CN115041099B - Diamond synthetic block and preparation method of diamond - Google Patents
Diamond synthetic block and preparation method of diamond Download PDFInfo
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- CN115041099B CN115041099B CN202210848422.9A CN202210848422A CN115041099B CN 115041099 B CN115041099 B CN 115041099B CN 202210848422 A CN202210848422 A CN 202210848422A CN 115041099 B CN115041099 B CN 115041099B
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- 239000010432 diamond Substances 0.000 title claims abstract description 147
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 141
- 238000002360 preparation method Methods 0.000 title abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 107
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 59
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 58
- 239000003054 catalyst Substances 0.000 claims abstract description 45
- 239000013078 crystal Substances 0.000 claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003086 colorant Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 92
- 229910002804 graphite Inorganic materials 0.000 claims description 65
- 239000010439 graphite Substances 0.000 claims description 65
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 54
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 48
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 47
- 229910000831 Steel Inorganic materials 0.000 claims description 28
- 239000010959 steel Substances 0.000 claims description 28
- 239000011780 sodium chloride Substances 0.000 claims description 27
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 18
- 239000000395 magnesium oxide Substances 0.000 claims description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 15
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 12
- 229910052749 magnesium Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000000903 blocking effect Effects 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005087 graphitization Methods 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- QCWXUUIWCKQGHC-BJUDXGSMSA-N zirconium-90 Chemical group [90Zr] QCWXUUIWCKQGHC-BJUDXGSMSA-N 0.000 claims description 2
- 239000010459 dolomite Substances 0.000 description 25
- 229910000514 dolomite Inorganic materials 0.000 description 25
- 238000001035 drying Methods 0.000 description 21
- 239000000203 mixture Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000008451 emotion Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 208000001840 Dandruff Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000012364 cultivation method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension 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
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
-
- 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
- B01J2203/0675—Structural or physico-chemical features of the materials processed
- B01J2203/068—Crystal growth
Abstract
The invention relates to the technical field of diamond synthesis, in particular to a diamond synthesis block and a preparation method of diamond. The diamond synthesis block comprises a diamond synthesis cavity; the diamond synthesis cavity comprises an upper cover, a female cavity and a lower cover; the upper cover and the lower cover are arranged on two sides of the female cavity; the upper cover is provided with a plurality of cavities, and a first heat conduction column is arranged in the cavity of the upper cover; the lower cover is provided with a plurality of cavities, and a second heat conduction column is arranged in the cavity of the lower cover; a plurality of subchambers are arranged in the main chamber; an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are sequentially connected are arranged in the subchamber. The diamond synthetic block can cultivate diamond with different colors and sizes at one time.
Description
Technical Field
The invention relates to the technical field of diamond synthesis, in particular to a diamond synthesis block and a preparation method of diamond.
Background
In recent years, the development of the diamond market is gradually changing the consumption habit of people, with the improvement of the living standard of substances, the consumption of people on spirit and emotion is gradually increasing, the diamond has been symbolized by love and forever for centuries due to the firm characteristic of the diamond, but the diamond can be cultivated, namely, the range of the expressed emotion can be further expanded, besides symbolizing love, the diamond can symbolize friends, relatives, teachers and students, war friends and the like, the carbon element can be extracted from human tissues such as hair, nails, teeth, body hair, fallen skin, dandruff and the like, and biological diamond can be manufactured in a specially manufactured cavity by using a high-temperature and high-pressure method by using the extracted carbon element, and the diamond jointly contains the carbon element extracted from a biological sample, so that the firmness of two or more people on the friendship is symbolized.
The existing growth cavities for cultivating the diamond synthetic blocks are all of a single-cavity structure, and the single-cavity structure can only grow 1-30 diamonds with the same color and similar size at a time. With the increasing demand for personalized customization, diamond cultivation methods for cultivating single colors and sizes at a time are no longer practical, and the single-cavity structure can lead to increased costs for manufacturers and reduced customer selectivity. For the case of customizing one diamond separately but with different color requirements, a single cavity structure is used to cultivate the diamond, which would be uneconomical and not cost effective to perform 5 syntheses based on the prior art in order to meet customer requirements. Under the condition that the colors of the diamonds are the same but the required Clar quality is different, a single cavity structure is adopted to cultivate the diamonds, the cultivation process is required to be completed according to the largest time in the synthesis, the longer the diamond grows, the diamond cultivated in the synthesis is approximately the same size, the diamond is cut into the target size according to the requirement, and the larger the diamond polishing cost is also larger, so that the cost for preparing the diamond is increased.
In view of this, the present invention has been made.
Disclosure of Invention
The first object of the present invention is to provide a diamond synthesis block, which solves the problem in the prior art that diamond with different colors and different sizes cannot be cultivated at one time, thereby effectively improving the utilization rate of a synthesis cavity and reducing the production cost of diamond.
A second object of the present invention is to provide a method for producing diamond, which synthesizes the diamond synthesis block described above under a certain condition, thereby producing different kinds of high quality diamond at one time.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the invention provides a diamond synthesis block, which comprises a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover, a female cavity and a lower cover;
the upper cover and the lower cover are arranged on two sides of the female cavity;
the upper cover is provided with a plurality of cavities, and a first heat conduction column is arranged in the cavity of the upper cover;
the lower cover is provided with a plurality of cavities, and a second heat conduction column is arranged in the cavity of the lower cover;
a plurality of subchambers are arranged in the main chamber;
an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are sequentially connected are arranged in the subchamber.
