CN115041100A - Diamond synthetic block cultivated by multilayer permeation type structure large-particle single crystal and preparation process thereof - Google Patents

Diamond synthetic block cultivated by multilayer permeation type structure large-particle single crystal and preparation process thereof Download PDF

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CN115041100A
CN115041100A CN202210868146.2A CN202210868146A CN115041100A CN 115041100 A CN115041100 A CN 115041100A CN 202210868146 A CN202210868146 A CN 202210868146A CN 115041100 A CN115041100 A CN 115041100A
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pressure
single crystal
diamond
powder
block
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CN115041100B (en
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刘乾坤
易良成
屈明
申幸卫
邢志华
周岩章
栗波
韩长余
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Zhongnan Diamond Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/065Presses for the formation of diamonds or boronitrides
    • B01J3/067Presses using a plurality of pressing members working in different directions

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Abstract

The invention discloses a multilayer permeable structure large-particle single crystal cultivation diamond synthetic block and a preparation process thereof, wherein the synthetic block comprises a columnar hollow pyrophyllite block, pyrophyllite rings and dolomite rings are sequentially distributed at two end parts of the pyrophyllite block from outside to inside along the radial direction, a conductive steel ring is further arranged at the center of the dolomite ring, the multilayer permeable structure synthetic block is adopted to replace the traditional sheet structure, the problem of poor surface layer purity at the later stage of high-temperature and high-pressure large-particle single crystal synthesis growth is optimized and improved, the growth speed of the large-particle single crystal cultivation diamond is controllable, the single crystal form is the shape accumulation of an octahedron (111) and a cube (100) which are complete in standard, the internal purity can reach more than a vs level, the color can reach an excellent white level, the stable synthesis can be realized, and the industrial production conditions can be completely met.

