal to grow continuously. Although this method is easy to grow a carat grade of precious stone grade diamond, the grown cultivated diamond has poor color and clarity.
CVD diamond is prone to many crystal defects such as vacancies and non-diamond crystal structure defects due to the limitations of the growth method, and the grown diamond is difficult to reach D, E, F grade color and VVS and above purity standards, and the above problems need to be ameliorated by subsequent modification treatments.
Disclosure of Invention
The application aims to provide an assembly block for high-temperature and high-pressure modification of CVD (chemical vapor deposition) cultivated diamond and a modification method, which can conduct ultrahigh pressure and generate heat to modify the CVD cultivated diamond, improve the crystallization quality and improve the color and the purity grade of the CVD cultivated diamond.
The application aims to achieve the aim, and the aim is achieved by the following technical scheme:
the utility model provides a CVD cultivates diamond high temperature high pressure and modifies and use assembled piece, includes and is located outer pyrophyllite piece, be equipped with the installation cavity that runs through it in the pyrophyllite piece, the both ends in installation cavity all set up rather than the conductive cap that the cross-section corresponds, be equipped with on the inboard terminal surface of conductive cap rather than the heating piece that contacts, two be equipped with the heating pipe between the heating piece, the axial vertical heating piece of heating pipe, just the annular terminal surface in both ends of heating pipe contacts with the heating piece of homonymy respectively, the outside of heating pipe has cup jointed first heat preservation pipe, be equipped with two heat preservation post in the heating pipe, two be used for placing the diamond between the heat preservation post.
The second heat preservation pipe is embedded on the inner wall of the installation cavity, and the heating plate is arranged in the second heat preservation pipe.
The installation cavity is circular, the conductive cap, the heating plate, the first heat preservation tube, the heating tube and the heating column are all circular pieces, and the outer diameters of the conductive cap, the heating plate and the first heat preservation tube are matched with the inner diameter of the installation cavity.
The length of the first heat preservation pipe is the same as that of the heating pipe, and the height of the heat preservation column is half of that of the heating pipe.
The conductive cap comprises a metal bowl and a filling core, wherein the metal bowl is made of a high-temperature-resistant metal material, the filling core is made of a high-temperature-resistant ceramic material, and the filling core is arranged on the inner side end face of the conductive cap.
The metal bowl is made of any one of low carbon steel, molybdenum and titanium;
and/or
The filling core is made of any one of dolomite, zirconia ceramic, magnesia ceramic and alumina ceramic.
The heating plate and/or the heating pipe is made of any one of artificial carbon, graphite plates and molybdenum.
The first heat preservation tube is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics;
and/or
The second heat preservation pipe is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics;
and/or
The heat-insulating column is made of any one of dolomite or zirconia ceramic, magnesia ceramic and alumina ceramic.
The pyrophyllite block comprises two symmetrical stone monomers which are arranged up and down, the two stone monomers are spliced up and down to form the pyrophyllite block, and the conductive cap is combined with the outer end opening of the stone monomers.
As another aspect of the present application, a high temperature and high pressure modification method for CVD grown diamond, using the above-described assembly block, placing CVD grown diamond between two heat-insulating columns, pressing six faces of the assembly block by a high temperature and high pressure pressing press top hammer during modification, generating pressure required for modification, and generating temperature required for modification by energizing a heating sheet and a heating pipe.
Compared with the prior art, the application has the beneficial effects that:
the application can carry out modification treatment on the CVD diamond, and the assembly block is put into a high-temperature high-pressure pressing machine, and the ultra-high pressure of 8GPa and the high temperature of more than 2000 ℃ can be realized in the block at the highest, so that the treatment on the modification of the CVD diamond is realized, and the color and the transparency of the diamond are obviously improved. And repairing structural defects such as vacancies, non-diamond crystals and the like, and reaching D, E, F-grade color and VVS and higher purity standards.
Drawings
Fig. 1 is a schematic view of the assembly of the present application in a disassembled state.
Fig. 2 is a combined schematic of the present application.
Fig. 3 is a schematic view of the internal structure of the present application.
FIG. 4 is a diagram of the present application.
FIG. 5 is a diagram showing the components of the present application.
