CN107188166B - Pyramid-shaped artificial diamond and preparation method thereof - Google Patents
Pyramid-shaped artificial diamond and preparation method thereof Download PDFInfo
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- CN107188166B CN107188166B CN201710497298.5A CN201710497298A CN107188166B CN 107188166 B CN107188166 B CN 107188166B CN 201710497298 A CN201710497298 A CN 201710497298A CN 107188166 B CN107188166 B CN 107188166B
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- 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
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
Abstract
The invention discloses a pyramid-shaped artificial diamond and a preparation method thereof, wherein the pyramid-shaped artificial diamond is prepared from the following raw materials: 40-75g of graphite rod core and 20-50g of catalyst sheet; wherein, the catalyst sheet comprises the following components in percentage by weight: 45-70% of nickel powder, 10-30% of iron powder and 5-10% of cobalt powder; the manufacturing method has the advantages of simple and feasible method, simple and convenient operation, simple formula, simple synthesis block structure, and well-controlled and well-regulated synthesis process, the pyramid-shaped diamond crystal form synthesized by the method is in a four-sided pyramid shape, and is favorable for polishing into a round diamond shape with 24-sided taper, the diamond crystal form has good transparency, is glittering and translucent, the color of the diamond is transparent, the polished color of fire is good, the particles are large, and the round diamond yield is up to 48 percent when the pyramid-shaped diamond is polished and processed into the round diamond shape.
Description
Technical Field
The invention relates to the technical field of artificial diamonds, in particular to a pyramid-shaped artificial true diamond and a manufacturing method thereof, which are suitable for jewelry, artware and ornaments.
Background
Graphite grows into diamond under the conditions of high pressure and high temperature; in the prior art, the generated diamonds are all oval or square, however, in the actual production and processing, the yield of the oval diamonds processed into the diamond shape is only about 30%, the pyramid-shaped diamonds are more suitable for processing and forming, the diamonds can be used as artware and ornaments, the processing difficulty is high, the yield is low, and no method for directly synthesizing the diamonds with the pyramid structures exists at present.
At present, diamond is prepared by a chemical vapor deposition method, the shape is square, and the yield is not high. In addition, the diamond prepared by the high-temperature high-pressure method is used for diamond rings, and people prefer large diamond with high yield in life.
Disclosure of Invention
The invention aims to provide a pyramid artificial real diamond and a preparation method thereof, the method has the advantages of simple and easy operation, simple formula, simple structure of a synthesis block, good adjustment of synthesis process, good blank shape and large particles of the synthesized pyramid diamond, less grinding part of a conical surface when the pyramid diamond is ground into a round diamond shape, short grinding time and high yield of the round diamond up to 48 percent.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a pyramid-shaped artificial diamond is prepared from the following raw materials:
raw material weight portion
40-75g graphite chip
20-50g of catalyst pieces;
the catalyst sheet comprises the following components in parts by weight:
preferably, the pyramid-shaped artificial diamond is prepared from the following raw materials:
raw material weight portion
Graphite chip 45-70g
25-45g of catalyst pieces;
the catalyst sheet comprises the following components in parts by weight: 20-30 parts of nickel powder, 10-20 parts of iron powder and 5-9 parts of cobalt powder.
More preferably, the pyramid-shaped artificial diamond is prepared from the following raw materials:
raw material weight portion
Graphite chip 50-65g
30-42g of catalyst pieces;
the catalyst sheet comprises the following components in parts by weight: 25-30 parts of nickel powder, 18-22 parts of iron powder and 6-8 parts of cobalt powder.
Further preferably, the pyramid-shaped artificial diamond is prepared from the following raw materials:
raw material weight portion
55-60g of graphite chip
34-38g of catalyst pieces;
the catalyst sheet comprises the following components in parts by weight: 19-21 parts of nickel powder, 20-18 parts of iron powder and 6.5-7.5 parts of cobalt powder.
