CN115041100B - Multilayer infiltration type structure large particle single crystal cultivation diamond synthetic block and preparation process thereof - Google Patents
Multilayer infiltration type structure large particle single crystal cultivation diamond synthetic block and preparation process thereof Download PDFInfo
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- CN115041100B CN115041100B CN202210868146.2A CN202210868146A CN115041100B CN 115041100 B CN115041100 B CN 115041100B CN 202210868146 A CN202210868146 A CN 202210868146A CN 115041100 B CN115041100 B CN 115041100B
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- 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
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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
- B01J3/065—Presses for the formation of diamonds or boronitrides
- B01J3/067—Presses using a plurality of pressing members working in different directions
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Abstract
The invention discloses a large-particle single crystal cultivation diamond synthetic block with a multilayer permeable structure and a preparation process thereof, wherein the diamond synthetic block comprises columnar hollow pyrophyllite blocks, pyrophyllite rings and dolomite rings are sequentially distributed at two ends of each pyrophyllite block along the radial direction from outside to inside, a conductive steel ring is further arranged at the annular part of each dolomite ring, the multilayer permeable structure synthetic block is adopted to replace the traditional sheet-shaped structure, the problem of poor surface layer purity in the later stage of high-temperature high-pressure large-particle single crystal synthesis growth is optimally improved, the controllable preparation of the growth speed of the large-particle single crystal cultivation diamond is realized, the single crystal form is a complete standard octahedron {111} and cube {100} aggregate, the inside of the single crystal form can reach over vs grade, the color can reach to optimal white grade, the stable synthesis can completely meet the industrialized production conditions.
Description
Technical Field
The invention belongs to the technical field of diamond cultivation by a high-temperature high-pressure method, and particularly relates to a large-particle single crystal cultivation diamond synthesis block with a multilayer permeable structure and a preparation process thereof.
Background
The physical and chemical properties of the cultivated diamond are identical to those of natural diamond, so that the cultivated diamond is gradually a new choice for diamond consumption. The cultured diamond product can be compared with natural diamond in the aspects of crystal structure integrity, transparency, refractive index, chromatic dispersion and the like, and can be widely used for manufacturing various ornaments such as diamond rings, necklaces, earrings, clothes and the like and other fashion consumer goods. At present, the permeability of the cultivated diamond is still very low, the quality of the diamond is improved along with the progress of the cultivation technology, and the consumption concept is changed, so that the cultivated diamond not only can replace natural diamond, but also can be popularized to more application scenes which are not popularized by the original natural diamond, more market demands are stimulated, and a wide space is available in the future.
The weight of high quality, programmable, carat-grade grown diamond single crystals increases by a factor of its commercial value. At present, the commercial development and application of the cultivated diamond in China are high-temperature high-pressure method synthetic cultivated diamond, wherein the cultivated diamond with the synthetic blank of 3-10 carats is a mainstream technology of various manufacturers of cultivated diamond, the large-particle single crystal technology with the weight of the synthetic blank exceeding 10 carats is still immature, the quality and the purity of the synthetic diamond are difficult to control stably, and the market popularization and application are impossible.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a large-particle single crystal cultivation diamond synthetic block with a multilayer infiltration structure and a preparation process thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a multilayer infiltration type large-particle single crystal cultivation diamond synthetic block comprises a columnar hollow pyrophyllite block, wherein pyrophyllite rings and dolomite rings are sequentially distributed at two end parts of the pyrophyllite block from outside to inside along the radial direction, and a conductive steel ring is also arranged at the annular center part of the dolomite;
the inner side of the pyrophyllite block is further sequentially provided with a dolomite outer lining, a carbon tube, a magnesium ring and an inner composite body from outside to inside along the radial direction, the two axial ends of the inner composite body are further sequentially provided with carbon paper and heat preservation sheets, the carbon paper is arranged on the inner wall of the conductive steel ring and extends to be paved on the dolomite outer lining, and the heat preservation sheets are arranged on the inner side of the carbon paper and extend to be paved on the carbon tube;
the internal synthesis body comprises a first carbon source sheet, a first composite catalyst column and a crystal bed which are sequentially laminated and laid along the axial direction, a containing cavity is formed in the first composite catalyst column, a second carbon source sheet and a second composite catalyst column are arranged in the containing cavity, and the second composite catalyst column is in contact with the crystal bed;
seed crystals are also arranged at the inner wall core part of the crystal bed.
