CN115041099A - Diamond synthesis block and preparation method of diamond - Google Patents
Diamond synthesis block and preparation method of diamond Download PDFInfo
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- CN115041099A CN115041099A CN202210848422.9A CN202210848422A CN115041099A CN 115041099 A CN115041099 A CN 115041099A CN 202210848422 A CN202210848422 A CN 202210848422A CN 115041099 A CN115041099 A CN 115041099A
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- 239000010432 diamond Substances 0.000 title claims abstract description 148
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 125
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 86
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000003054 catalyst Substances 0.000 claims abstract description 44
- 239000013078 crystal Substances 0.000 claims abstract description 36
- 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
- 238000010438 heat treatment Methods 0.000 claims description 85
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 64
- 229910002804 graphite Inorganic materials 0.000 claims description 64
- 239000010439 graphite Substances 0.000 claims description 64
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 47
- 239000011780 sodium chloride Substances 0.000 claims description 32
- 229910000831 Steel Inorganic materials 0.000 claims description 28
- 239000010959 steel Substances 0.000 claims description 28
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 19
- 239000000395 magnesium oxide Substances 0.000 claims description 17
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 17
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 17
- 238000003825 pressing Methods 0.000 claims description 17
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 16
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000000903 blocking effect Effects 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 14
- 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
- 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
- 239000000956 alloy Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 238000005520 cutting process Methods 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
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- QCWXUUIWCKQGHC-BJUDXGSMSA-N zirconium-90 Chemical group [90Zr] QCWXUUIWCKQGHC-BJUDXGSMSA-N 0.000 claims description 3
- 239000003086 colorant Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 description 31
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 28
- 238000001035 drying Methods 0.000 description 28
- 239000010459 dolomite Substances 0.000 description 26
- 229910000514 dolomite Inorganic materials 0.000 description 26
- 238000000748 compression moulding Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008451 emotion Effects 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000004080 punching Methods 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
- 238000000227 grinding Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000002452 interceptive effect Effects 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
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 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
Images
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 mother 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 first heat-conducting columns are arranged in the cavities of the upper cover; the lower cover is provided with a plurality of cavities, and second heat-conducting columns are arranged in the cavities of the lower cover; a plurality of sub-cavities are arranged in the mother cavity; an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are connected in sequence are arranged in the sub-cavity. The diamond synthesis block of the invention can be used for cultivating diamonds 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
The growth of the diamond market in recent years is gradually changing the consumption habits of people, and the consumption of people for spirit and emotion is gradually increased along with the improvement of the living standard of the substances, and the diamond is always symbolized by love and eternity for centuries due to the firm characteristic, and nowadays the diamond is cultivated, namely, diamond, can continue to expand the scope of expressed emotion, which can symbolize friendship, familiarity, teacher-student's emotion, war friendship, etc. in addition to symbolizing love, carbon elements can be extracted from human tissues such as hair, nails, teeth, body hair, fallen skin, dandruff, etc. at present, and the extracted carbon element is used for manufacturing the biological diamond in a specially manufactured cavity by a high-temperature high-pressure method, these diamonds will collectively contain carbon elements extracted from a biological sample, indicating the adherence of two or more people to companionship.
The existing growth cavity for cultivating the diamond synthesis block is of a single-cavity structure, and only 1-30 diamonds with the same color and similar size can grow in the single-cavity structure at a time. With the increasing demand for customized customization, the method of cultivating diamonds of a single color and size at a time is no longer practical, and the structure of a single chamber results in increased cost for the manufacturer and reduced selectivity for the customer. For the case of individually customized diamonds but with different color requirements, the use of a single cavity structure to cultivate diamonds would be uneconomical and cost-effective to meet customer needs based on the prior art requiring 5 syntheses. Under the condition that the diamonds are the same in color but different in required carat quality, the diamonds are cultivated by adopting a single cavity structure, the cultivation process needs to be completed according to the maximum required time in the synthesis, the larger the diamond growth, the longer the time, and finally, the diamonds cultivated in the synthesis are all similar in size, the diamonds are cut into the target size according to the requirement, the larger the diamond grinding cost is, and the diamond preparation cost is increased.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a diamond synthesis block, which is used for completely or partially solving the problem that diamonds with different colors and sizes cannot be cultivated at one time in the prior art, effectively improving the utilization rate of a synthesis cavity and reducing the production cost of the diamonds.
The second purpose of the invention is to provide a method for preparing diamond, which synthesizes the diamond synthesis block under certain conditions and can prepare diamond with different types and high quality at one time.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a diamond synthesis block, which comprises a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover, a mother 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 first heat-conducting columns are arranged in the cavities of the upper cover;
the lower cover is provided with a plurality of cavities, and second heat-conducting columns are arranged in the cavities of the lower cover;
a plurality of sub-cavities are arranged in the mother cavity;
an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are connected in sequence are arranged in the sub-cavity.