The invention also provides a preparation method of the diamond, which comprises the following steps:
and synthesizing the dried diamond synthesized block for 5-10 days under the condition of 5.5-6 GPa and 5-7 kw of power, and taking out after synthesis.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the diamond synthesis block, the whole large main cavity comprises the plurality of small subchambers, raw materials for growing diamond with different colors can be added into each subchamber according to requirements, and the raw materials among the cavities cannot interfere with each other, so that diamond with different colors can be grown; in addition, the first heat conduction column and the second heat conduction column with different heat conductivities are placed above and below each subchamber, so that the temperature difference above and below each subchamber can be effectively controlled in a section, the purpose of controlling the growth speed of diamond is achieved, the sizes of the diamond obtained by different growth speeds in the subchambers are different, and the diamond with different sizes can be grown.
(2) According to the preparation method of the diamond, the diamond synthesis blocks with the multi-cavity structure are adopted for synthesis, the growth conditions in each subchamber can be independently controlled, reasonable partition cultivation can be carried out in the one-time synthesis process according to production requirements and requirements on the diamond, and the diamond of different types can be grown in different areas, so that different requirements on the diamond can be met, and the production cost is greatly reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural view of a diamond synthesis chamber according to the present invention.
Fig. 2 is a schematic structural view of a diamond-synthesized block according to the present invention.
Reference numerals:
1-an upper cover; 11-a first heat conducting column; 2-a mother cavity;
21-subchambers; 211-upper insulation plug; 212-carbon source;
213-catalyst; 214-copper sheet; 215-crystal bed
216-seed crystal; 3-a lower cover; 31-a second heat conducting post;
41-a first heating plate; 42-a second heating plate; 5-pyrophyllite block;
51-lining; 52-heating the pipe; 61-a first plugging ring;
62-a second plugging ring; 71-a first pyrophyllite ring; 711-a first conductive steel cap;
72-a second pyrophyllite ring; 721-second conductive steel cap.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and detailed description, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative of the present invention only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The following describes a diamond synthesis block and a method for producing diamond according to an embodiment of the present invention.
Referring to body 1, in some embodiments of the invention there is provided a diamond synthesis block comprising a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover 1, a female cavity 2 and a lower cover 3;
the upper cover 1 and the lower cover 3 are arranged on two sides of the female cavity 2;
the upper cover 1 is provided with a plurality of cavities, and a first heat conduction column 11 is arranged in the cavity of the upper cover 1;
the lower cover 3 is provided with a plurality of cavities, and a second heat conduction column 31 is arranged in the cavity of the lower cover 3;
a plurality of subchambers 21 are arranged in the main chamber 2;
an upper insulating plug 211, a carbon source 212, a catalyst 213, a copper sheet 214 and a crystal bed 216 which are sequentially connected are arranged in the subchamber 21.
The diamond synthesis block provided by the invention comprises a plurality of subchambers 21, different types of catalysts 213 can be placed in the cavity of each subchamber 21, and heat conduction columns with the same or different heat conductivities can be placed in each cavity of the lower cover 3 and the upper cover 1, so that the growth conditions of each subchamber 21 can be independently controlled, and interference is not generated; by controlling the catalyst 213 and the temperature gradient in each sub-chamber 21 individually, diamond of different colors and different sizes can be produced in one synthesis of the diamond synthesis block.
The conventional diamond single crystal growth chamber has a structure in which only one catalyst 213 is placed and which corresponds to only one temperature gradient, so that it is suitable for growing diamond of one color and similar size; in the diamond synthesis block of the present invention, the growth cavity is divided into a plurality of subchambers 21, firstly, different catalysts 213, carbon sources 212 and crystal beds 215 for growing diamond of different colors are placed in each subchamber 21, and secondly, the same or different heat conduction columns are placed in the reserved cavities of the upper cover 1 and the lower cover 3 at both sides of each subchamber 21, so that different kinds of diamond are manufactured in one synthesis process.
Referring to fig. 2, in some embodiments of the present invention, the diamond synthesis block further includes a first conductive steel cap 711, a second conductive steel cap 721, a first heating sheet 41, a second heating sheet 42, and a heating pipe 52;
the first heating sheet 41 and the second heating sheet 42 are disposed at both sides of the heating pipe 52; the first heating plate 41, the second heating plate 42 and the heating pipe 52 are enclosed to form a containing cavity, and the diamond synthesis cavity is placed in the containing cavity;
the first conductive steel cap 711 is connected to the first heating plate 41;
the first heating plate 41 is connected with the upper cover 1;
the second conductive steel cap 721 is connected to the second heating plate 42;
the second heating plate 42 is connected to the lower cover 3.
In some embodiments of the present invention, the diamond-synthesized block further comprises a first pyrophyllite ring 71, a second pyrophyllite ring 72, a first plugging ring 61, a second plugging ring 62, an inner liner 51, and a pyrophyllite block 5;
the first heating plate 41 is connected with the first plugging ring 61; the first plugging ring 61 is connected with a first pyrophyllite ring 71; the first conductive steel cap 711 is arranged in the accommodating cavity formed by the first plugging ring 61 and the pyrophyllite ring 71;
the second heating plate 42 is connected with a second blocking ring 62; the second plugging ring 62 is connected to a second pyrophyllite ring 72; the second conductive steel cap 721 is disposed in the receiving cavity formed by the second plugging ring 62 and the second pyrophyllite ring 72;
the middle part of the pyrophyllite block 5 is provided with a hollow cavity with a hollow structure;
the side wall of the cavity of the pyrophyllite block 5 is connected with the inner liner 51; the liner 51 is connected to a heating tube 52.
In the diamond composite block of the present invention, the first pyrophyllite ring 71 and the first stopper ring 61 form a cavity penetrating the upper and lower surfaces, and the first conductive steel cap 711 is disposed in the cavity, i.e., the periphery of the first conductive steel cap 711 is filled with the first pyrophyllite ring 71 and the first stopper ring 61. The second pyrophyllite ring 72 and the second plugging ring 62 form a cavity penetrating the upper and lower surfaces, and the second conductive steel cap 721 is disposed in the cavity, i.e. the periphery of the second conductive steel cap 721 is filled with the second pyrophyllite ring 72 and the second plugging ring 62.