The first composite catalyst column is of a hollow cylindrical structure, and the inner surface of the first composite catalyst column is coated with an aluminum film; the second composite catalyst column is of a columnar structure, and an aluminum film is coated on the second composite catalyst column.
The first carbon source sheet and the second carbon source sheet are high-purity graphite sheets for cultivating diamonds.
The purity of the high-purity graphite flake is 99.99%.
The first composite catalyst column comprises the following components in percentage by weight: 70.0% -83.0% of high-purity iron powder, 7.0% -15.0% of nickel powder, 12.0% -25.0% of cobalt powder and 0.8% -1.8% of aluminum powder, wherein the purity of the high-purity iron powder is 99.9%, the granularity of the nickel powder is 200-300 meshes, and the granularity of the cobalt powder is 200-300 meshes.
The second composite catalyst column comprises the following components in percentage by weight: 63.0 to 76.0 percent of high-purity iron powder, 3.0 to 10.0 percent of nickel powder, 15.0 to 28.0 percent of cobalt powder, 4.0 to 12.0 percent of manganese powder and 0.3 to 1.1 percent of aluminum powder, wherein the purity of the high-purity iron powder is 99.9 percent, the granularity of the nickel powder is 300 to 400 meshes, the granularity of the cobalt powder is 300 to 400 meshes, and the granularity of the manganese powder is 300 to 400 meshes.
The granularity of the aluminum powder is 50nm.
The seed crystal adopts hexa-octahedral high-temperature high-pressure diamond.
The preparation process of the multilayer infiltration type structure large particle single crystal cultivation diamond synthetic block comprises the following steps:
(1) Placing the synthesized block in a synthesis cavity of a hexahedral top press, uniformly boosting the pressure to 50-62MPa in 30-100 seconds, and keeping the constant pressure for 1000-5000 seconds;
(2) Boosting the pressure to 65-75MPa again at a constant speed for 30-100 seconds, and then boosting the pressure to 80-90MPa at a constant speed for 20-48 hours;
(3) Boosting the pressure to 95-105MPa at a constant speed for 60-96 hours, and keeping the pressure at a constant pressure for 130-165 hours;
(4) Heating when the pressure is increased to 20-40MPa, heating to 1330-1430 ℃ at a constant speed for 200-600 seconds, preserving heat for 1000-5000 seconds, then cooling for the first time, cooling to 1280-1320 ℃ at a constant speed for 20-48 hours, and preserving heat for 60-80 hours;
and then cooling for the second time, cooling to 1150-1270 ℃ at a constant speed for 130-165 hours, and finally finishing the synchronous with the pressure time to obtain the large-particle cultivated diamond.
In the step (1), the synthetic block is placed in a synthetic cavity of a hexahedral press, and is uniformly boosted to 58MPa and kept at constant pressure for 30min;
step (2) is carried out for 1min to uniformly boost the pressure to 68MPa again, and then 36h is carried out to uniformly boost the pressure to 15MPa, namely to 83MPa;
step (3) is to boost the pressure to 100MPa at a constant speed for 72 hours, and keep the pressure for 145 hours at a constant pressure;
in the step (4), when the pressure is increased to 30MPa, heating to 1350 ℃ at a constant speed for 350s, preserving heat for 2000s, then cooling to 50 ℃ at a constant speed for 36h, namely cooling to 1300 ℃, and preserving heat for 72h; and then cooling again, and cooling at a constant speed for 145h to 50 ℃, namely cooling to 1250 ℃, and finally finishing the synchronous with the pressure time to obtain the large-particle cultivated diamond.
The beneficial effects of the invention are as follows:
the multilayer infiltration type structure large-particle single crystal cultivation diamond synthesis block and the preparation process thereof adopt the multilayer infiltration type structure synthesis block to replace the traditional sheet structure, optimize and improve the problem of poor surface layer purity in the later stage of high-temperature and high-pressure large-particle single crystal synthesis growth, realize controllable preparation of the growth speed of the large-particle single crystal cultivation diamond, and the crystal form of the single crystal is a complete standard octahedron {111} and cube {100} aggregation, the internal purity can reach over vs grade, the color can reach excellent white grade, the stable synthesis can be realized, and the industrialized production condition can be completely satisfied.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a process graph of the present invention;
reference numerals illustrate:
1. the composite pyrophyllite comprises a pyrophyllite composite block, 2, a pyrophyllite ring, 3, yun Danhuan, 4, a conductive steel ring, 5, a dolomite outer lining, 6, carbon paper, 7, a carbon tube, 8, a magnesium cup, 9, a heat preservation sheet, 10, a crystal bed, 11, a first carbon source sheet, 12, a first composite catalyst column, 13, a second carbon source sheet, 14, a second composite catalyst column, 15 and seed crystals.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
The invention provides a large-particle single crystal cultivation diamond synthetic block with a multilayer penetrating structure, which is shown in fig. 1 and 2.