Most preferably, the pyramid-shaped artificial diamond is prepared from the following raw materials:
raw material weight portion
Graphite chip 65g
35g of catalyst pieces;
the catalyst sheet comprises the following components in parts by weight: 10 parts of nickel powder, 20 parts of iron powder and 5 parts of cobalt powder.
In addition, the invention also provides a preparation method of the pyramid-shaped artificial diamond, which comprises the following steps:
A. preparing a graphite rod core, and stamping natural graphite into round pieces with the thickness of 1 mm;
B. mixing nickel powder, iron powder and cobalt powder according to a proportion to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting the graphite rod core with a catalyst sheet, and connecting the catalyst sheet with dolomite embedded with diamond seeds and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, uniformly boosting the pressure to 32-35MPa within 1-90 seconds, and simultaneously raising the temperature to 300 ℃; then increasing the pressure to 81MPa at a constant speed within 320 seconds of 300-; the temperature is 1000-1050 ℃, and the pressure is 81-83 Mpa; and then, starting first cooling at 800 ℃ under the pressure of 70MPa for 28-32 seconds, then carrying out second uniform cooling at 600 ℃ under the pressure of 40MPa for 22-26 minutes, then carrying out third uniform cooling at 100 ℃ under the pressure of 10MPa, and stopping the machine after the temperature is kept for 28-32 minutes and the pressure is reduced to 0MPa to obtain the synthetic pyramid-shaped diamond.
Wherein the diamond seed crystal is a six-octahedral artificial diamond with a complete crystal form.
The synthesis auxiliary part consists of a dolomite cup, a dolomite tube, a heating tube, a plug with dolomite, an iron sheet, a graphite heating sheet, a dolomite cushion block and a pyrophyllite block; wherein the graphite rod core, the catalyst sheet and the dolomite embedded with the diamond seed crystal form a synthetic column; a dolomite cup is sleeved outside the synthetic column, the upper end of the dolomite cup is connected with a graphite heating sheet, and the graphite heating sheet is connected with an iron sheet; the lower end of the dolomite cup is connected with a dolomite cushion block, the dolomite cushion block is connected with a graphite heating sheet, the graphite heating sheet is connected with an iron sheet, a dolomite tube is sleeved outside the whole connection, a heating tube is sleeved outside the dolomite tube, the two ends of the heating tube are connected with plugs, and pyrophyllite blocks are sleeved outside the heating tube.
Compared with the prior art, the invention has the advantages that:
(1) the manufacturing method has the advantages of simple and feasible method, simple and convenient operation, simple formula, simple structure of the synthesis block, and good control and regulation of the synthesis process, the crystal form of the pyramid diamond synthesized by the invention is in a four-sided pyramid shape, and is beneficial to polishing into a round diamond shape with 24-sided taper, the crystal form of the diamond has good transparency, crystal clearness and bright color, the polished crystal has good fire color and large particles, and when the pyramid diamond is polished and processed into the round diamond shape, the round diamond yield reaches 48%;
(2) the invention solves the problems of small diamond particles with diameters of 0.5-5mm, irregular shapes, poor transparency, large polishing difficulty and the like in the prior art, and the technical scheme of the invention is mainly different from the prior art in that the synthesis adopts slow temperature rise and slow pressure rise and constant temperature and constant pressure synthesis, the diameter of the synthesized diamond blank particles is 5-10mm, the diamond blank is in a pyramid shape, the crystal form transparency is good, the diamond is crystal clear, the color of the diamond is transparent, the cleanliness after polishing is high, the fire color is good, and the particles are large.
Drawings
FIG. 1 is a schematic diagram of a synthetic block assembled by graphite chips, catalyst sheets, diamond seed crystals and auxiliary synthetic components.
Fig. 2 is a schematic diagram of a photograph of the diamond produced in example 2.
Fig. 3 is a schematic diagram of a photograph of the diamond produced in example 1.