In some embodiments of the present invention, the upper cover 1 is connected to the upper insulating block 211.
In some embodiments of the invention, the lower cover 3 is connected to the crystal bed 215.
In some embodiments of the invention, a seed crystal 216 is disposed within the crystal bed 215; the seed crystal is positioned within the beds 215 adjacent to one side of the copper sheet 214, and the seed crystal 216 is placed at the center of the upper end of each of the beds 215.
In some embodiments of the present invention, a copper sheet 214 is coated over the seed 216 to protect the seed 216.
In some embodiments of the invention, seed 216 has a particle size of 0.4 to 0.6mm.
In some embodiments of the present invention, the number of cavities of the upper cover 1 and the number of subcavities 21 are the same as the number of cavities of the lower cover 3; the number of the subchambers 21 is not strictly limited, and can be adjusted according to actual requirements.
In some embodiments of the present invention, the upper cover 1 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia; preferably, the preparation method of the upper cover 1 includes: uniformly mixing sodium chloride and zirconia, drying at 80-120 ℃ for more than or equal to 12 hours, and then compacting; preferably, the pressure of the press forming is 20 to 30 tons. The moisture in the raw material can be removed by drying.
In some embodiments of the invention, the lower cover 3 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia; preferably, the preparation method of the lower cover 3 includes: uniformly mixing sodium chloride and zirconia, drying at 80-120 ℃ for more than or equal to 12 hours, and then compacting; preferably, the pressure of the press forming is 20 to 30 tons.
In some embodiments of the invention, the female cavity 2 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia; preferably, the preparation method of the female cavity 2 comprises the following steps: uniformly mixing sodium chloride and zirconia, drying at 80-120 ℃ for more than or equal to 12 hours, and then compacting; preferably, the pressure of the press forming is 25 to 30 tons.
In some embodiments of the present invention, upper insulator plug 211 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia; preferably, the preparation method of the upper insulating plug 211 comprises the following steps: uniformly mixing sodium chloride and zirconia, drying at 80-120 ℃ for more than or equal to 12 hours, and then compacting; preferably, the pressure of the press forming is 20 to 30 tons.
In some embodiments of the invention, the carbon source 212 comprises graphite powder; preferably, the purity of the graphite powder is more than or equal to 99.99 percent, and the graphitization degree of the graphite powder is more than or equal to 99.8 percent; preferably, the graphite powder has an effective density of 1.99g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the method for preparing the carbon source 212 includes: drying the carbon source 212 at 80-120 ℃ for more than or equal to 12 hours, pressing and forming, and then drying at 80-120 ℃ for more than or equal to 12 hours; preferably, the pressure of the press forming is 20 to 30 tons. Because the purity of the carbon source 212 is required to be high, the preparation process of the carbon source 212 needs to be operated in a special dust-free space to prevent other impurities from being mixed.
In some embodiments of the invention, the crystal bed 215 comprises a magnesium oxide crystal bed; preferably, the preparation method of the crystal bed 215 comprises the following steps: calcining magnesium oxide with purity more than or equal to 99.5 ℃ at 1100-1300 ℃ for 2-5 h, and then compacting and forming; preferably, the pressure of the press forming is 15-25 tons.
In some embodiments of the present invention, a hole is punched in the center of the upper end of each of the pressed beds 215 and a seed crystal 216 is placed.
In some embodiments of the invention, catalyst 213 comprises the following components in parts by weight: 60 to 75 parts of Fe, 25 to 35 parts of Ni, 1 to 5 parts of Al, 1 to 3 parts of Cu and 0.004 to 0.008 part of B; the diamond prepared by the catalyst 212 with the components is blue diamond;
alternatively, the catalyst 213 comprises the following components in parts by weight: 60-75 parts of Fe, 25-35 parts of Ni, 1-5 parts of Al and 1-3 parts of Cu; the diamond prepared by the catalyst 213 with the components is colorless diamond;
alternatively, the catalyst 213 comprises the following components in parts by weight: 60-75 parts of Fe and 25-35 parts of Ni; the diamond produced by the catalyst 213 of the above composition is yellow diamond.
In some embodiments of the invention, the method for preparing catalyst 213 comprises: preparing various alloy components according to the components of the catalyst 213, smelting at 1650-1750 ℃, cooling, cutting and forming.
In the diamond synthesis block of the present invention, catalysts 213 for growing diamond of different colors may be placed in each of the sub-chambers 21 according to the need, and raw materials between each of the sub-chambers 21 may not interfere with each other, thereby growing diamond of different colors.
In some embodiments of the present invention, the first heat conductive post 11 comprises the following components in parts by weight: 5-10 parts of magnesium oxide and/or zirconium oxide and 90-95 parts of sodium chloride; preferably, the first heat conductive pillar 11 is prepared by the following steps: after the raw materials are uniformly mixed, drying is carried out for more than or equal to 12 hours at the temperature of 80-120 ℃, and then compression molding is carried out; preferably, the pressure of the press forming is 10 to 20 tons.
In some embodiments of the present invention, the first heat conductive post 11 comprises the following components in parts by weight: 5-10 parts of magnesium oxide and 90-95 parts of sodium chloride; alternatively, the first heat conductive column 11 includes the following components in parts by weight: 5-10 parts of zirconia and 90-95 parts of sodium chloride.