The multi-layer infiltration type structure large-particle single crystal cultivation diamond synthetic block comprises a columnar hollow pyrophyllite block 1, wherein pyrophyllite rings 2 and dolomite rings 3 are sequentially distributed at two end parts of the pyrophyllite block 1 from outside to inside along the radial direction, and a conductive steel ring 4 is also arranged at the center part of the dolomite ring 3;
the inner side of the pyrophyllite block 1 is further sequentially provided with a dolomite outer lining 5, a carbon tube 7, a magnesium ring 8 and an inner composite body from outside to inside along the radial direction, the two axial ends of the inner composite body are further sequentially provided with carbon paper 6 and heat preservation sheets 9, the carbon paper 6 is arranged on the inner wall of the conductive steel ring 4 and extends to be paved on the dolomite outer lining 5, and the heat preservation sheets 9 are arranged on the inner side of the carbon paper 6 and extend to be paved on the carbon tube 7;
the inner synthesis body comprises a first carbon source sheet 11, a first composite catalyst column 12 and a crystal bed which are sequentially laminated and laid along the axial direction, a containing cavity is formed in the first composite catalyst column 12, a second carbon source sheet 13 and a second composite catalyst column 14 are correspondingly arranged in the containing cavity, and the second composite catalyst column 14 is in contact with the crystal bed 10;
seed crystals 15 are further arranged at the inner wall center of the crystal bed 10, and the seed crystals are hexa-octahedral high-temperature high-pressure diamond, wherein the diamond size is 1.6 mm-3.2 mm.
The first composite catalyst column 12 is provided with a hollow cylindrical structure, and the inner surface of the first composite catalyst column is coated with an aluminum film.
The second composite catalyst column 14 is formed in a columnar structure, and is coated with an aluminum film on the outside thereof.
The first carbon source sheet 11 and the second carbon source sheet 13 are high-purity graphite sheets special for diamond cultivation, and the purity of the high-purity graphite sheets is 99.99%.
The first composite catalyst column 12 comprises the following components in percentage by weight: 70.0% -83.0% of high-purity iron powder, 7.0% -15.0% of nickel powder, 12.0% -25.0% of cobalt powder and 0.8% -1.8% of aluminum powder, wherein the purity of the high-purity iron powder is 99.9%, the granularity of the nickel powder is 200-300 meshes, the granularity of the cobalt powder is 200-300 meshes, the granularity of the aluminum powder is 50nm, in the embodiment, the outer diameter of the first composite catalyst column 12 is 50mm, the height is 44mm, the inner diameter of a containing cavity is 30mm, and the height is 28mm; the iron powder, the nickel powder and the cobalt powder are pressed into a hollow cylindrical structure with a containing cavity after the procedures of mixing, granulating, reducing and passivating, and an aluminum film is coated on the surface of the first composite catalyst column in a vacuum environment.
The second composite catalyst column 14 comprises the following components in percentage by weight: 63.0% -76.0% of high-purity iron powder, 3.0% -10.0% of nickel powder, 15.0% -28.0% of cobalt powder, 4.0% -12.0% of manganese powder and 0.3% -1.1% of aluminum powder, wherein the purity of the high-purity iron powder is 99.9%, the granularity of the nickel powder is 300-400 meshes, the granularity of the cobalt powder is 300-400 meshes and the granularity of the manganese powder is 300-400 meshes, the granularity of the aluminum powder is 50nm, and in the embodiment, the diameter of the second composite catalyst column 14 is 30mm, and the height is 25mm; the iron powder, the nickel powder and the cobalt powder are pressed into a columnar structure after the procedures of mixing, granulating, reducing and passivating, and an aluminum film is coated on the surface of the second composite catalyst column in a vacuum environment.