Detailed Description
The invention is further illustrated by the following examples:
example 1
A pyramidal artificial diamond, which is prepared from the following raw materials by mass:
a method for preparing pyramid artificial real diamond comprises the following steps:
A. preparing a graphite chip; stamping natural graphite into 1mm round pieces;
B. mixing nickel powder, iron powder and cobalt powder according to a certain weight ratio to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 65g of graphite chip with 35g of catalyst sheet, wherein the graphite chip is arranged on the upper part, the three layers of catalyst sheets are arranged on the lower part, and the catalyst sheets are connected with dolomite embedded with diamond seeds and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, uniformly increasing the pressure to 34MPa within 45 seconds, and simultaneously increasing the temperature to 300 ℃; then increasing the pressure to 81MPa at a constant speed within 310 seconds, increasing the temperature to 1000 ℃ at a constant speed, then keeping the temperature and the constant pressure for 120 hours, wherein the temperature is 1000 ℃ and the pressure is 82 MPa; and then, starting first cooling, wherein the temperature is 800 ℃, the pressure is 70MPa, the first cooling time is 30 seconds, then carrying out second uniform cooling, the temperature is 600 ℃, the pressure is 40MPa, the cooling time is 24 minutes, then carrying out third uniform cooling, the temperature is 100 ℃, the pressure is 10MPa, keeping the temperature for 30 minutes, stopping the machine after the pressure is reduced to 0MPa, and obtaining the synthetic pyramid-shaped diamond, wherein the diameter of a diamond blank is 5-10mm, the transparency is good, and the color is good.
Example 2:
a method for preparing pyramid artificial real diamond comprises the following steps:
A. preparing a graphite chip; stamping natural graphite into 1mm round pieces;
B. mixing 55 parts by weight of nickel powder, 30 parts by weight of iron powder and 15 parts by weight of cobalt powder to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 68 g of graphite chip with 32 g of catalyst sheet, and connecting the catalyst sheet with dolomite embedded with diamond seed crystals and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, averagely boosting the pressure to 33MPa in 50 seconds, boosting the pressure at a constant speed to 82.5MPa in 300 seconds, and maintaining the pressure at a constant temperature and a constant pressure for 24 hours; meanwhile, within 24 hours and 90 seconds, starting to heat up from 30 seconds, wherein the heating process is 300 seconds, uniformly heating up to 5.6kw, then keeping the constant temperature for 300 seconds, then starting to cool down for the first time, the first cooling time is 30 seconds, cooling down to 5kw, then performing uniform cooling for the second time, the cooling time is 24 minutes, uniformly cooling down to 4kw, and stopping the machine after keeping the temperature for 30 minutes; the synthetic oval diamond is obtained, the diameter of a diamond blank is 0.5-2mm, the transparency is poor, and the color difference is poor.
Example 3:
a method for preparing pyramid artificial real diamond comprises the following steps:
A. preparing a graphite chip; stamping natural graphite into 1mm round pieces;
B. mixing 58 parts by weight of nickel powder, 32 parts by weight of iron powder and 10 parts by weight of cobalt powder to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 64 g of graphite rod core with 36 g of catalyst sheet, and connecting the catalyst sheet with dolomite embedded with diamond seeds and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, averagely boosting the pressure to 33MPa in 30 seconds, boosting the pressure at a constant speed to 82.5MPa in 300 seconds, and maintaining the pressure at a constant temperature and a constant pressure for 24 hours; meanwhile, within 24 hours and 90 seconds, the temperature is raised from 30 seconds, the temperature raising process is 300 seconds, the temperature is raised to 5.6kw at a constant speed, then the constant temperature is kept for 300 seconds, then the first temperature reduction is started, the first temperature reduction time is 30 seconds and is reduced to 5kw, then the second temperature reduction is carried out at a constant speed, the temperature reduction time is 24 minutes, the temperature reduction is carried out at a constant speed to 4kw, the machine is stopped after the temperature is kept for 30 minutes, and the synthetic oval diamond is obtained, wherein the diameter of a diamond blank is 1-2.5mm, the transparency is poor, and the color difference is poor.