In some embodiments of the present invention, the second heat conductive post 31 comprises the following components in parts by weight: 80-90 parts of magnesium oxide and 10-20 parts of graphite powder; preferably, the second heat conductive pillar 31 is prepared by the following steps: uniformly mixing magnesium oxide and graphite powder, drying at 80-120 ℃ for more than or equal to 12 hours, and then compacting and forming; preferably, the pressure of the press forming is 10 to 20 tons.
In the diamond synthesis block of the present invention, the first heat conduction column 11 and the second heat conduction column 31 with different heating efficiencies can be placed above and below each subchamber 21, so that the temperature difference above and below each subchamber 21 can be effectively controlled in a section, the purpose of controlling the growth speed of diamond is achieved, and the different growth speeds in each subchamber 21 determine the growth size of diamond in each chamber in one synthesis.
In some embodiments of the present invention, the first heater plate 41 comprises one or more of graphite, silicon carbide, and magnesium.
In some embodiments of the present invention, the first heating sheet 41 is made of graphite; or the first heating plate 41 is made of graphite and silicon carbide, and the mass ratio of the graphite to the silicon carbide is 94-96: 4 to 6; or the first heating plate 41 is made of graphite and magnesium; the mass ratio of graphite to magnesium is 90-95: 5 to 10. Preferably, the first heating sheet 41 is a first graphite heating sheet.
In some embodiments of the present invention, the second heater plate 42 comprises one or more of graphite, silicon carbide, and magnesium.
In some embodiments of the present invention, the material of the second heating sheet 42 is graphite; or the material of the second heating plate 42 is graphite and silicon carbide, and the mass ratio of the graphite to the silicon carbide is 94-96: 4 to 6; or the second heating plate 42 is made of graphite and magnesium; the mass ratio of graphite to magnesium is 90-95: 5 to 10. Preferably, the second heating sheet 42 is a second graphite heating sheet.
In some embodiments of the present invention, the heating tube 52 comprises one or more of graphite, silicon carbide, and magnesium.
In some embodiments of the present invention, the heating tube 52 is made of graphite; or the heating pipe 52 is made of graphite and silicon carbide, and the mass ratio of the graphite to the silicon carbide is 94-96: 4 to 6; or the heating tube 52 is made of graphite and magnesium; the mass ratio of graphite to magnesium is 90-95: 5 to 10. Preferably, the heating tube 52 is a graphite heating tube.
In some embodiments of the invention, the liner 51 comprises a dolomite liner or a composite liner; the composite material lining is made of zirconia; or the composite material lining is made of zirconia and sodium chloride, and the mass ratio of the zirconia to the sodium chloride is 40-80: 20 to 60.
In some embodiments of the present invention, the material of the first plugging ring 61 comprises dolomite or a composite material, the composite material comprising zirconia and sodium chloride; the mass ratio of the zirconia to the sodium chloride is 80-90:: 10 to 20. Preferably, the first plugging ring 61 is a first dolomite ring.
In some embodiments of the present invention, the material of the second plugging ring 62 comprises dolomite or a composite material comprising zirconia and sodium chloride; the mass ratio of the zirconia to the sodium chloride is 80-90:: 10 to 20. Preferably, the second plugging ring 62 is a second dolomite ring.
In some embodiments of the invention, the shape of the upper cover 1, the shape of the female cavity 2 and the shape of the lower cover 3 are the same, the shape of the female cavity 2 comprising a cylindrical shape; preferably, the diameters of the upper cap 1, the female chamber 2 and the lower cap 3 are the same.
In some embodiments of the invention, the shape of the cavity of the upper cover 1, the shape of the subcavities 21 and the shape of the cavity of the lower cover 3 are the same; the shape of the subchamber 21 comprises a cylindrical shape; preferably, the diameters of the cavity of the upper cover 1, the subchamber 21 and the cavity of the lower cover 3 are the same.
In some embodiments of the present invention, the shape of the upper insulating plug 211, the shape of the carbon source 212, the shape of the catalyst 213, and the shape of the crystal bed 215 are the same, and the shape of the carbon source 212 includes a cylindrical shape; preferably, the diameters of the upper insulator plug 211, the carbon source 212, the catalyst 213, and the crystal bed 215 are the same.
In some embodiments of the present invention, the shape of the copper sheet 214 includes a circle; preferably, the diameter of the copper sheet 214 is the same as the diameter of the crystal bed 215.
In some embodiments of the invention, the shape and size of each structure in the composite block of diamond is as follows:
the upper cover 1 is cylindrical in shape; preferably, the diameter of the upper cover 1 is 55-59 mm; the height of the upper cover 1 is 8-12 mm; the cavity of the upper cover 1 is cylindrical, the diameter of the cavity of the upper cover 1 is 4-10 mm, and the height of the cavity of the upper cover 1 is 8-12 mm;
the first heat conductive pillar 11 is cylindrical in shape; preferably, the diameter of the first heat conduction column 11 is 4-10 mm, and the height of the first heat conduction column 11 is 8-10 mm;
the lower cover 3 is cylindrical in shape; preferably, the diameter of the lower cover 3 is 55 to 59mm; the height of the lower cover 3 is 8-12 mm; the cavity of the lower cover 3 is cylindrical, the diameter of the cavity of the lower cover 3 is 4-10 mm, and the height of the cavity of the lower cover 3 is 8-12 mm;
the shape of the second heat conductive pillar 31 includes a cylindrical shape; preferably, the diameter of the second heat conductive pillars 31 is 4 to 10mm, and the height of the second heat conductive pillars 31 is 8 to 10mm;
the shape of the female cavity 2 is cylindrical; preferably, the diameter of the female cavity 2 is 55-59 mm; the height of the female cavity 2 is 24-28 mm; more preferably, the subchamber 21 comprises a cylindrical shape, the subchamber 21 has a diameter of 4 to 10mm, and the subchamber 21 has a height of 24 to 28mm;
the upper insulating plug 211 is cylindrical in shape, preferably, the diameter of the upper insulating plug 211 is 4-10 mm, and the height of the upper insulating plug 211 is 4-6 mm;
the carbon source 212 is cylindrical in shape; preferably, the diameter of the carbon source 212 is 4 to 10mm, and the height of the carbon source 212 is 4 to 8mm;
the catalyst 213 is cylindrical in shape; preferably, the diameter of the catalyst 213 is 4-10 mm, and the height of the catalyst 213 is 8-12 mm;
the shape of the copper sheet 214 is circular; preferably, the diameter of the copper sheet 214 is 4-10 mm, and the thickness of the copper sheet 214 is 0.05-0.1 mm;
the shape of the crystal bed 215 is cylindrical, preferably, the diameter of the crystal bed 215 is 4-10 mm, and the height of the crystal bed 215 is 4-6 mm;
the first heating plate 41 is circular, and the diameter of the first heating plate 41 is 57-61 mm;
the second heating plate 42 is circular, and the diameter of the second heating plate 42 is 57-61 mm;
the wall thickness of the heating pipe 52 is 0.5-1.5 mm; preferably, the outer diameter of the heating tube 52 is 57-61 mm; the height of the heating pipe 52 is 40-52 mm;
the pyrophyllite block 5 is cylindrical in shape; preferably, the inner diameter of the pyrophyllite block 5 is 57-65 mm; the height of the pyrophyllite block 5 is 70-80 mm. The inside diameter of pyrophyllite block 5 is the size after the lining is inlaid.