The invention also provides a preparation method of the diamond, which comprises the following steps:
and (3) synthesizing the dried diamond synthesis block for 5-10 days under the conditions that the pressure is 5.5-6 GPa and the power is 5-7 kw, and taking out the diamond synthesis block after the synthesis is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the diamond synthesis block, the whole large mother cavity comprises a plurality of small sub-cavities, raw materials for growing diamonds with different colors can be added into each sub-cavity according to requirements, the raw materials between the sub-cavities cannot interfere with each other, and therefore diamonds with different colors can be grown; in addition, place the first heat conduction post and the second heat conduction post of different thermal conductivities in every sub cavity corresponding top and below, can be in the interval effectual every sub cavity top of control and the temperature difference of below like this to reach the purpose of the growth rate of control diamond, the size of the diamond that the growth rate difference obtained in the sub cavity is different, thereby can grow out the diamond of different sizes.
(2) The preparation method of the diamond adopts the diamond synthesis block with a multi-cavity structure to synthesize, the growth conditions in each sub-cavity can be independently controlled, reasonable partition cultivation can be carried out in one synthesis process according to production requirements and requirements on the diamond, different types of diamond can grow in different areas, 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 used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural view of a diamond synthesis chamber according to the present invention.
Fig. 2 is a schematic view of the structure of the diamond composite block of the present invention.
Reference numerals:
1-covering the upper cover; 11-a first thermally conductive post; 2-a female cavity;
21-a subcavity; 211-upper insulation block; 212-a carbon source;
213-catalyst; 214-copper sheet; 215-crystal bed
216-seed crystal; 3-lower cover; 31-a second thermally conductive post;
41-a first heating plate; 42-a second heat patch; 5-pyrophyllite block;
51-an inner liner; 52-heating tube; 61-a first plugging ring;
62-a second plugging ring; 71-first pyrophyllite ring; 711-a first conductive steel cap;
72-second pyrophyllite ring; 721-second conductive steel cap.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
A diamond synthesis block and a method for producing diamond according to an embodiment of the present invention will be specifically described below.
Referring to figure 1, in some embodiments of the invention there is provided a diamond synthesis block comprising a diamond synthesis chamber;
the diamond synthesis cavity comprises an upper cover 1, a mother cavity 2 and a lower cover 3;
the upper cover 1 and the lower cover 3 are arranged at two sides of the mother cavity 2;
the upper cover 1 is provided with a plurality of cavities, and the cavities of the upper cover 1 are internally provided with first heat-conducting columns 11;
the lower cover 3 is provided with a plurality of cavities, and second heat-conducting columns 31 are arranged in the cavities of the lower cover 3;
a plurality of sub-cavities 21 are arranged in the mother cavity 2;
an upper insulating plug 211, a carbon source 212, a catalyst 213, a copper sheet 214 and a crystal bed 216 which are connected in sequence are arranged in the sub-cavity 21.
The diamond synthesis block provided by the invention comprises a plurality of sub-cavities 21, different catalysts 213 can be placed in the cavity of each sub-cavity 21, and heat-conducting 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 sub-cavity 21 can be independently controlled without interfering with each other; by individually controlling the catalyst 213 and temperature gradient in each sub-chamber 21, diamonds of different colors and sizes can be produced in a single synthesis of the diamond synthesis block.
The traditional diamond single crystal growth cavity can only contain one catalyst 213, and the structure can only correspond to one temperature gradient, so that the traditional diamond single crystal growth cavity is only suitable for growing diamonds with one color and similar size; in the diamond synthesis block of the invention, the growth cavity is divided into a plurality of sub-cavities 21, firstly different catalysts 213, carbon sources 212 and crystal beds 215 for growing diamonds with different colors are put into each sub-cavity 21, and secondly the same or different heat conduction columns are put in the reserved cavities of the upper cover 1 and the lower cover 3 at the two sides of each sub-cavity 21, thereby preparing diamonds with different types in one synthesis process.
Referring to fig. 2, in some embodiments of the present invention, the diamond composite block further includes a first conductive steel cap 711, a second conductive steel cap 721, a first heating plate 41, a second heating plate 42, and a heating pipe 52;
the first and second heating sheets 41 and 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 an accommodating cavity, and the diamond synthesis cavity is placed in the accommodating cavity;
the first conductive steel cap 711 is connected with the first heating sheet 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 sheet 42;
the second heating sheet 42 is connected to the lower cover 3.