The technical scheme of the diamond preparation and cultivation process is as follows:
placing the synthetic block of the raw material proportioning scheme in a synthesis cavity of a hexahedral top press, firstly, adopting 30-100 seconds to uniformly boost the pressure to 50-62MPa, then keeping the pressure for 1000-5000 seconds at constant pressure, and fully melting and uniformly mixing a second composite catalyst column in a low-pressure high-temperature state; then the pressure is increased to 65-75MPa at a constant speed in 30-100 seconds, and then the pressure is increased to 80-90MPa at a constant speed in 20-48 hours, so that the first carbon source and the first composite catalyst column, and the second carbon source and the second composite catalyst column are fully co-melted and co-infiltrated; then the pressure is increased to 95-105MPa at a constant speed for 60-96 hours, and then the constant pressure is kept for 130-165 hours under the pressure of 95-105 MPa.
In the pressure control process, heating is started when the pressure is increased to 20-40MPa, heating is performed for 200-600 seconds to 1330-1430 ℃, the constant temperature is kept for 1000-5000 seconds at the temperature, then the first cooling is started, the constant temperature is kept for 60-80 hours at the constant temperature after 20-48 hours to 1280-1320 ℃, then the second cooling is started, the constant temperature is kept for 130-165 hours to 1150-1270 ℃, and finally the time keeping with the pressure is finished synchronously, so that the large-particle cultivated diamond can be obtained.
In this embodiment, the synthetic block of the raw material proportioning scheme is placed in the synthesis cavity of the hexahedral press, and is first pressurized to 58MPa at a constant speed in 55 seconds, then kept at constant pressure for 1800 seconds, then pressurized to 68MPa at a constant speed in 60 seconds, then pressurized to 83MPa at a constant speed in 36 hours, then pressurized to 100MPa at a constant speed in 72 hours, and then kept at constant pressure for 145 hours under 100 MPa.
In the pressure control process, heating is started when the pressure is increased to 30MPa, heating is performed for 350 seconds to 1350 ℃, the temperature is kept constant for 2000 seconds, then the first cooling is started, the temperature is uniformly reduced to 1300 ℃ for 36 hours, the temperature is kept constant for 72 hours, then the second cooling is started, the temperature is uniformly reduced to 1250 ℃ for 145 hours, finally the time keeping with the pressure is finished synchronously, and the large-particle cultivated diamond with the diameter of 14.5mm and the height of 8.41mm, the weight of 11.5 carats, the color of excellent white and the internal purity of VVS level can be obtained.
The invention provides a large-particle single crystal cultivation diamond synthetic block with a multilayer permeable structure, and the grown diamond manufactured by the large-particle single crystal cultivation diamond synthetic block with the multilayer permeable structure has the blank size reaching 14mm diameter and 8.3mm height, the weight reaching more than 10ct, and the single crystal form being the shape of the complete standard octahedron {111} and the cube {100}, the internal purity reaching vs grade, the color reaching excellent white grade, and the stable synthesis, and completely meeting the industrialized production conditions.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which are all within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents.
In the description of the present invention, it should be understood that the directions or positional relationships indicated by the terms "front", "rear", "left", "right", "center", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or element to be referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the protection of the present invention.
Claims (9)
1. A multilayer infiltration type structure large granule single crystal cultivation diamond synthetic block which characterized in that: comprises a columnar hollow pyrophyllite block, wherein both ends of the pyrophyllite block are sequentially distributed with a pyrophyllite ring and a dolomite ring from outside to inside along the radial direction, and the annular center of the dolomite is also provided with a conductive steel ring;
the inner side of the pyrophyllite block is further sequentially provided with a dolomite outer lining, a carbon tube, a magnesium ring and an inner composite body from outside to inside along the radial direction, the two axial ends of the inner composite body are further sequentially provided with carbon paper and heat preservation sheets, the carbon paper is arranged on the inner wall of the conductive steel ring and extends to be paved on the dolomite outer lining, and the heat preservation sheets are arranged on the inner side of the carbon paper and extend to be paved on the carbon tube;
the internal synthesis body comprises a first carbon source sheet, a first composite catalyst column and a crystal bed which are sequentially laminated and laid along the axial direction, a containing cavity is formed in the first composite catalyst column, a second carbon source sheet and a second composite catalyst column are arranged in the containing cavity, and the second composite catalyst column is in contact with the crystal bed;
seed crystals are also arranged at the inner wall center of the crystal bed;
the first composite catalyst column is of a hollow cylindrical structure, and the inner surface of the first composite catalyst column is coated with an aluminum film; the second composite catalyst column is of a columnar structure, and an aluminum film is coated on the second composite catalyst column.