The shape and the size of each structure of the diamond synthesis block are not strictly limited, and the diamond synthesis block can be adjusted according to actual conditions.
In some embodiments of the invention, the assembly of diamond-synthesized blocks includes: 1. the second heat conduction columns 311 are plugged into the corresponding cavities of the lower cover 3; 2. the mother cavity 2 is arranged on the lower cover 3, and a crystal bed 215, a copper sheet 214, a catalyst 213, a carbon source 212 and an upper insulating plug 211 are respectively arranged in a sub-cavity 21 of the mother cavity 2 from bottom to top; 3. the first heat conduction columns 11 are placed in the corresponding cavities of the upper covers 1, and the corresponding holes are covered above the female cavities 2; 4. placing the assembled assembly into a heating tube 52; 5. the first heating plate 41 and the second heating plate 42 are respectively placed at the upper and lower ends of the heating pipe 52; 6 placing the assembled structure in the liner 51 and then in the pyrophyllite block 5; 7. the first conductive steel cap 711, the second conductive steel cap 722, the first blocking ring 61, the second blocking ring 62, the first pyrophyllite ring 71 and the second pyrophyllite ring 72 are arranged at the upper end and the lower end of the diamond synthetic block, and the diamond synthetic block is completely assembled.
In some embodiments of the present invention, there is also provided a method of preparing diamond, comprising the steps of:
synthesizing the dried diamond synthesized block for 5-10 days under the conditions of pressure of 5.5-6 GPa and power of 5-7 kw, and taking out after synthesis;
preferably, the dried diamond synthesized block is placed in a top press, the pressure is increased from 0GPa to 5.5-6 GPa within 3 hours, the power is increased from 0kw to 5-7 kw, the diamond synthesized block is synthesized for 5-10 days, and the diamond synthesized block is taken out after the synthesis is completed.
In some embodiments of the invention, after the diamond synthetic block is taken out, the taken-out diamond synthetic block is knocked into pieces to obtain a sintered synthetic column, the synthetic column is placed into a beaker filled with hydrochloric acid solution with the concentration of 35-38wt%, and the beaker is placed on an electric furnace with the temperature of 180-220 ℃ to be heated until the alloy is completely reacted and drops to expose the diamond, thus obtaining the diamond.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The diamond synthesis block provided by the embodiment comprises a first conductive steel cap 711, a second conductive steel cap 712, a first graphite sheet, a second graphite sheet, a graphite heating pipe, a first pyrophyllite ring 71, a second pyrophyllite ring 72, a first dolomite ring, a second dolomite ring, a dolomite liner, pyrophyllite blocks 5 and a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover 1, a female cavity 2 and a lower cover 3; the upper cover 1 and the lower cover 3 are fixed on two sides of the female cavity 2; the upper cover 1 is provided with a plurality of cavities, and a first heat conduction column 11 is arranged in the cavity of the upper cover 1; the lower cover 3 is provided with a plurality of cavities, and a second heat conduction column 31 is arranged in the cavity of the lower cover 3; a plurality of subchambers 21 are arranged in the main chamber 2; an upper insulating plug 211, a carbon source 212, a catalyst 213, a copper sheet 214 and a crystal bed 215 which are sequentially connected are arranged in the subchamber 21; the upper cover 1 is connected with an upper insulating plug 211; the lower cover 3 is connected with the crystal bed 215; a seed crystal 216 is arranged in the crystal bed 215, and the seed crystal 216 is adjacent to one side of the copper sheet 214; the number of the cavities of the upper cover 1 and the number of the subcavities 21 are the same as the number of the cavities of the lower cover 3;
the first graphite heating plate and the second graphite heating plate are arranged on two sides of the graphite heating pipe; the first graphite heating plate, the second graphite heating plate and the graphite heating pipe are enclosed to form a containing cavity, and the diamond synthesis cavity is placed in the containing cavity;
the first conductive steel cap 711 is connected with the first graphite heating plate; the first graphite heating plate is connected with the upper cover 1; the first graphite heating plate is connected with the first dolomite ring; the first dolomite ring is connected to the first pyrophyllite ring 71; the first conductive steel cap 711 is disposed in a receiving cavity formed by the first dolomitic stone ring and the first pyrophyllite 71 ring;
the second conductive steel cap 721 is connected to a second graphite heating plate; the second graphite heating plate is connected with the lower cover 3; the second graphite heating plate is connected with a second dolomite ring; the second dolomite ring is connected to the second pyrophyllite ring 72; the second conductive steel cap 721 is disposed in the receiving cavity formed by the second dolomite ring and the second pyrophyllite ring 72;
the middle part of the pyrophyllite block 5 is provided with a hollow cavity with a hollow structure; the side wall of the cavity of the pyrophyllite block 5 is connected with a dolomite lining; the dolomite lining is connected with a graphite heating pipe.