Description

Diamond synthetic block cultivated by multilayer permeation type structure large-particle single crystal and preparation process thereof
Technical Field
The invention belongs to the technical field of diamond synthesis by high-temperature high-pressure method cultivation, and particularly relates to a diamond synthesis block with a multilayer permeation type structure and large-particle single crystal cultivation and a preparation process thereof.
Background
The cultured diamonds are completely called laboratory cultured diamonds, the physicochemical properties of the cultured diamonds are completely the same as those of natural diamonds, and the cultured diamonds become new choices for diamond consumption gradually. The cultivated diamond product can be compared favorably with natural diamond in the aspects of crystal structure integrity, transparency, refractive index, 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 diamonds is still very low, along with the progress of the cultivation technology, the quality of the diamonds is improved, and the consumption concept is changed, so that the cultivated diamonds not only can replace natural diamonds, but also can be popularized to more application scenes where the original natural diamonds are not popularized, more market demands are stimulated, and a wide space is provided in the future.
The weight of a high quality, programmable carat grade grown diamond single crystal is multiplied by its commercial value. At present, the cultured diamonds which are well commercialized, developed and applied in China are synthesized and cultured diamonds by a high-temperature high-pressure method, wherein the synthesized blank of 3-10 carat cultured diamonds is the mainstream technology of various diamond culturing manufacturers, but the large-grain single crystal technology for synthesizing blanks with the weight of more than 10 carat is not mature, the quality and the purity of the synthesized diamonds are difficult to stably control, and the synthesized diamonds cannot be popularized and applied in a market.
Disclosure of Invention
The invention aims to provide a synthetic block of large-particle single crystal cultivated diamond with a multilayer permeable structure and a preparation process thereof, aiming at the defects of the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that:
a multi-layer large-particle single crystal cultivation diamond synthetic block with a penetration structure 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 further arranged in the center of the dolomite ring;
the inner side of the pyrophyllite block is sequentially provided with a dolomite outer lining, a carbon tube, a magnesium ring and an inner synthetic body from outside to inside along the radial direction, the two axial ends of the inner synthetic body are 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 to the dolomite outer lining, and the heat preservation sheets are arranged on the inner side of the carbon paper and extends to be paved to the carbon tube;
the internal synthetic body comprises a first carbon source sheet, a first composite catalyst column and a crystal bed which are sequentially stacked 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;
and seed crystals are also arranged at the center of the inner wall 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 outer surface of the second composite catalyst column.
The first carbon source sheet and the second carbon source sheet are both made of 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 particle size of the nickel powder is 200-300 meshes, and the particle size of the cobalt powder is 200-300 meshes.
The second composite catalyst column 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 50 nm.
The seed crystal adopts a six-octahedron high-temperature high-pressure diamond.
The preparation process of the multilayer permeation type structure large-particle single crystal cultivated diamond synthetic block comprises the following steps:
(1) placing the synthesis block in a synthesis cavity of a cubic press, uniformly boosting the pressure to 50-62MPa in 30-100 seconds, and keeping the pressure at constant pressure for 1000-5000 seconds;
(2) boosting the pressure to 65-75MPa at constant speed again within 30-100 seconds, and then boosting the pressure to 80-90MPa at constant speed within 20-48 hours;
(3) uniformly boosting the pressure to 95-105MPa within 60-96 hours, and keeping the pressure at constant pressure for 130-165 hours;
(4) when the pressure is increased to 20-40MPa, the temperature is increased to 1330-1430 ℃ at a constant speed for 600 seconds and is kept for 1000 seconds and 5000 seconds, then the temperature is reduced for the first time, and the temperature is reduced to 1280-1320 ℃ at a constant speed for 20-48 hours and is kept for 60-80 hours at a constant temperature;
and then, cooling for the second time, cooling to 1150-1270 ℃ at a constant speed within 130-165 hours, and finally finishing the process of keeping synchronization with the pressure time, thus obtaining the large-particle cultivated diamond.
In the step (1), the synthesis block is placed in a synthesis cavity of a cubic press, the pressure is increased to 58MPa at a constant speed, and the constant pressure is kept for 30 min;
in the step (2), the pressure is increased to 68MPa again at a constant speed for 1min, and then the pressure is increased to 15MPa at a constant speed for 36h, namely the pressure is increased to 83 MPa;
in the step (3), the pressure is increased to 100MPa at a constant speed for 72h, and is kept at a constant pressure for 145 h;
in the step (4), when the pressure is increased to 30MPa, the temperature is increased to 1350 ℃ at a constant speed for 350s and is kept for 2000s, and then the temperature is reduced to 50 ℃ at a constant speed for 36h, namely 1300 ℃, and is kept at a constant temperature for 72 h; and then cooling again, uniformly cooling for 145h to 50 ℃, namely cooling to 1250 ℃, and finally keeping synchronization with the pressure time to finish the process, thus obtaining the large-particle cultured diamond.
The invention has the beneficial effects that:
this multilayer infiltration formula structure large granule single crystal cultivation diamond synthesis piece and preparation technology thereof adopts multilayer infiltration formula structure synthesis piece, replaces traditional sheet structure, optimizes the problem that high temperature high pressure large granule single crystal synthesis growth later stage surface layer cleanliness is poor, realizes that large granule single crystal cultivation diamond growth speed is controllable to be prepared, and the single crystal form is the poly shape of octahedron { 111 } and cube { 100 } of complete standard, and inside cleanliness can reach more than the vs level, and the colour can reach the excellent white level, can stably synthesize, satisfies the industrialization condition of putting into production completely.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a process diagram of the present invention;