Example 4:
a method for preparing pyramid artificial real diamond comprises the following steps:
A. preparing a graphite chip; stamping natural graphite into a round sheet with the thickness of 1 mm;
B. mixing 61 parts by weight of nickel powder, 34 parts by weight of iron powder and 5 parts by weight of cobalt powder to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 62 g of graphite chip with 38g of catalyst piece, and connecting the catalyst piece with dolomite embedded with diamond seed crystals and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, averagely boosting the pressure to 33MPa in 60 seconds, boosting the pressure at a constant speed to 82.5MPa in 300 seconds, and maintaining the pressure at a constant temperature and a constant pressure for 24 hours; meanwhile, within 24 hours and 90 seconds, the temperature is increased from 30 seconds, the temperature is increased to 5.6kw at a constant speed within 300 seconds, then the temperature is kept constant for 300 seconds, then the temperature is decreased for the first time, the first temperature is decreased for 30 seconds to 5kw, then the temperature is decreased at a constant speed for the second time, the temperature is decreased for 24 minutes,cooling to 4kw at constant speed, keeping the temperature for 30 minutes, and stopping the machine to obtain the synthetic oval diamond, wherein the diameter of the diamond blank is 1-3mm, the transparency is poor, and the color difference is poor.
Example 5:
a method for preparing pyramid artificial real diamond comprises the following steps:
A. preparing a graphite chip; stamping natural graphite into a round sheet with the thickness of 1 mm;
B. mixing 62 parts by weight of nickel powder, 35 parts by weight of iron powder and 3 parts by weight of cobalt powder to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 65g of graphite rod core with 35g of catalyst sheet, and connecting the catalyst sheet with dolomite embedded with diamond seed crystals and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, averagely boosting the pressure to 33MPa in 90 seconds, boosting the pressure at a constant speed to 82.5MPa in 300 seconds, and maintaining the pressure at a constant temperature and a constant pressure for 24 hours; meanwhile, within 24 hours and 90 seconds, the temperature is raised from 30 seconds, the temperature raising process is 300 seconds, the temperature is raised to 5.6kw at a constant speed, then the constant temperature is kept for 300 seconds, then the first temperature reduction is started, the first temperature reduction time is 30 seconds and is reduced to 5kw, then the second temperature reduction is carried out at a constant speed, the temperature reduction time is 24 minutes, the temperature reduction is carried out at a constant speed to 4kw, the machine is stopped after the temperature is kept for 30 minutes, and the synthetic oval diamond is obtained, wherein the diameter of a diamond blank is 0.5-2mm, the transparency is general, and the color is good.
The diamonds prepared in each example were subjected to a related performance test, the results of which are shown in table 1:
it should be noted that the above-described embodiments may enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. Thus, it will be appreciated by those skilled in the art that the invention may be modified and equivalents may be substituted; all technical solutions and modifications thereof which do not depart from the spirit and technical essence of the present invention should be covered by the scope of the present patent.
Claims (3)
1. A pyramidal synthetic diamond, made from the following raw materials:
graphite rod core 65g
35g of catalyst pieces;
wherein, the catalyst sheet comprises the following components in percentage by weight:
10g of nickel powder, namely 10g of nickel powder,
20g of iron powder is added into the reaction kettle,
5g of cobalt powder.