FIG. 6 shows a CVD diamond grown prior to modification using the present application.
FIG. 7 is a graph of CVD grown diamond modified by the technique of the present application.
The reference numbers shown in the drawings:
1. pyrophyllite block; 2. a conductive cap; 3. a heating sheet; 4. heating pipes; 5. a first heat-preserving tube; 6. a second insulating tube; 7. a heat preservation column; 8. a mounting cavity; 9. filling the core; 10. a metal bowl.
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Further, it will be understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the application, and equivalents thereof fall within the scope of the application as defined by the claims.
The instruments, reagents, materials, etc. used in the examples described below are conventional instruments, reagents, materials, etc. known in the art, and are commercially available. The experimental methods, detection methods, and the like in the examples described below are conventional experimental methods, detection methods, and the like that are known in the prior art unless otherwise specified.
Example 1: assembled block for high-temperature and high-pressure modification of diamond cultivated by CVD
Comprises a pyrophyllite block 1, a conductive cap 2, a heating plate 3, a heating pipe 4, a first heat preservation pipe 5, a second heat preservation pipe 6 and a heat preservation column 7.
The pyrophyllite block 1 is positioned at the outermost periphery and is used as a pressure transmission and sealing medium, so that the pressure on the top hammer of the high-temperature high-pressure pressing machine can be transmitted into the assembly block, and meanwhile, a certain sealing effect is achieved, the pressure in the assembly block can be sealed, and the high-temperature high-pressure modification safety is ensured. The pyrophyllite block 1 is provided with a cylindrical mounting cavity 8 which is centered and penetrates up and down. The other components comprise a conductive cap 2 x 2, a heating plate 3 x 2, a heating pipe 4 x 1, a first heat-preserving pipe 5 x 1, a second heat-preserving pipe 6 x 1 and a heat-preserving column 7 x 2; wherein the second heat preservation pipe 6 is nested and fixed on the inner wall of the installation cavity 8.
The conductive cap 2 is composed of a metal bowl 10 and a filling core 9 in the bowl, wherein the metal bowl 10 is made of low carbon steel, and has the functions of conducting electricity and transmitting pressure, and the filling core 9 in the bowl is made of dolomite, and has the functions of heat preservation and transmitting pressure. The metal bowl 10 is cylindrical, the outer diameter of the metal bowl corresponds to the inner diameter of the installation cavity 8, the metal bowl can be inserted into the installation cavity 8, and when the metal bowl is specifically assembled, the metal bowl is positioned at two ends of the installation cavity 8, and the filling cores 9 are assembled oppositely. The inner side end surface of the conductive cap 2 is positioned in the second heat preservation pipe 6.
The heating plates 3 are round metal plates and are manufactured by molybdenum, the outer diameter of the heating plates corresponds to the outer diameter of the conductive cap 2, and the two heating plates 3 are symmetrically assembled in the mounting cavity 8 and positioned on the inner side of the conductive cap 2 to be in contact with the conductive cap 2. The conductive cap 2 plays a role of energizing and heating.
The first heat preservation pipe 5 is arranged between the two heating plates 3, and annular end surfaces on two sides of the first heat preservation pipe are respectively contacted with opposite side surfaces of the two heating plates 3. The external diameter of the first heat preservation tube 5 is matched with the internal diameter of the installation cavity 8, a heating tube 4 is sleeved in the first heat preservation tube 5, the heating tube 4 is also manufactured by molybdenum processing, and the external diameter corresponds to the internal diameter of the first heat preservation tube 5, so that the effect of electrifying and heating is achieved.
Two heat preservation posts 7 are assembled in the heating pipe 4, the heat preservation posts 7 are cylindrical pieces, and the height of the heat preservation posts is half of that of the heating pipe 4.
The first heat preservation pipe 5, the second heat preservation pipe 6 and the heat preservation column 7 are made of zirconia ceramics, and play a role in heat preservation and pressure transmission.
The modification method using the above-mentioned combined block is as follows:
1) And (3) assembling: the pyrophyllite block is prepared, the conductive cap 2 and the heating plates 3 are symmetrically assembled at two ends, a first heat preservation pipe 5 and a heating pipe 4 are assembled between the two heating plates 3 from outside to inside, two heat preservation columns 7 are assembled in the heating pipe 4, and diamond to be modified is placed between the heat preservation columns 7.