The assembly of the diamond composite block includes: 1. the second heat conduction columns 31 are plugged into the corresponding cavities of the lower cover 3; 2. the mother cavity 2 is arranged on the lower cover 3, and a crystal bed 215, a copper sheet 214, a catalyst 213, a carbon source 212 and an upper insulating plug 211 are respectively arranged in a sub-cavity 21 of the mother cavity 2 from bottom to top; 3. the first heat conduction columns 11 are placed in the corresponding cavities of the upper covers 1, and the corresponding holes are covered above the female cavities 2; 4. placing the assembled component into a graphite heating pipe; 5. the first graphite sheet and the second graphite sheet are respectively arranged at the upper end and the lower end of a graphite heating pipe; 6, placing the assembled structure into a dolomite lining, and then placing the dolomite lining into a pyrophyllite block 5; 7. the first conductive steel cap 711, the second conductive steel cap 722, the first dolomite ring, the second dolomite ring, the first pyrophyllite ring 71 and the second pyrophyllite ring 72 are arranged at the upper end and the lower end of the diamond synthetic block, and the diamond synthetic block is completely assembled.
Example 2
The diamond synthesis block provided in this example refers to example 1, in which the preparation method of each structure is as follows:
the preparation method of the upper cover 1 comprises the following steps: placing 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully and uniformly mix, and placing the mixture in a drying oven at 100 ℃ for more than 12 hours to dry water; then placing the mixture into a die, and pressing and forming the mixture under the pressure of 20-30 tons by using a tablet press;
the preparation method of the lower cover 3 comprises the following steps: placing 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully and uniformly mix, and placing the mixture in a drying oven at 100 ℃ for more than 12 hours to dry water; then placing the mixture into a die, and pressing and forming the mixture under the pressure of 20-30 tons by using a tablet press;
the preparation method of the female cavity 2 comprises the following steps: placing 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully and uniformly mix, and placing into a drying oven at 100 ℃ to dry water for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture under the pressure of 25-30 tons by using a tablet press;
the preparation method of the upper insulating plug 211 comprises the following steps: placing 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully and uniformly mix, and placing into a drying oven at 100 ℃ to dry water for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture under the pressure of 20-30 tons by using a tablet press;
the method for preparing the carbon source 212 includes: the purity is more than or equal to 99.99 percent, the graphitization degree is more than or equal to 99.8 percent, and the effective density is 1.99g/cm 3 Placing the graphite powder in a drying oven at 100 ℃ for more than 12 hours, drying the moisture in the graphite, and pressing the graphite powder into a shape by a tablet press under the pressure of 20-30 tons; then placing the mixture into a drying oven at 100 ℃ for more than 12 hours to dry the mixture; because the purity requirement of the carbon source 211 is high, the preparation process of the carbon source 211 needs to be operated in a special dust-free space to prevent other impurities from being mixed;
the catalyst 213 includes one or more of a catalyst of colorless diamond, a catalyst of blue diamond, and a catalyst of yellow diamond;
the catalyst for the colorless diamond comprises the following components in parts by weight: 67.5 parts of Fe, 30 parts of Ni, 5 parts of Al and 1 part of Cu;
the catalyst of the blue diamond comprises the following components in parts by weight: 67.495 parts of Fe, 30 parts of Ni, 1.5 parts of Al, 1 part of Cu and 0.005 part of B;
the catalyst for the yellow diamond comprises the following components in parts by weight: 60-75 parts of Fe and 25-35 parts of Ni;
the preparation method of the catalyst 213 comprises the following steps: preparing various alloy components according to the components of the catalyst 213, sequentially placing the alloy components into a vacuum magnetic suspension smelting furnace from bottom to top according to the unit mass from light to heavy, fully melting all raw materials at 1700 ℃, naturally cooling to obtain an alloy ingot, and cutting the alloy ingot into shapes by using linear cutting equipment;
the preparation method of the crystal bed 215 comprises the following steps: calcining magnesium oxide with purity more than or equal to 99.5% at 1200-1400 ℃ for 3.5-5 h, then placing the calcined magnesium oxide into a die, and pressing and forming the magnesium oxide by using a tablet press under 15-25 tons of pressure; punching a hole in the center of the upper end of the pressed crystal bed (near to the catalyst 213 side), placing a seed crystal 216 with the diameter of 0.5mm, and then placing the seed crystal 216 in a drying oven with the temperature of 100 ℃ for more than 12 hours to dry the water;
the preparation method of the first heat conduction column 11 comprises the following steps: 5-10 parts of magnesium oxide and 90-95 parts of sodium chloride are put into a three-dimensional mixer to be stirred for 1-2 hours, and after being fully and uniformly mixed, the mixture is dried at 100 ℃ for more than or equal to 12 hours and then is pressed and molded by a tablet press under the pressure of 10-20 tons;
the second heat conductive pillar 31 is prepared by the following steps: placing 80-90 parts of magnesium oxide and 10-20 parts of graphite powder with purity more than or equal to 99% into a three-dimensional mixer, stirring for 1-2 hours to fully and uniformly mix the materials, drying the materials at 100 ℃ for more than or equal to 12 hours, and then pressing the materials into a shape by using a tablet press under the pressure of 10-20 tons;
the preparation method of the first graphite flake and the second graphite flake comprises the following steps: stamping a wafer by using graphite paper with the thickness of 1-1.5 mm;
the preparation method of the graphite heating pipe comprises the following steps: turning a graphite pipe on a lathe by the high-purity graphite column, placing the graphite pipe in a drying oven at 100 ℃ for more than 12 hours, and drying the moisture in the graphite pipe.