In some embodiments of the present invention, the diamond composite block further comprises a first pyrophyllite ring 71, a second pyrophyllite ring 72, a first blocking ring 61, a second blocking ring 62, an inner liner 51, and a pyrophyllite block 5;
the first heating plate 41 is connected with the first blocking ring 61; the first plugging ring 61 is connected with the first pyrophyllite ring 71; the first conductive steel cap 711 is arranged in a containing cavity formed by the first blocking ring 61 and the pyrophyllite ring 71;
the second heating plate 42 is connected with the second blocking ring 62; the second plugging ring 62 is connected with the second pyrophyllite ring 72; a second conductive steel cap 721 is arranged in the accommodating cavity formed by the second blocking 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 synthesis block of the present invention, the first pyrophyllite ring 71 and the first blocking ring 61 form a cavity penetrating the upper and lower surfaces, and the first conductive steel cap 711 is disposed in the cavity, that is, the first pyrophyllite ring 71 and the first blocking ring 61 are filled around the first conductive steel cap 711. The second pyrophyllite ring 72 and the second blocking ring 62 form a cavity penetrating through the upper surface and the lower surface, and the second conductive steel cap 721 is arranged in the cavity, namely the second pyrophyllite ring 72 and the second blocking ring 62 are filled around the second conductive steel cap 721.
In some embodiments of the present invention, the upper cap 1 is connected to the upper insulating plug 211.
In some embodiments of the present invention, the lower lid 3 is connected to the seed bed 215.
In some embodiments of the present invention, a seed crystal 216 is disposed within the seed bed 215; the seed crystal is positioned within the seed beds 215 adjacent to the sides of the copper sheets 214, and the seed crystal 216 is positioned at the center of the upper end of each seed bed 215.
In some embodiments of the present invention, a layer of copper sheet 214 is covered on the seed 216 to protect the seed 216.
In some embodiments of the present invention, the seed 216 has a particle size of 0.4 to 0.6 mm.
In some embodiments of the present invention, the number of cavities of the upper cover 1 and the number of the sub-cavities 21 are the same as the number of cavities of the lower cover 3; the number of the sub-cavities 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 zirconium oxide; preferably, the method for preparing the upper cap 1 includes: after sodium chloride and zirconia are mixed uniformly, drying the mixture at the temperature of 80-120 ℃ for more than or equal to 12 hours, and then pressing and forming the mixture; preferably, the pressure of the compression molding is 20-30 tons. By drying, the moisture in the raw material can be removed.
In some embodiments of the present invention, the lower cover 3 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide; preferably, the method for preparing the lower cap 3 includes: after sodium chloride and zirconia are mixed uniformly, drying the mixture at the temperature of 80-120 ℃ for more than or equal to 12 hours, and then pressing and forming the mixture; preferably, the pressure of the compression molding is 20-30 tons.
In some embodiments of the present invention, the master cavity 2 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide; preferably, the preparation method of the mother cavity 2 comprises: after sodium chloride and zirconia are mixed uniformly, drying the mixture at the temperature of 80-120 ℃ for more than or equal to 12 hours, and then pressing and forming the mixture; preferably, the pressure of the compression molding is 25-30 tons.
In some embodiments of the present invention, the upper insulating plug 211 comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide; preferably, the preparation method of the upper insulating plug 211 includes: after sodium chloride and zirconia are mixed uniformly, drying the mixture at the temperature of 80-120 ℃ for more than or equal to 12 hours, and then pressing and forming the mixture; preferably, the pressure of the compression molding is 20-30 tons.
In some embodiments of the invention, 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 (ii) a Preferably, the method for preparing the carbon source 212 comprises: drying the carbon source 212 at 80-120 ℃ for more than or equal to 12 hours, then pressing and forming, and then drying at 80-120 ℃ for more than or equal to 12 hours; preferably, the pressure of the compression molding is 20-30 tons. Since the purity of the carbon source 212 is required to be high, the preparation process of the carbon source 212 needs to be performed in a dedicated dust-free space to prevent the mixing of other impurities.
In some embodiments of the present invention, the bed 215 comprises a bed of magnesium oxide; preferably, the preparation method of the crystal bed 215 includes: calcining the magnesium oxide with the purity of more than or equal to 99.5% at 1100-1300 ℃ for 2-5 h, and then pressing and forming; preferably, the pressure of the compression molding is 15-25 tons.
In some embodiments of the present invention, a hole is punched in the center of the upper end of each pressed seed bed 215 and a seed 216 is placed therein.
In some embodiments of the invention, 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, 1-3 parts of Cu and 0.004-0.008 parts of B; the diamond prepared by the catalyst 212 with the components is blue diamond;
or, 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 above components is colorless diamond;
or, 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 using the catalyst 213 of the above composition is yellow diamond.