2) The assembled block with diamond is installed on a high-temperature high-pressure synthesis press, six faces of the assembled block are extruded by a top hammer to generate pressure of 8-9 GPa required by modification, and the heating plate 3 and the heating pipe 4 are electrified to generate temperature of 1800-2200 ℃ required by modification.
Example 2: assembled block for high-temperature and high-pressure modification of diamond cultivated by CVD
Most of the structure of the assembled block is the same as in example 1, with the two examples differing in the specific structure of the pyrophyllite block 1, as well as the materials used for the individual components.
1) The structure of pyrophyllite block 1: in this example, the pyrophyllite block adopts a structure divided into an upper block monomer and a lower block monomer, and the structure is convenient to assemble.
2) Conductive cap 2, heating plate 3, heating pipe 4, first heat preservation pipe 5, second heat preservation pipe 6, the material of using of heat preservation post 7:
the metal bowl 10 of the conductive cap 2 uses titanium; the filling core 9 of the conductive cap 2 is made of alumina ceramic material;
the heating plate 3 and the heating pipe 4 use artificial carbon;
the first heat preservation pipe 5, the second heat preservation pipe 6 and the heat preservation column 7 use magnesia ceramics.
The above components were not different from those of example 1 in terms of the materials used.
Claims (1)
1. The high-temperature high-pressure modification method for cultivating the diamond by CVD is characterized by comprising an assembly block, wherein the assembly block comprises a pyrophyllite block positioned on the outer layer, a mounting cavity penetrating the pyrophyllite block is arranged in the pyrophyllite block, conductive caps corresponding to the sections of the pyrophyllite block are arranged at two ends of the mounting cavity, heating plates contacted with the conductive caps are arranged on the inner side end surfaces of the conductive caps, heating pipes are arranged between the two heating plates, the axial vertical heating plates of the heating pipes are arranged, annular end surfaces at two ends of the heating pipes are respectively contacted with the heating plates at the same side, a first heat preservation pipe is sleeved outside the heating pipes, two heat preservation columns are arranged in the heating pipes, diamonds are placed between the two heat preservation columns, the heat preservation columns are cylindrical pieces, the height of each heat preservation column is half of that of the heating pipe, the inner side end surfaces of the conductive caps are positioned in a second heat preservation pipe, and the inner side end surfaces of the conductive caps correspond to the annular end surfaces of the first heat preservation pipe; the conductive cap comprises a metal bowl and a filling core, wherein the metal bowl is made of a high-temperature-resistant metal material, the filling core is made of a high-temperature-resistant ceramic material, and the filling core is arranged on the inner side end face of the conductive cap; the diameter of the filling core is larger than that of the heating pipe;
the method for modifying the assembly blocks comprises the following steps:
1) And (3) assembling: preparing pyrophyllite blocks, symmetrically assembling the conductive caps and the heating plates according to two ends, assembling a first heat-insulating pipe and a heating pipe between the two heating plates from outside to inside, assembling two heat-insulating columns in the heating pipe, and placing diamond to be modified between the heat-insulating columns;
2) The assembled block with diamond is installed on a high-temperature high-pressure press, six faces of the assembled block are extruded by a top hammer to generate pressure of 8-9 GPa required by modification, and a heating plate and a heating pipe are electrified to generate temperature of 1800-2200 ℃ required by modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010541379.2A CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010541379.2A CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111659318A CN111659318A (en) | 2020-09-15 |
| CN111659318B true CN111659318B (en) | 2023-10-27 |
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|---|---|---|---|
| CN202010541379.2A Active CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Country Status (1)
| Country | Link |
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| CN111659318A (en) | 2020-09-15 |
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Denomination of invention: An assembly block and modification method for CVD cultivation of diamond high-temperature and high-pressure modification Granted publication date: 20231027 Pledgee: China Construction Bank Liaocheng Shizhong Sub branch Pledgor: SHANDONG LIAOCHENG JUNRUI SUPERHARD MATERIAL Co.,Ltd. Registration number: Y2024980005671 |