Assembling structure for synthesizing diamond by high-temperature and high-pressure method

Abstract

The utility model discloses an assembly structure for synthesizing diamonds by a high-temperature and high-pressure method, which relates to the technical field of diamond synthesis and comprises an outer layer structure, a middle layer heating and insulating system, a core reaction layer and a top covering layer which are sequentially arranged from outside to inside, the outer-layer structure comprises a pyrophyllite composite block, a pyrophyllite ring surrounding the outer side of the pyrophyllite composite block and a conductive steel cap fixed to the top, the middle-layer heating and insulating system comprises a heating sleeve embedded into the pyrophyllite composite block, a heating piece is arranged in the heating sleeve, a magnesium oxide insulating sleeve is wrapped in the heating piece, and the outer-layer structure and the middle-layer heating and insulating system are arranged in the heating sleeve. A vertically supported thick zirconium oxide column is arranged below the heating sleeve, the core reaction layer comprises a magnesium oxide crystal bed, a carbon source is placed on the magnesium oxide crystal bed, alloy is distributed around the carbon source, and the top covering layer comprises a thin zirconium oxide column covering the core reaction layer. The problems that in the prior art, obtained seeds with high carbon content grow fast, but the impurity removal capacity is weak, and the quality is poor are solved; the seeds with low carbon content are good in quality but small in size, and the economic benefit is low.

Description

Technical Field

[0001] This utility model relates to the field of diamond synthesis technology, specifically to an assembly structure for synthesizing diamonds using a high-temperature and high-pressure method. Background Technology

[0002] In conventional diamond synthesis, multiple seeds within the same synthesis block grow multiple diamonds simultaneously. However, due to variations in temperature uniformity within the synthesis cavity—caused by differences in the heat output of the heating element and the distance between the seeds and the heating element—this uneven distribution is difficult to eliminate. Consequently, each seed within the same cavity receives varying amounts of carbon, leading to variations in diamond size and quality. Diamonds with higher carbon content grow faster but have reduced impurity removal capabilities and lower quality; those with lower carbon content may have acceptable quality but smaller sizes, resulting in poor economic returns—neither of which meets the producer's initial objectives. Uneven carbon distribution also increases crystal defects and reduces diamond clarity.

[0003] Existing technologies cannot completely solve the above problems. Therefore, there is an urgent need for an assembly structure for high-temperature and high-pressure diamond synthesis that can ensure the independent growth of multiple seeds and uniform carbon distribution. Utility Model Content

[0004] The purpose of this invention is to provide an assembly structure for high-temperature and high-pressure synthetic diamonds, in order to solve the problems in the prior art where high carbon content results in faster growth, reduced impurity removal ability, and poor quality; while low carbon content results in acceptable quality but smaller size and poor economic benefits, neither of which meets the producer's original intention; and uneven carbon content distribution leads to increased crystal defects and decreased diamond clarity.

[0005] An assembly structure for synthesizing diamonds using a high-temperature, high-pressure method includes, from the outside to the inside, an outer layer structure, a middle heating and insulation system, a core reaction layer, and a top covering layer. The outer layer structure includes a pyrophyllite composite block, a pyrophyllite ring surrounding the outside of the pyrophyllite composite block, and a conductive steel cap fixed to the top. The middle heating and insulation system includes a heating sleeve embedded inside the pyrophyllite composite block, with heating elements inside the heating sleeve. The heating sleeve is wrapped with a magnesium oxide insulating sleeve, and a vertically supported zirconia thick column is provided below the heating sleeve. The core reaction layer includes a magnesium oxide crystal bed, with a carbon source placed on the magnesium oxide crystal bed and an alloy distributed around the carbon source. The top covering layer includes a zirconia thin column covering the core reaction layer.

[0006] Preferably, the magnesium oxide separator has a thickness of 1.0 mm and a height equal to the total thickness of the alloy and the carbon source.

[0007] Preferably, the alloy consists of six equally sized sector-shaped iron-nickel alloy blocks, with a 1.0 mm gap between adjacent blocks.

[0008] Preferably, the surface of the magnesium oxide crystal bed is provided with six equally divided seed positioning holes, the hole diameter being slightly smaller than the seed diameter and the depth being consistent with the seed height.

[0009] Preferably, the carbon source consists of six fan-shaped high-purity graphite sheets, each corresponding to an alloy block.

[0010] Preferably, the pyrophyllite composite block and the pyrophyllite ring are tightly bonded together with a high-temperature adhesive to form a sealed cavity.