In some embodiments of the invention, the method of 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 invention, catalysts 213 for growing diamonds with different colors can be placed in each sub-cavity 21 according to requirements, and raw materials among the sub-cavities 21 cannot interfere with each other, so that diamonds with different colors can be grown.
In some embodiments of the present invention, the first thermally conductive pillar 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 method for preparing the first heat conduction column 11 includes: uniformly mixing the raw materials, drying at the temperature of 80-120 ℃ for more than or equal to 12 hours, and pressing for forming; preferably, the pressure of the compression molding is 10 to 20 tons.
In some embodiments of the present invention, the first thermally conductive pillar 11 comprises the following components in parts by weight: 5-10 parts of magnesium oxide and 90-95 parts of sodium chloride; or, the first heat conduction column 11 comprises the following components in parts by weight: 5-10 parts of zirconium oxide and 90-95 parts of sodium chloride.
In some embodiments of the present invention, the second thermally conductive pillar 31 comprises the following components in parts by weight: 80-90 parts of magnesium oxide and 10-20 parts of graphite powder; preferably, the method for manufacturing the second heat conduction pillar 31 includes: uniformly mixing magnesium oxide and graphite powder, drying at 80-120 ℃ for more than or equal to 12 hours, and pressing for forming; preferably, the pressure of the compression molding is 10 to 20 tons.
In the diamond synthesis block of the invention, the first heat-conducting column 11 and the second heat-conducting column 31 with different heating efficiencies can be arranged above and below the corresponding sub-cavity 21, so that the temperature difference above and below each sub-cavity 21 can be effectively controlled in an interval, the purpose of controlling the growth speed of diamond is achieved, and the growth speed different in each sub-cavity 21 determines the growth size of diamond in each cavity in one synthesis.
In some embodiments of the present invention, the first heating sheet 41 comprises one or more of graphite, silicon carbide, and magnesium.
In some embodiments of the present invention, the first heating plate 41 is made of graphite; or the first heating sheet 41 is made of graphite and silicon carbide, and the mass ratio of the graphite to the silicon carbide is 94-96: 4-6; or the first heating plate 41 is made of graphite and magnesium; the mass ratio of the graphite to the 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 heating sheet 42 comprises one or more of graphite, silicon carbide, and magnesium.
In some embodiments of the present invention, the second heating plate 42 is made of graphite; or the second heating sheet 42 is made of graphite and silicon carbide, and the mass ratio of the graphite to the silicon carbide is 94-96: 4-6; or the second heating plate 42 is made of graphite and magnesium; the mass ratio of the graphite to the 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: 4-6; or the heating pipe 52 is made of graphite and magnesium; the mass ratio of the graphite to the 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 zirconium oxide; or the composite material lining is made of zirconium oxide and sodium chloride, and the mass ratio of the zirconium oxide 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 comprises zirconia and sodium chloride; the mass ratio of the zirconium oxide 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 invention, the material of the second plug ring 62 comprises dolomite or a composite material comprising zirconia and sodium chloride; the mass ratio of the zirconium oxide 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 cylinder; preferably, the upper cap 1, the female cavity 2 and the lower cap 3 have the same diameter.
In some embodiments of the present invention, the shape of the cavity of the upper cap 1, the shape of the sub-cavity 21, and the shape of the cavity of the lower cap 3 are the same; the shape of subchamber 21 comprises a cylinder; preferably, the cavity of the upper cap 1, the sub-cavity 21 and the cavity of the lower cap 3 have the same diameter.
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 insulating 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 seed bed 215.
In some embodiments of the invention, the shape and size of each structure in the composite mass of diamond is as follows:
the upper cover 1 is cylindrical; 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-conducting column 11 is cylindrical; preferably, the diameter of the first heat-conducting column 11 is 4-10 mm, and the height of the first heat-conducting column 11 is 8-10 mm;
the lower cover 3 is cylindrical; preferably, the diameter of the lower cover 3 is 55-59 mm; 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 conduction column 31 includes a cylindrical shape; preferably, the diameter of the second heat-conducting column 31 is 4-10 mm, and the height of the second heat-conducting column 31 is 8-10 mm;
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 mother cavity 2 is 24-28 mm; more preferably, the sub-cavity 21 comprises a cylindrical shape, the diameter of the sub-cavity 21 is 4-10 mm, and the height of the sub-cavity 21 is 24-28 mm;
the upper insulating plug 211 is cylindrical, 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 catalyst 213 is cylindrical in shape; preferably, the diameter of the catalyst 213 is 4 to 10mm, and the height of the catalyst 213 is 8 to 12 mm;
the copper sheet 214 is circular in shape; preferably, the diameter of the copper sheet 214 is 4 to 10mm, and the thickness of the copper sheet 214 is 0.05 to 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 thickness of the tube wall of the heating tube 52 is 0.5-1.5 mm; preferably, the outer diameter of the heating pipe 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 inner diameter of the pyrophyllite block 5 is the dimension after the lining is inlaid.