Example 3
The diamond synthesis block provided in this example refers to example 2, in which the shape and size of each structure are as follows;
upper cover 1: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 5mm; the height of the cavity is 10mm;
lower cover 3: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 5mm; the height of the cavity is 10mm;
female chamber 2: a porous (subchamber) cylinder of height 26mm and diameter 57 mm; the diameter of the subchamber 21 is 5mm, and the height of the subchamber 21 is 26mm;
upper insulating plug 211: a cylinder with a height of 5mm and a diameter of 5mm;
carbon source 212: a cylinder with a height of 6mm and a diameter of 5mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 5mm;
copper sheet 214: a wafer with thickness of 0.05mm and diameter of 5mm;
crystal bed 215: a cylinder with a height of 5mm and a diameter of 5mm;
first heat conduction column 11: cylinder with height of 10mm and diameter of 5mm
Second heat conductive post 311: cylinder with height of 10mm and diameter of 5mm
First graphite flake: a disc of 59mm diameter;
a second graphite sheet; a disc of 59mm diameter;
graphite heating pipe: a graphite tube with a height of 46mm, an outer diameter of 59mm and a tube wall thickness of 1mm;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner hole diameter (the dimension after embedding the dolomite liner) of 59mm; the dolomite lining has a thickness of 3mm.
The preparation method of the diamond with the improved implementation comprises the following steps:
placing the diamond synthetic block in a drying box at 100 ℃ for 12 hours, placing the dried diamond synthetic block in a hexahedral top press, increasing the pressure from 0GPa to 5.7GPa within 3 hours, increasing the power from 0kw to 5.5-6.5 kw, synthesizing for 5-6 days, reducing the power to 0kw within 1 hour after synthesis is completed, reducing the pressure to 0GPa within 2 hours, and then taking out the synthetic block;
breaking the extracted diamond synthetic block to obtain a sintered synthetic column, putting the synthetic column into a beaker filled with hydrochloric acid solution with the concentration of 35-38wt%, and heating the beaker on an electric furnace at 200 ℃ until the alloy completely reacts and drops to expose the diamond, thus obtaining the diamond.
The diamond produced in this example was 1 to 1.2 carats.
Example 4
The diamond synthesis block provided in this example refers to example 2, in which the shape and size of each structure are as follows;
upper cover 1: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 7mm; the height of the cavity is 10mm;
lower cover 3: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 7mm; the height of the cavity is 10mm;
female chamber 2: a porous (subchamber) cylinder of height 26mm and diameter 57 mm; the diameter of the subchamber 21 is 7mm, and the height of the subchamber 21 is 26mm;
upper insulating plug 211: a cylinder 7mm in height and 5mm in diameter;
carbon source 212: a cylinder with a height of 6mm and a diameter of 7mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 7mm;
copper sheet 214: a wafer with a thickness of 0.05mm and a diameter of 7mm;
crystal bed 215: a cylinder with a height of 5mm and a diameter of 7mm;
first heat conductive column 111: a cylinder with a height of 10mm and a diameter of 7mm;
second heat conductive post 311: a cylinder with a height of 10mm and a diameter of 7mm;
first graphite flake: a disc of 59mm diameter;
a second graphite sheet; a disc of 59mm diameter;
graphite heating pipe: a graphite tube with a height of 46mm, an outer diameter of 59mm and a tube wall thickness of 1mm;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner hole diameter (the dimension after embedding the dolomite liner) of 59mm; the dolomite lining has a thickness of 3mm.
The preparation method of the diamond improved in this embodiment is described with reference to example 3, except that the synthesis time is 5 to 7 days.
The diamond produced in this example was 3 to 3.5 carats.
Example 5
The diamond synthesis block provided in this example refers to example 2, in which the shape and size of each structure are as follows;
upper cover 1: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 9mm; the height of the cavity is 10mm;
lower cover 3: a cylinder with a height of 10mm and a diameter of 57mm and containing a plurality of cylindrical cavities; the diameter of the cavity is 9mm; the height of the cavity is 10mm;
female chamber 2: a porous (subchamber) cylinder of height 26mm and diameter 57 mm; the diameter of the subchamber 21 is 5mm, and the height of the subchamber 21 is 26mm;
upper insulating plug 211: a cylinder with a height of 5mm and a diameter of 9mm;
carbon source 212: a cylinder with a height of 6mm and a diameter of 9mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 9mm;
copper sheet 214: a wafer with thickness of 0.05mm and diameter of 9mm;
crystal bed 215: a cylinder with a height of 5mm and a diameter of 9mm;
first heat conduction column 11: a cylinder with a height of 10mm and a diameter of 9mm;
second heat conductive column 31: a cylinder with a height of 10mm and a diameter of 9mm;
first graphite flake: a disc of 59mm diameter;
a second graphite sheet; a disc of 59mm diameter;
graphite heating pipe: a graphite tube with a height of 46mm, an outer diameter of 59mm and a tube wall thickness of 1mm;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner hole diameter (the dimension after embedding the dolomite liner) of 59mm; the dolomite lining has a thickness of 3mm.
The preparation method of the diamond improved in this embodiment is described with reference to example 3, except that the synthesis time is 5 to 8 days.