[0011] Preferably, the conductive steel cap is made of copper alloy and is electrically connected to the heating sleeve to transmit current to the heating element.

[0012] Preferably, the thickness of the magnesium oxide insulating sleeve is 3-5 mm, and its inner wall is fitted with the outer wall of the heating sleeve to form a heat insulation layer.

[0013] The advantages of this invention are as follows: The assembly structure for high-temperature and high-pressure diamond synthesis in this invention uses a partitioning assembly method, employing magnesium oxide sheets to completely separate each seed, the alloy required for growth, and the carbon source, creating independent growth spaces. The benefits are: as long as the temperature is within the range required for diamond growth and the temperature difference is constant, each seed grows independently, fundamentally solving the problem of seeds competing for carbon resources. This ensures consistent diamond size within the same synthetic block and controls the diamond growth rate, thus providing favorable conditions for growing high-quality diamonds. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of a typical large single crystal synthesis block structure in this utility model.

[0015] Figure 2 This is a diagram showing the distribution of seed positioning holes in the magnesium oxide crystal bed of this invention.

[0016] Figure 3 This is a layout diagram of the sector-shaped alloy in this utility model.

[0017] Figure 4 This is a schematic diagram of the steel mold in this utility model.

[0018] Figure 5 This illustrates the assembly relationship between the fan-shaped graphite sheet and the magnesium oxide separator in this utility model.

[0019] Figure 6 This is a schematic diagram of the magnesium oxide structure processed into sheet form in this utility model.

[0020] Among them, 1. Pyrophyllite composite block; 2. Pyrophyllite ring; 3. Conductive steel cap; 4. Heating plate; 5. Heating sleeve; 6. Magnesium oxide insulating sleeve; 7. Zirconia thick column; 8. Carbon source; 9. Alloy; 10. Magnesium oxide crystal bed; 11. Zirconia thin column. Detailed Implementation

[0021] To make the technical means, creative features, objectives and effects of this utility model easier to understand, the present utility model will be further described below in conjunction with specific embodiments.

[0022] like Figures 1 to 6 As shown, an assembly structure for synthesizing diamonds using a high-temperature, high-pressure method includes, from the outside to the inside, an outer layer structure, a middle heating and insulation system, a core reaction layer, and a top covering layer. The outer layer structure includes a pyrophyllite composite block 1, a pyrophyllite ring 2 surrounding the outside of the pyrophyllite composite block 1, and a conductive steel cap 3 fixed to the top. The middle heating and insulation system includes a heating sleeve 5 embedded inside the pyrophyllite composite block 1. The heating sleeve 5 is provided with a heating element 4 inside, and a magnesium oxide insulating sleeve 6 is wrapped around the heating sleeve 5. A vertically supported zirconia thick column 7 is provided below the heating sleeve 5. The core reaction layer includes a magnesium oxide crystal bed 10, on which a carbon source 8 is placed, and an alloy 9 is distributed around the carbon source 8. The top covering layer includes a zirconia thin column 11 covering the core reaction layer.

[0023] In the above scheme, components such as the pyrophyllite composite block 1, the pyrophyllite ring 2, and the zirconia thick pillar 7 provide stable support and protection for the entire assembly structure, capable of withstanding the enormous pressure under high temperature and high pressure conditions, ensuring the integrity of the structure during the synthesis process, and reducing synthesis failures caused by structural instability; the heating element 4 inside the heating sleeve 5 can quickly and uniformly heat the core reaction layer, and the magnesium oxide insulating sleeve 6 effectively prevents heat loss and current leakage, improving heating efficiency and energy utilization, while ensuring the safety of equipment and operators; the magnesium oxide crystal bed 10 provides a stable growth substrate for the carbon source 8, and the distribution of alloy 9 helps to react with the carbon source 8 under high temperature and high pressure, reducing the conditions required for diamond growth, promoting rapid crystallization and growth of diamond, and improving the quality and yield of diamond synthesis; the zirconia thin pillar 11 of the top covering layer can prevent external impurities from entering the core reaction layer, while also helping to uniformly distribute pressure and temperature, creating a more favorable environment for diamond growth and improving the quality of synthesized diamonds.

[0024] In this embodiment, the magnesium oxide separator has a thickness of 1.0 mm and a height equal to the total thickness of alloy 9 and carbon source 8.

[0025] In this embodiment, the alloy 9 consists of six equally sized sector-shaped iron-nickel alloy blocks, with a 1.0mm gap between adjacent blocks.