The shape and size of each structure of the diamond synthesis block are not strictly limited, and can be adjusted according to actual conditions.
In some embodiments of the invention, the assembling of the diamond composite block comprises: 1. the second heat conduction column 311 is plugged into the cavity of the corresponding lower cover 3; 2. the mother cavity 2 is placed on the lower cover 3, and the crystal bed 215, the copper sheet 214, the catalyst 213, the carbon source 212 and the upper insulating plug 211 are respectively placed into the sub-cavities 21 of the mother cavity 2 from bottom to top; 3. placing the first heat-conducting column 11 into the corresponding cavity of the upper cover 1, and covering the corresponding hole position above the mother cavity 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 into an inner liner 51 and then placing the structure into a pyrophyllite block 5; 7. and placing a first conductive steel cap 711, a second conductive steel cap 722, a first blocking ring 61, a second blocking ring 62, a first pyrophyllite ring 71 and a second pyrophyllite ring 72 at the upper end and the lower end of the diamond synthetic block, and completely assembling the diamond synthetic block.
There is also provided in some embodiments of the present invention a method of making diamond, comprising the steps of:
synthesizing the dried diamond synthesis block for 5-10 days under the conditions that the pressure is 5.5-6 GPa and the power is 5-7 kw, and taking out the diamond synthesis block after synthesis;
preferably, the dried diamond synthesis 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 and then the diamond synthesis block is synthesized for 5-10 days, and the diamond synthesis block is taken out after the synthesis is finished.
In some embodiments of the invention, after the diamond synthesis block is taken out, the diamond synthesis block taken out is broken into pieces to obtain a sintered synthesis column, the synthesis column is placed in a beaker filled with a hydrochloric acid solution with the concentration of 35 wt% -38 wt%, and the beaker is placed on an electric furnace at 180-220 ℃ to be heated until the alloy completely reacts and falls off to expose the diamond, so that the diamond can be obtained.
The features and properties of the present invention are described in further detail below with reference to 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 lining, a pyrophyllite block 5 and a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover 1, a mother 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 the cavities of the upper cover 1 are internally provided with first heat-conducting columns 11; the lower cover 3 is provided with a plurality of cavities, and second heat-conducting columns 31 are arranged in the cavities of the lower cover 3; a plurality of sub-cavities 21 are arranged in the mother cavity 2; an upper insulating plug 211, a carbon source 212, a catalyst 213, a copper sheet 214 and a crystal bed 215 which are connected in sequence are arranged in the sub-cavity 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 and the number of the sub-cavities 21 of the upper cover 1 are the same as the number of the cavities of the lower cover 3;
the first graphite heating sheet and the second graphite heating sheet are arranged on two sides of the graphite heating pipe; the first graphite heating sheet, the second graphite heating sheet and the graphite heating pipe are enclosed to form an accommodating cavity, and the diamond synthesis cavity is placed in the accommodating cavity;
the first conductive steel cap 711 is connected with the first graphite heating sheet; the first graphite heating sheet is connected with the upper cover 1; the first graphite heating sheet is connected with the first dolomite ring; the first dolomite ring is connected with the first pyrophyllite ring 71; a first conductive steel cap 711 is arranged in a containing cavity formed by the first dolomite ring and the first pyrophyllite 71 ring;
a second conductive steel cap 721 is connected to the second graphite heating sheet; the second graphite heating sheet is connected with the lower cover 3; the second graphite heating sheet is connected with the second dolomite ring; the second dolomite ring is connected with the second pyrophyllite ring 72; a second conductive steel cap 721 is disposed in the accommodating 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; the side wall of the cavity of the pyrophyllite block 5 is connected with the dolomite lining; the dolomite inner lining is connected with the graphite heating pipe.
The assembly of the diamond composite block comprises: 1. the second heat conduction column 31 is plugged into the cavity of the corresponding lower cover 3; 2. the mother cavity 2 is placed on the lower cover 3, and the crystal bed 215, the copper sheet 214, the catalyst 213, the carbon source 212 and the upper insulating plug 211 are respectively placed into the sub-cavities 21 of the mother cavity 2 from bottom to top; 3. placing the first heat-conducting column 11 into the corresponding cavity of the upper cover 1, and covering the corresponding hole position above the mother cavity 2; 4. putting the assembled component into a graphite heating pipe; 5. respectively placing a first graphite sheet and a second graphite sheet at the upper end and the lower end of a graphite heating pipe; 6, putting the assembled structure into a dolomite lining, and then putting the dolomite lining into a pyrophyllite block 5; 7. and placing a first conductive steel cap 711, a second conductive steel cap 722, a first dolomite ring, a second dolomite ring, a first pyrophyllite ring 71 and a second pyrophyllite ring 72 at the upper end and the lower end of the diamond synthetic block, and completely assembling the diamond synthetic block.