description of reference numerals:
1. the catalyst comprises pyrophyllite synthesis blocks, 2, pyrophyllite rings, 3, dolomite rings, 4, conductive steel rings, 5, dolomite outer linings, 6, carbon paper, 7, carbon tubes, 8, magnesium cups, 9, heat preservation sheets, 10, a crystal bed, 11, first carbon source sheets, 12, first composite catalyst columns, 13, second carbon source sheets, 14, second composite catalyst columns, 15 and seed crystals.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
The invention provides a large-grain single crystal cultivation diamond synthetic block with a multilayer permeable structure, which is shown in figures 1 and 2.
The large-particle single crystal cultivation diamond synthetic block with the multilayer permeation type structure 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 further arranged in the center of each dolomite ring 3;
the inner side of the pyrophyllite block 1 is also sequentially provided with a dolomite outer lining 5, a carbon tube 7, a magnesium ring 8 and an inner synthetic body from outside to inside along the radial direction, the two axial ends of the inner synthetic body are also 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 internal synthetic body comprises a first carbon source sheet 11, a first composite catalyst column 12 and a crystal bed which are sequentially stacked and paved 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;
the seed crystal 15 is arranged at the center of the inner wall of the crystal bed 10 and is a six-octahedron high-temperature high-pressure diamond, wherein the size of the diamond is 1.6 mm-3.2 mm.
The first composite catalyst column 12 is a hollow cylindrical structure, and the inner surface thereof is coated with an aluminum film.
The second composite catalyst column 14 is a columnar structure, and an aluminum film is coated on the outer surface thereof.
The first carbon source plate 11 and the second carbon source plate 13 both adopt high-purity graphite sheets special for cultivating diamonds, 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 particle size of the nickel powder is 200-300 meshes, the particle size of the cobalt powder is 200-300 meshes, and the particle size of the aluminum powder is 50 nm; the iron powder, the nickel powder and the cobalt powder are pressed into a hollow cylindrical structure with a containing cavity after the processes 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 particle size of the nickel powder is 300-400 meshes, the particle size of the cobalt powder is 300-400 meshes, the particle size of the manganese powder is 300-400 meshes, and the particle size of the aluminum powder is 50nm, in the embodiment, the diameter of the second composite catalyst column 14 is 30mm, and the height of the second composite catalyst column is 25 mm; 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 preparation and cultivation process of the multilayer permeation type structure large-particle single crystal cultivation diamond synthetic block is as follows:
placing the synthesis block of the raw material proportioning scheme in a synthesis cavity of a cubic 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 the second composite catalyst column under the low-pressure high-temperature state; uniformly boosting the pressure to 65-75MPa within 30-100 seconds, and uniformly boosting the pressure to 80-90MPa within 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 uniformly increasing the pressure to 95-105MPa within 60-96 hours, and then keeping constant pressure for 130-165 hours under the pressure of 95-105 MPa.
In the pressure control process, the temperature is raised to 1330-1430 ℃ by adopting 200-.
In this embodiment, the synthesis block of the raw material proportioning scheme is placed in a synthesis cavity of a cubic press, and first, the pressure is increased to 58MPa at a constant speed for 55 seconds, then kept at a constant pressure for 1800 seconds under the pressure, then increased to 68MPa at a constant speed for 60 seconds, then increased to 83MPa at a constant speed for 36 hours, then increased to 100MPa at a constant speed for 72 hours, and then kept at a constant pressure for 145 hours under the pressure of 100 MPa.
In the pressure control process, the temperature is raised when the pressure is raised to 30MPa, the temperature is raised to 1350 ℃ in 350 seconds, the temperature is kept for 2000 seconds at constant temperature, then the temperature is first lowered, the temperature is lowered to 1300 ℃ in 36 hours at constant speed, then the temperature is kept at constant temperature for 72 hours, then the temperature is second lowered, the temperature is lowered to 1250 ℃ in 145 hours at constant speed, and finally the temperature is kept synchronously with the pressure time, so that the large-particle cultivated diamond can be prepared, wherein the diameter of the large-particle cultivated diamond is 14.5mm, the height of the large-particle cultivated diamond is 8.41mm, the weight of the large-particle cultivated diamond reaches 11.5 carats, the color of the large-particle cultivated diamond is excellent and white, the interior of the large-particle cultivated diamond is pure, and the cleanliness reaches VVS level.
The invention provides a multilayer permeation structure large-particle single crystal cultivated diamond synthetic block, a cultivated diamond manufactured by using the multilayer permeation structure large-particle single crystal cultivated diamond synthetic block provided by the invention has a blank size of more than 14mm in diameter and 8.3mm in height and a weight of more than 10ct, and a single crystal form is a conglomerate of octahedrons { 111 } and cubes { 100 } which are complete in standard, the internal purity can reach a vs level, the color can reach an excellent level, the synthetic block can be stably synthesized, and the industrial production conditions can be completely met.
The foregoing shows and describes the general principles, essential 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, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents.
In the description of the present invention, it is to be understood that the terms "front", "rear", "left", "right", "center", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the scope of the present invention.