[0026] In this embodiment, the surface of the magnesium oxide crystal bed 10 is provided with six equally divided seed positioning holes, the hole diameter being slightly smaller than the seed diameter and the depth being consistent with the seed height.

[0027] In this embodiment, the carbon source 8 consists of six fan-shaped high-purity graphite sheets, each corresponding to an alloy block.

[0028] Magnesium oxide powder with a purity of 99.99% and a mesh size of 200 was pressed into a disc shape using a mold and sintered at 1200℃ for 12 hours to form a crystal bed 10. Seed positioning holes were opened on the surface according to a six-part rule. Cylindrical iron-nickel alloy wire was cut into 6 sector-shaped blocks, with a 1.0mm gap between adjacent blocks. High-purity graphite powder with a purity of 99.999% was pressed into 6 sector-shaped graphite sheets 8 using a 200T press, with a thickness matching the alloy blocks. The magnesium oxide sheets were 1.0mm thick and their height was equal to the total thickness of the alloy and graphite. They were stacked in the following order:

[0029] Lower pyrophyllite composite block 1 → Lower pyrophyllite ring 2 → Lower conductive steel cap 3 → Lower heating plate 4 → Heating sleeve 5 → Magnesium oxide insulating sleeve 6 → Magnesium oxide crystal bed 10; Place sector-shaped alloy block 9 and graphite sheet 8, insert magnesium oxide separator to form an independent unit; Cover with thick magnesium oxide sheet 7 → Upper heating plate → Upper pyrophyllite composite block → Upper pyrophyllite ring → Upper conductive steel cap; After assembly, bake at 120℃ for 6 hours, then pressurize to 5.5GPa, heat to 1400℃, and hold for 12 hours.

[0030] In this embodiment, the pyrophyllite composite block 1 and the pyrophyllite ring 2 are tightly bonded together with a high-temperature adhesive to form a sealed cavity.

[0031] In the above scheme, the pyrophyllite composite block 1 and the pyrophyllite ring 2 are tightly bonded together by a high-temperature adhesive to form a sealed cavity, which can effectively prevent external impurities from entering the interior of the assembly structure, avoid impurities from interfering with the diamond synthesis process, and ensure the quality of the synthesized diamond. The tightly bonded pyrophyllite composite block 1 and pyrophyllite ring 2 enhance the stability and strength of the outer structure, enabling it to better withstand the enormous pressure under high temperature and high pressure conditions, protect the internal middle heating and insulation system, core reaction layer and other components, and ensure the smooth progress of the synthesis process.

[0032] In this embodiment, the conductive steel cap 3 is made of copper alloy and is electrically connected to the heating sleeve 5 to transmit current to the heating element 4.

[0033] In the above scheme, the conductive steel cap 3, made of copper alloy, has good conductivity, which can effectively transfer current to the heating element 4, reduce energy loss during current transmission, improve heating efficiency, and ensure that the heating element 4 can heat up quickly and stably, providing a suitable temperature environment for diamond synthesis. As part of the outer structure, the conductive steel cap 3 not only performs the function of conducting electricity but also provides structural support for the entire assembly structure. The copper alloy material has high strength and corrosion resistance, and can maintain stable performance under high temperature and high pressure environments, extending the service life of the assembly structure.

[0034] In this embodiment, the thickness of the magnesium oxide insulating sleeve 6 is 3-5 mm, and its inner wall is fitted with the outer wall of the heating sleeve 5 to form a heat insulation layer.

[0035] In the above scheme, the heat insulation layer formed by the 3-5mm thick magnesium oxide insulating sleeve 6 and the outer wall of the heating sleeve 5 can effectively prevent heat from being transferred from the heating sleeve 5 to the outside, reduce heat loss, improve heating efficiency, and enable the core reaction layer to carry out diamond synthesis under more stable temperature conditions, which helps to improve the quality and yield of synthetic diamonds.

[0036] Working Process and Principle: Taking the synthesis of 6 seeds as an example, a magnesium oxide crystal bed 10 is fabricated using conventional methods. 200-mesh 99.99% magnesium oxide is selected. The outer diameter of the crystal bed is determined by the mold size, and the height is determined by pressure and weight. The bed is held at 1200℃ for 12 hours to obtain a disc of the required size. For specific seed positioning, a circle is drawn approximately 6mm from the center of the crystal bed edge. This circle is then divided into 6 equal parts, and holes are drilled at the intersections of the 6-part lines and the circle. Figure 2 As shown. The aperture is slightly smaller than the seed diameter, and the depth is the same as the seed height, to ensure that after the seed is filled into the hole, the seed face and the crystal bed surface are on the same plane, without protruding or sinking.