Example 2
The diamond synthesis block provided in this example is referred to example 1, wherein the preparation method of each structure is as follows:
the preparation method of the upper cover 1 comprises the following steps: putting 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully mix the sodium chloride and the zirconia uniformly, and then placing the mixture in a drying oven at 100 ℃ for drying the water for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture by using a tablet press under the pressure of 20-30 tons;
the preparation method of the lower cover 3 comprises the following steps: putting 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully mix the sodium chloride and the zirconia uniformly, and then placing the mixture in a drying oven at 100 ℃ for drying the water for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture by using a tablet press under the pressure of 20-30 tons;
the preparation method of the mother cavity 2 comprises the following steps: putting 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully mix the sodium chloride and the zirconia uniformly, putting the mixture into a drying oven at 100 ℃, and placing the mixture for drying for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture by using a tablet press under the pressure of 25-30 tons;
the preparation method of the upper insulating plug 211 comprises the following steps: putting 65-80 parts of sodium chloride and 20-35 parts of zirconia into a three-dimensional mixer, stirring for 1-2 hours to fully mix the sodium chloride and the zirconia uniformly, putting the mixture into a drying oven at 100 ℃, and placing the mixture for drying for more than 12 hours; then placing the mixture into a die, and pressing and forming the mixture by using a tablet press under the pressure of 20-30 tons;
the preparation method of the carbon source 212 comprises the following steps: 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 water in the graphite, and pressing and forming the graphite powder by using a tablet press under the pressure of 20-30 tons; then placing the mixture into a drying oven at 100 ℃ and placing the mixture for drying for more than 12 hours; 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 for colorless diamond, a catalyst for blue diamond, and a catalyst for yellow diamond;
the catalyst of the colorless diamond comprises the following components in parts by weight: fe 67.5 parts, Ni 30 parts, Al 5 parts and Cu 1 parts;
the catalyst of the blue diamond comprises the following components in parts by weight: fe 67.495 parts, Ni 30 parts, Al 1.5 parts, Cu 1 part and B0.005 part;
the yellow diamond catalyst 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 includes: preparing various alloy components according to the components of the catalyst 213, sequentially putting the components into a vacuum magnetic suspension smelting furnace from bottom to top in the sequence of unit mass from light to heavy, fully melting all raw materials at 1700 ℃, naturally cooling the molten raw materials to obtain an alloy ingot, and cutting and molding the alloy ingot by using linear cutting equipment;
the preparation method of the crystal bed 215 comprises the following steps: calcining magnesium oxide with the purity of more than or equal to 99.5% at 1200-1400 ℃ for 3.5-5 h, putting the calcined magnesium oxide into a die, and pressing and forming the calcined magnesium oxide under the pressure of 15-25 tons by using a tablet press; punching a hole at the center of the upper end of the pressed crystal bed (close to one side of the catalyst 213), putting a 0.5mm crystal seed 216 into the hole, and then putting the hole into a drying oven at 100 ℃ for drying water for more than 12 hours;
the preparation method of the first heat conduction column 11 comprises the following steps: putting 5-10 parts of magnesium oxide and 90-95 parts of sodium chloride into a three-dimensional mixer, stirring for 1-2 hours to fully mix the magnesium oxide and the sodium chloride, drying at 100 ℃ for more than or equal to 12 hours, and then pressing and forming by using a tablet press under the pressure of 10-20 tons;
the preparation method of the second heat conduction column 31 comprises the following steps: putting 80-90 parts of magnesium oxide and 10-20 parts of graphite powder with purity of more than or equal to 99% into a three-dimensional mixer, stirring for 1-2 hours to fully mix the magnesium oxide and the graphite powder, drying at 100 ℃ for more than or equal to 12 hours, and then pressing and forming by using a tablet press under the pressure of 10-20 tons;
the method of making the first and second graphite sheets comprises: punching 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 the high-purity graphite column to form a graphite tube on a lathe, placing the graphite tube in a drying oven at 100 ℃ for more than 12 hours, and drying the moisture in the graphite tube.