The diamond produced in this example was 5 to 6 carats.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (12)
1. A diamond synthesis block comprising a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover, a female cavity and a lower cover;
the upper cover and the lower cover are arranged on two sides of the female cavity;
the upper cover is provided with a plurality of cavities, and a first heat conduction column is arranged in the cavity of the upper cover;
the lower cover is provided with a plurality of cavities, and a second heat conduction column is arranged in the cavity of the lower cover;
a plurality of subchambers are arranged in the main chamber;
an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are sequentially connected are arranged in the subchamber;
the diamond synthesis block further comprises a first heating plate, a second heating plate and a heating pipe;
the first heating plate and the second heating plate are arranged on two sides of the heating pipe; the first heating plate, the second heating plate and the heating pipe are enclosed to form a containing cavity, and the diamond synthesis cavity is arranged in the containing cavity;
the heat conductivity of the first heat conduction column and the heat conductivity of the second heat conduction column at the two ends of each subchamber are different;
placing the catalyst for growing diamond with different colors in each subchamber;
the first heating plate is circular, and the diameter of the first heating plate is 57-61 mm;
the second heating plate is round, and the diameter of the second heating plate is 57-61 mm;
the height of the heating pipe is 40-52 mm;
the pipe wall thickness of the heating pipe is 0.5-1.5 mm;
the diameter of the first heat conduction column is 4-10 mm, and the height of the first heat conduction column is 8-10 mm;
the diameter of the second heat conduction column 31 is 4-10 mm, and the height of the second heat conduction column is 8-10 mm;
the diameter of the subchamber is 4-10 mm, and the height of the subchamber is 24-28 mm;
the second heating plate is connected with the lower cover;
the first heat conduction column comprises the following components in parts by weight: 5-10 parts of magnesium oxide and/or zirconium oxide and 90-95 parts of sodium chloride;
the second heat conduction column comprises the following components in parts by weight: 80-90 parts of magnesium oxide and 10-20 parts of graphite powder;
the first heating sheet comprises one or more of graphite, silicon carbide and magnesium;
the second heating sheet comprises one or more of graphite, silicon carbide and magnesium;
the heating tube comprises one or more of graphite, silicon carbide and magnesium.
2. The diamond-composite block according to claim 1, further comprising a first conductive steel cap and a second conductive steel cap;
the first conductive steel cap is connected with the first heating plate;
the second conductive steel cap is connected with the second heating plate.
3. The diamond composite block according to claim 2, further comprising a first pyrophyllite ring, a second pyrophyllite ring, a first plugging ring, a second plugging ring, a liner, and a pyrophyllite block;
the first heating piece is connected with the first plugging ring; the first plugging ring is connected with the first pyrophyllite ring; the first conductive steel cap is arranged in a containing cavity formed by the first plugging ring and the first pyrophyllite ring;
the second heating piece is connected with the second blocking ring; the second plugging ring is connected with the second pyrophyllite ring; the second conductive steel cap is arranged in a containing cavity formed by the second plugging ring and the second pyrophyllite ring;
the middle part of the pyrophyllite block is provided with a hollow cavity with a hollow structure;
the side wall of the cavity of the pyrophyllite block is connected with the lining; the inner liner is connected with the heating pipe.
4. The diamond compact of claim 1 wherein said upper cap is connected to said upper insulating plug;
the lower cover is connected with the crystal bed;
a seed crystal is arranged in the crystal bed;
the number of the cavities of the upper cover and the number of the subchambers are the same as the number of the cavities of the lower cover.
5. The diamond compact of claim 1 wherein said cap comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia;
the lower cover comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia;
the female cavity comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia.
6. The diamond compact of claim 1 wherein said upper insulating plug comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconia;
the carbon source comprises graphite powder;
the crystal bed comprises a magnesium oxide crystal bed.
7. The diamond-synthesized block according to claim 6, wherein the purity of the graphite powder is not less than 99.99%, and the graphitization degree of the graphite powder is not less than 99.8%.
8. The diamond synthesis block according to claim 6, wherein the method of preparing the crystal bed comprises: calcining magnesium oxide with purity not less than 99.5% at 1100-1500 deg.c for 2-5 hr, and pressing to form.
9. The diamond compact of claim 1 wherein said catalyst comprises the following components in parts by weight: 60 to 75 parts of Fe, 25 to 35 parts of Ni, 1 to 5 parts of Al, 1 to 3 parts of Cu and 0.004 to 0.008 part of B;
or the catalyst comprises the following components in parts by weight: 60-75 parts of Fe, 25-35 parts of Ni, 1-5 parts of Al and 1-3 parts of Cu;
or the catalyst comprises the following components in parts by weight: 60-75 parts of Fe and 25-35 parts of Ni.
10. The diamond compact of claim 9 wherein said catalyst is prepared by a process comprising: preparing various alloy components according to the components of the catalyst, smelting at 1650-1750 ℃, cooling, cutting and forming.
11. A method for preparing diamond, comprising the steps of:
synthesizing the dried diamond synthesized block according to any one of claims 1 to 10 for 5 to 10 days under the conditions of pressure of 5.5 to 6GPa and power of 5 to 7kw, and taking out the synthesized diamond synthesized block after synthesis.
12. The method of manufacturing diamond according to claim 11, wherein the dried diamond synthetic block is put into a top press, the pressure is increased from 0GPa to 5.5 to 6GPa, the power is increased from 0kw to 5 to 7kw, and the diamond synthetic block is synthesized for 5 to 10 days, and the diamond synthetic block is taken out after the synthesis is completed.
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| 合成腔的结构对合成金刚石的影响;王松顺;探矿工程(岩土钻掘工程)(第01期);全文 * |
| 王松顺.合成腔的结构对合成金刚石的影响.探矿工程(岩土钻掘工程).1989,(01),全文. * |
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