Claims (10)

1. The utility model provides a diamond synthesis piece is cultivated to multilayer infiltration formula structure large granule single crystal which characterized in that: the conductive pyrophyllite cable comprises a columnar hollow pyrophyllite block, 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 further arranged in the center of each dolomite ring;
the inner side of the pyrophyllite block is sequentially provided with a dolomite outer lining, a carbon tube, a magnesium ring and an inner synthetic body from outside to inside along the radial direction, the two axial ends of the inner synthetic body are 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 to the dolomite outer lining, and the heat preservation sheets are arranged on the inner side of the carbon paper and extends to be paved to the carbon tube;
the internal synthetic body comprises a first carbon source sheet, a first composite catalyst column and a crystal bed which are sequentially stacked 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;
and seed crystals are also arranged at the center of the inner wall of the crystal bed.
2. The synthetic mass of multilayer percolated large grain single crystal grown diamond of claim 1, wherein: 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 outer surface of the second composite catalyst column.
3. The synthetic mass of multilayer percolated large grain single crystal grown diamond of claim 1, wherein: the first carbon source sheet and the second carbon source sheet are both made of high-purity graphite sheets for cultivating diamonds.
4. The multi-layered infiltration type structure large-grain single crystal cultivation diamond synthetic block of claim 3, wherein: the purity of the high-purity graphite flake is 99.99%.
5. The synthetic mass of multilayer percolated large grain single crystal grown diamond of 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 particle size of the nickel powder is 200-300 meshes, and the particle size of the cobalt powder is 200-300 meshes.
6. The synthetic mass of multilayer percolated large grain single crystal grown diamond of claim 1, wherein: the second composite catalyst column 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.
7. The large grain single crystal grown diamond composite block of multilayer permeable structure according to claim 5 or 6, wherein: the granularity of the aluminum powder is 50 nm.
8. The large grain single crystal grown diamond composite block of multilayer permeable structure according to claim 5 or 6, wherein: the seed crystal adopts a six-octahedron high-temperature high-pressure diamond.
9. The process for preparing a multi-layer permeable structure large-grain single crystal cultured diamond synthetic block according to any one of claims 1 to 6, comprising the steps of:
(1) placing the synthesis block in a synthesis cavity of a cubic press, uniformly boosting the pressure to 50-62MPa in 30-100 seconds, and keeping the pressure at constant pressure for 1000-5000 seconds;
(2) boosting the pressure to 65-75MPa at constant speed again within 30-100 seconds, and then boosting the pressure to 80-90MPa at constant speed within 20-48 hours;
(3) uniformly boosting the pressure to 95-105MPa within 60-96 hours, and keeping the pressure at constant pressure for 130-165 hours;
(4) when the pressure is increased to 20-40MPa, the temperature is raised to 1330-1430 ℃ at a constant speed for 600 seconds and is kept for 1000 seconds and 5000 seconds, then the first temperature reduction is started, the temperature is reduced to 1280-1320 ℃ at a constant speed for 20-48 hours and is kept for 60-80 hours at a constant temperature;
and then, cooling for the second time, cooling to 1150-1270 ℃ at a constant speed within 130-165 hours, and finally finishing the process of keeping synchronization with the pressure time, thus obtaining the large-particle cultivated diamond.
10. The process of claim 9, wherein the diamond synthesis block is prepared by a process comprising the steps of:
in the step (1), the synthesis block is placed in a synthesis cavity of a cubic press, the pressure is increased to 58MPa at a constant speed, and the constant pressure is kept for 30 min;
in the step (2), the pressure is increased to 68MPa again at a constant speed for 1min, and then the pressure is increased to 15MPa at a constant speed for 36h, namely the pressure is increased to 83 MPa;
in the step (3), the pressure is increased to 100MPa at a constant speed for 72h, and is kept at a constant pressure for 145 h;
in the step (4), when the pressure is increased to 30MPa, the temperature is increased to 1350 ℃ at a constant speed for 350s and is kept for 2000s, and then the temperature is reduced to 50 ℃ at a constant speed for 36h, namely 1300 ℃, and is kept at a constant temperature for 72 h; and then cooling again, uniformly cooling for 145h to 50 ℃, namely cooling to 1250 ℃, and finally keeping synchronization with the pressure time to finish the process, thus obtaining the large-particle cultured diamond.
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