[0037] The production of Alloy 9 involves wire cutting a standard cylindrical alloy into six equally sized sector-shaped alloy blocks, such as... Figure 3 As shown. During processing, each radius edge of the sector alloy is cut by an additional 0.5mm. When they are reassembled into a circle of the original diameter, a gap of about 1.0mm is left between each sector alloy.

[0038] The preparation of carbon source 8 involves granulating 200-mesh high-purity graphite (99.999%) powder, and before pressing it into a cylindrical mold, [the following steps are taken]. Figure 4 The steel mold shown is placed into the mold cavity, the weighed graphite is added, and then it is placed into a 200T press. The pressure is adjusted to 100-150T to press, and then 6 fan-shaped graphite sheets as shown in Figure ⑤ are obtained. Figure 4 The mold can be made of mold steel, wire cut, with a thickness of 1.0mm and a height that is about 0.5mm smaller than the height of the finished graphite sheet to be processed, to avoid the upper pressure head pressing on the mold.

[0039] To fabricate the separator sheets, magnesium oxide, the same material used in the crystal bed, is processed into sheet shapes using a mold, such as... Figure 6 As shown. The height is equal to the thickness of the alloy plus graphite, which is 1.0 mm. The length is equal to or slightly less than the radius of the crystal bed disk.

[0040] Assemble the following blocks: Lower pyrophyllite → Lower pyrophyllite ring → Lower conductive steel cap → Lower heating element → Heating sleeve → Insulating sleeve → Thin magnesium oxide sheet → Crystal bed → Fan-shaped alloy sheet → Magnesium oxide separator → Fan-shaped graphite sheet → Thick magnesium oxide sheet → Upper heating element → Upper pyrophyllite block → Upper pyrophyllite ring → Upper conductive steel cap. After assembly, bake in a 120℃ oven for 6 hours before use for synthesis.

[0041] The conventional synthesis process involves: loading the block → pressurizing → heating → maintaining the temperature and pressure → stopping the heat → depressurizing → removing the block → smashing the block → refining and synthesizing the column → obtaining a diamond of the required size.

[0042] As is known from common technical knowledge, this utility model can be implemented through other embodiments that do not depart from its spirit or essential characteristics. Therefore, the disclosed embodiments described above are merely illustrative in all respects and are not the only ones. All modifications within the scope of this utility model or its equivalents are included in this utility model.

Claims

1. An assembly structure for synthesizing diamonds using a high-temperature, high-pressure method, characterized in that: The system comprises an outer structure, a middle heating and insulation system, a core reaction layer, and a top cover layer arranged sequentially from the outside to the inside. The outer structure includes a pyrophyllite composite block (1), a pyrophyllite ring (2) surrounding the outside of the pyrophyllite composite block (1), and a conductive steel cap (3) fixed to the top. The middle heating and insulation system includes a heating sleeve (5) embedded inside the pyrophyllite composite block (1). The heating sleeve (5) is provided with a heating element (4). The heating sleeve (5) is wrapped with a magnesium oxide insulating sleeve (6), and a vertically supported zirconia thick column (7) is provided below the heating sleeve (5). The core reaction layer includes a magnesium oxide crystal bed (10), on which a carbon source (8) is placed. An alloy (9) is distributed around the carbon source (8). The top cover layer includes a zirconia thin column (11) covering the core reaction layer.

2. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The alloy (9) consists of six equal-sized sector-shaped iron-nickel alloy blocks, with a 1.0mm gap between adjacent blocks.

3. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The surface of the magnesium oxide crystal bed (10) is provided with six equally divided seed positioning holes, the diameter of which is slightly smaller than the diameter of the seed and the depth is consistent with the height of the seed.

4. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The carbon source (8) consists of six fan-shaped high-purity graphite sheets, each corresponding to an alloy block.

5. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The pyrophyllite composite block (1) and the pyrophyllite ring (2) are tightly bonded together by a high-temperature adhesive to form a sealed cavity.

6. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The conductive steel cap (3) is made of copper alloy and is electrically connected to the heating sleeve (5) to transmit current to the heating element (4).

7. The assembly structure for high-temperature and high-pressure synthetic diamond according to claim 1, characterized in that: The thickness of the magnesium oxide insulating sleeve (6) is 3-5 mm, and its inner wall is fitted with the outer wall of the heating sleeve (5) to form a heat insulation layer.

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