Example 3
The diamond synthesis block provided in this example is referred to example 2, in which the shape and size of each structure are as follows;
an upper cover 1: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 5 mm; the height of the cavity is 10 mm;
a lower cover 3: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 5 mm; the height of the cavity is 10 mm;
and (3) a female cavity 2: a porous (sub-cavity) cylinder 26mm in height and 57mm in diameter; the diameter of the sub-cavity 21 is 5mm, and the height of the sub-cavity 21 is 26 mm;
upper insulating plug 211: a cylinder with a height of 5mm and a diameter of 5 mm;
carbon source 212: a cylinder with a height of 6mm and a diameter of 5 mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 5 mm;
the copper sheet 214: a wafer with the thickness of 0.05mm and the diameter of 5 mm;
a crystal bed 215: a cylinder with a height of 5mm and a diameter of 5 mm;
first heat-conductive column 11: cylinder with height of 10mm and diameter of 5mm
Second heat-conductive pillar 311: cylinder with height of 10mm and diameter of 5mm
A first graphite sheet: a disc having a diameter of 59 mm;
a second graphite sheet; a disc having a diameter of 59 mm;
a graphite heating pipe: the graphite pipe is 46mm in height, 59mm in outer diameter and 1mm in pipe wall thickness;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner bore diameter (dimension after insertion of the dolomite liner) of 59 mm; the thickness of the dolomite lining is 3 mm.
The preparation method of the diamond improved by the implementation comprises the following steps:
the diamond synthesis block of the embodiment is placed in a drying box at 100 ℃ for 12 hours, the dried diamond synthesis block is placed in a cubic press, the pressure is increased from 0GPa to 5.7GPa within 3 hours, the power is increased from 0kw to 5.5-6.5 kw and then synthesized for 5-6 days, after the synthesis is finished, the power is reduced to 0kw within 1 hour and the pressure is reduced to 0GPa within 2 hours, and then the synthesis block is taken out;
and breaking the taken-out diamond synthesis block to obtain a sintered synthesis column, putting the synthesis column into a beaker filled with 35-38 wt% hydrochloric acid solution, and heating the beaker on an electric furnace at 200 ℃ until the alloy completely reacts and falls off to expose the diamond, thus obtaining the diamond.
The diamond prepared by the embodiment is 1-1.2 carats.
Example 4
The diamond synthesis block provided in this example is referred to example 2, in which the shape and size of each structure are as follows;
an upper cover 1: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 7 mm; the height of the cavity is 10 mm;
a lower cover 3: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 7 mm; the height of the cavity is 10 mm;
and (3) a female cavity 2: a porous (sub-cavity) cylinder 26mm in height and 57mm in diameter; the diameter of the sub-cavity 21 is 7mm, and the height of the sub-cavity 21 is 26 mm;
upper insulating plug 211: a cylinder with a height of 7mm and a diameter of 5 mm;
carbon source 212: a cylinder with a height of 6mm and a diameter of 7 mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 7 mm;
the copper sheet 214: a wafer with the thickness of 0.05mm and the diameter of 7 mm;
a crystal bed 215: a cylinder with a height of 5mm and a diameter of 7 mm;
first heat-conductive pillar 111: a cylinder with a height of 10mm and a diameter of 7 mm;
second heat-conductive pillar 311: a cylinder with a height of 10mm and a diameter of 7 mm;
a first graphite sheet: a disc with a diameter of 59 mm;
a second graphite sheet; a disc having a diameter of 59 mm;
a graphite heating pipe: the graphite pipe is 46mm in height, 59mm in outer diameter and 1mm in pipe wall thickness;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner bore diameter (dimension after insertion of the dolomite liner) of 59 mm; the thickness of the dolomite lining is 3 mm.
The method for preparing diamond improved by the implementation is referred to as example 3, and the difference is that the synthesis time is 5-7 days.
The diamond prepared by the embodiment is 3-3.5 carats.
Example 5
The diamond synthesis block provided in this example is referred to example 2, in which the shape and size of each structure are as follows;
an upper cover 1: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 9 mm; the height of the cavity is 10 mm;
a lower cover 3: the cylinder is 10mm in height and 57mm in diameter and comprises a plurality of cylindrical cavities; the diameter of the cavity is 9 mm; the height of the cavity is 10 mm;
and (3) a female cavity 2: a porous (sub-cavity) cylinder 26mm in height and 57mm in diameter; the diameter of the sub-cavity 21 is 5mm, and the height of the sub-cavity 21 is 26 mm;
upper insulating plug 211: a cylinder with a height of 5mm and a diameter of 9 mm;
carbon source 212: a cylinder with a height of 6mm and a diameter of 9 mm;
catalyst 213: a cylinder with a height of 10mm and a diameter of 9 mm;
the copper sheets 214: a wafer with the thickness of 0.05mm and the diameter of 9 mm;
a crystal bed 215: a cylinder with a height of 5mm and a diameter of 9 mm;
first heat-conductive column 11: a cylinder with a height of 10mm and a diameter of 9 mm;
second heat-conductive pillar 31: a cylinder with a height of 10mm and a diameter of 9 mm;
a first graphite sheet: a disc having a diameter of 59 mm;
a second graphite sheet; a disc having a diameter of 59 mm;
a graphite heating pipe: the graphite pipe is 46mm in height, 59mm in outer diameter and 1mm in pipe wall thickness;
pyrophyllite block 5: a cylinder with a height of 74mm and an inner bore diameter (dimension after insertion of the dolomite liner) of 59 mm; the thickness of the dolomite lining is 3 mm.