2. A multi-layer infiltration structured large grain single crystal grown diamond synthetic block according to claim 1, wherein: the first carbon source sheet and the second carbon source sheet are high-purity graphite sheets for cultivating diamonds.
3. A multi-layer infiltration structured large grain single crystal grown diamond synthetic block according to claim 2, wherein: the purity of the high-purity graphite flake is 99.99%.
4. A multi-layer infiltration structured large grain single crystal grown diamond synthetic block according to claim 1, wherein: the first composite catalyst column comprises the following components in percentage by weight: 70.0% -83.0% of high-purity iron powder, 7.0% -15.0% of nickel powder, 12.0% -25.0% of cobalt powder and 0.8% -1.8% of aluminum powder, wherein the purity of the high-purity iron powder is 99.9%, the granularity of the nickel powder is 200-300 meshes, and the granularity of the cobalt powder is 200-300 meshes.
5. A multi-layer infiltration structured large grain single crystal grown diamond synthetic block according to claim 1, wherein: the second composite catalyst column comprises the following components in percentage by weight: 63.0 to 76.0 percent of high-purity iron powder, 3.0 to 10.0 percent of nickel powder, 15.0 to 28.0 percent of cobalt powder, 4.0 to 12.0 percent of manganese powder and 0.3 to 1.1 percent of aluminum powder, wherein the purity of the high-purity iron powder is 99.9 percent, the granularity of the nickel powder is 300 to 400 meshes, the granularity of the cobalt powder is 300 to 400 meshes, and the granularity of the manganese powder is 300 to 400 meshes.
6. A multi-layered infiltration structured large grain single crystal grown diamond synthetic block according to claim 4 or 5, wherein: the granularity of the aluminum powder is 50nm.
7. A multi-layered infiltration structured large grain single crystal grown diamond synthetic block according to claim 4 or 5, wherein: the seed crystal adopts hexa-octahedral high-temperature high-pressure diamond.
8. A process for preparing a diamond composite block for growing large-grain single crystals of multilayer infiltration structure according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) Placing the synthesized block in a synthesis cavity of a hexahedral top press, uniformly boosting the pressure to 50-62MPa in 30-100 seconds, and keeping the constant pressure for 1000-5000 seconds;
(2) Boosting the pressure to 65-75MPa again at a constant speed for 30-100 seconds, and then boosting the pressure to 80-90MPa at a constant speed for 20-48 hours;
(3) Boosting the pressure to 95-105MPa at a constant speed for 60-96 hours, and keeping the pressure at a constant pressure for 130-165 hours;
(4) Heating when the pressure is increased to 20-40MPa, heating to 1330-1430 ℃ at a constant speed for 200-600 seconds, preserving heat for 1000-5000 seconds, then cooling for the first time, cooling to 1280-1320 ℃ at a constant speed for 20-48 hours, and preserving heat for 60-80 hours;
and then cooling for the second time, cooling to 1150-1270 ℃ at a constant speed for 130-165 hours, and finally finishing the synchronous with the pressure time to obtain the large-particle cultivated diamond.
9. The process for preparing the large-particle single crystal grown diamond synthetic block with the multilayer infiltration structure according to claim 8, wherein the process comprises the following steps:
in the step (1), the synthetic block is placed in a synthetic cavity of a hexahedral press, and is uniformly boosted to 58MPa and kept at constant pressure for 30min;
step (2) is carried out for 1min to uniformly boost the pressure to 68MPa again, and then 36h is carried out to uniformly boost the pressure to 15MPa, namely to 83MPa;
step (3) is to boost the pressure to 100MPa at a constant speed for 72 hours, and keep the pressure for 145 hours at a constant pressure;
in the step (4), when the pressure is increased to 30MPa, heating to 1350 ℃ at a constant speed for 350s, preserving heat for 2000s, then cooling to 50 ℃ at a constant speed for 36h, namely cooling to 1300 ℃, and preserving heat for 72h; and then cooling again, and cooling at a constant speed for 145h to 50 ℃, namely cooling to 1250 ℃, and finally finishing the synchronous with the pressure time to obtain the large-particle cultivated diamond.
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