2. A method of making the pyramidal synthetic diamond of claim 1, comprising the steps of:
A. preparing a graphite chip; stamping natural graphite into 1mm round pieces;
B. mixing nickel powder, iron powder and cobalt powder according to a certain weight ratio to obtain a mixture, pouring and casting the mixture, smelting, and pressing into a round sheet with the thickness of 0.2mm to obtain a catalyst sheet;
C. connecting 65g of graphite chip with 35g of catalyst sheet, wherein the graphite chip is arranged on the upper part, the three layers of catalyst sheets are arranged on the lower part, and the catalyst sheets are connected with dolomite embedded with diamond seeds and a synthesis accessory to assemble a synthesis block;
D. placing the synthesized block onPressing and synthesizing in a cubic diamond synthesizing press, uniformly increasing the pressure to 34MPa within 45 seconds, and simultaneously increasing the temperature to 300 ℃; then raising the pressure to 81MPa at a constant speed within 310 seconds, raising the temperature at a constant speed to 1000 ℃, and then keeping the temperature and the constant pressure for 120 hoursThe temperature is 1000 ℃, and the pressure is 82 Mpa; and then, starting first cooling, wherein the temperature is 800 ℃, the pressure is 70MPa, the first cooling time is 30 seconds, then carrying out second uniform cooling, the temperature is 600 ℃, the pressure is 40MPa, the cooling time is 24 minutes, then carrying out third uniform cooling, the temperature is 100 ℃, the pressure is 10MPa, keeping the temperature for 30 minutes, stopping the machine after the pressure is reduced to 0MPa, and obtaining the synthetic pyramid-shaped diamond, wherein the diameter of a diamond blank is 5-10mm, the transparency is good, and the color is good.
3. The method of claim 2, wherein the synthetic auxiliary consists of a dolomite cup, a dolomite tube, a heating tube, a plug with dolomite, an iron sheet, a graphite heating sheet, a dolomite spacer, a pyrophyllite block; wherein the graphite rod core, the catalyst sheet and the dolomite embedded with the diamond seed crystal form a synthetic column; a dolomite cup is sleeved outside the synthetic column, the upper end of the dolomite cup is connected with a graphite heating sheet, and the graphite heating sheet is connected with an iron sheet; the lower end of the dolomite cup is connected with a dolomite cushion block, the dolomite cushion block is connected with a graphite heating sheet, the graphite heating sheet is connected with an iron sheet, a dolomite tube is sleeved outside the whole connection, a heating tube is sleeved outside the dolomite tube, the two ends of the heating tube are connected with plugs, and pyrophyllite blocks are sleeved outside the heating tube.
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| CN111763986A (en) * | 2020-07-08 | 2020-10-13 | 彭伟华 | Method for preparing diamond |
| CN115739100B (en) * | 2022-12-14 | 2024-02-06 | 佳睿福钻石(河南)有限公司 | Spontaneous nucleation white diamond catalyst and apparatus for producing thereof |
Citations (4)
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|---|---|---|---|---|
| CN1686611A (en) * | 2005-02-25 | 2005-10-26 | 江苏工业学院 | Powdered catalyst for synthesizing diamond containing oxide |
| CN102580618A (en) * | 2012-01-13 | 2012-07-18 | 河南省联合磨料磨具有限公司 | Protogenic diamond fine particle for precisio machining and production method thereof |
| CN103097011A (en) * | 2009-01-16 | 2013-05-08 | 六号元素有限公司 | High pressure high temperature (HPHT) method for the production of single crystal diamonds |
| WO2013156537A1 (en) * | 2012-04-19 | 2013-10-24 | Element Six Limited | Synthetic diamond crystals |
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- 2017-06-26 CN CN201710497298.5A patent/CN107188166B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686611A (en) * | 2005-02-25 | 2005-10-26 | 江苏工业学院 | Powdered catalyst for synthesizing diamond containing oxide |
| CN103097011A (en) * | 2009-01-16 | 2013-05-08 | 六号元素有限公司 | High pressure high temperature (HPHT) method for the production of single crystal diamonds |
| CN102580618A (en) * | 2012-01-13 | 2012-07-18 | 河南省联合磨料磨具有限公司 | Protogenic diamond fine particle for precisio machining and production method thereof |
| WO2013156537A1 (en) * | 2012-04-19 | 2013-10-24 | Element Six Limited | Synthetic diamond crystals |
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Denomination of invention: A kind of pyramid-shaped artificial diamond and preparation method thereof Effective date of registration: 20220815 Granted publication date: 20191224 Pledgee: Bank of China Limited Ezhou branch Pledgor: Believe diamond new material limited liability company in Hubei Province Registration number: Y2022420000257 |
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