The method for preparing diamond improved by the implementation is referred to as example 3, and the difference is that the synthesis time is 5-8 days.
The diamond prepared by the embodiment is 5-6 carats.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A diamond synthesis block is characterized by comprising a diamond synthesis cavity;
the diamond synthesis cavity comprises an upper cover, a mother 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 first heat-conducting columns are arranged in the cavities of the upper cover;
the lower cover is provided with a plurality of cavities, and second heat-conducting columns are arranged in the cavities of the lower cover;
a plurality of sub-cavities are arranged in the mother cavity;
an upper insulating plug, a carbon source, a catalyst, a copper sheet and a crystal bed which are connected in sequence are arranged in the sub-cavity.
2. The diamond synthesis block of claim 1, further comprising a first conductive steel cap, a second conductive steel cap, a first heater plate, a second heater plate, and a heating tube;
the first heating sheet and the second heating sheet are arranged on two sides of the heating pipe; the first heating sheet, the second heating sheet and the heating pipe are enclosed to form an accommodating cavity, and the diamond synthesis cavity is placed in the accommodating cavity;
the first conductive steel cap is connected with the first heating sheet;
the first heating sheet is connected with the upper cover;
the second conductive steel cap is connected with the second heating sheet;
the second heating plate is connected with the lower cover.
3. The diamond composite block of claim 2, further comprising a first pyrophyllite ring, a second pyrophyllite ring, a first block ring, a second block ring, a liner, and a pyrophyllite block;
the first heating plate is connected with the first blocking 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 blocking ring and the first pyrophyllite ring;
the second heating plate is connected with the second plugging 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 inner liner; the inner liner is connected with the heating pipe.
4. The diamond synthesis block of claim 1, wherein the upper cap is connected to the upper insulating plug;
preferably, the lower cover is connected with the crystal bed;
preferably, a seed crystal is arranged in the crystal bed;
preferably, the number of the cavities of the upper cover and the number of the sub-cavities are the same as the number of the cavities of the lower cover.
5. The diamond composite block of claim 1, wherein the upper cover comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide;
preferably, the lower cover comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide;
preferably, the mother cavity comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide.
6. The diamond synthesis block of claim 1, wherein the upper insulating plug comprises the following components in parts by weight: 65-80 parts of sodium chloride and 20-35 parts of zirconium oxide;
preferably, the carbon source 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 bed comprises a bed of magnesium oxide crystals;
preferably, the preparation method of the crystal bed comprises the following steps: calcining the magnesium oxide with the purity of more than or equal to 99.5% at 1100-1500 ℃ for 2-5 h, and then pressing and forming.
7. The diamond synthesis block of claim 1, wherein 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, 1-3 parts of Cu and 0.004-0.008 parts 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;
preferably, the preparation method of the catalyst comprises: preparing various alloy components according to the components of the catalyst, smelting at 1650-1750 ℃, cooling, cutting and forming.
8. The diamond synthesis block of claim 1, wherein the first thermally conductive pillar comprises, in parts by weight: 5-10 parts of magnesium oxide and/or zirconium oxide and 90-95 parts of sodium chloride;
preferably, 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.
9. The diamond synthesis block of claim 2, wherein the first heating plate comprises one or more of graphite, silicon carbide, and magnesium;
preferably, the second heating sheet comprises one or more of graphite, silicon carbide and magnesium;
preferably, the heating tube comprises one or more of graphite, silicon carbide and magnesium.
10. A method for preparing diamond is characterized by comprising the following steps:
synthesizing the dried diamond synthesis block according to any one of claims 1 to 9 under the conditions of pressure of 5.5 to 6GPa and power of 5 to 7kw for 5 to 10 days, and taking out after the synthesis is completed;
preferably, the dried diamond synthesis 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 and then the diamond synthesis block is synthesized for 5-10 days, and the diamond synthesis block is taken out after synthesis.
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