CN210875234U - Graphite tube heating body and diamond large single crystal synthesis cavity - Google Patents
Graphite tube heating body and diamond large single crystal synthesis cavity Download PDFInfo
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- CN210875234U CN210875234U CN201921000836.6U CN201921000836U CN210875234U CN 210875234 U CN210875234 U CN 210875234U CN 201921000836 U CN201921000836 U CN 201921000836U CN 210875234 U CN210875234 U CN 210875234U
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Abstract
The utility model discloses a graphite pipe heating member, including body A section and B section, body A section with body B section is fashioned graphite material tubular structure for the integration, body B section is close to one side periphery of body A section forms the recess of annular structure through the cutting, the peripheral movable sleeve of recess is equipped with insulating ring. A diamond large single crystal synthesis cavity comprises the graphite tube heating body and an accommodating structure. The resistance of the groove part in the utility model can be increased, thus the temperature gradient in the synthetic cavity can be reduced, and the quality of IIa type diamond large single crystal is further improved, therefore, an auxiliary heat source is not needed to be added on the lower part of the graphite tube heating body; the design can ensure the effective transmission of the synthetic pressure and simultaneously avoid the damage of the groove part in the boosting process; the volume in the cavity can be enlarged under the condition that the volume of the whole cavity is not changed, and the research and development directions of preparing diamond single crystals by a high-temperature high-pressure method are combined.
Description
Technical Field
The utility model relates to a synthetic technical field of diamond single crystal specifically is a synthetic cavity of graphite tube heating member and big single crystal of diamond.
Background
Diamond is commonly called as 'diamond', is a limiting functional material which integrates multiple excellent performances such as maximum hardness, maximum thermal conductivity, minimum compression ratio, widest light-transmitting wave band, fastest sound velocity, strong acid and strong base corrosion resistance, radiation resistance, high breakdown voltage, high carrier mobility and the like in the materials in the world at present, and is widely applied to various fields such as industry, military, science and technology, medical treatment, jewelry and the like. In view of potential scientific research and commercial value of diamond, the diamond synthesis technology is extremely secret abroad. Therefore, the advanced high-performance diamond synthesis technology with independent intellectual property rights plays an extremely important role in the whole future industrialized development, the overall improvement of technological level, the overall enhancement of national defense strength and the like of a country.
The high temperature and high pressure method is one of the most effective technological means for synthesizing large diamond single crystal, and its growth driving force is the axial temperature gradient of graphite tube heating body, i.e. the growth rate of large diamond single crystal is directly proportional to the axial temperature gradient of graphite tube heating body.
The reason why the large diamond single crystal synthesized by the high-temperature high-pressure method (6.0GPa and 1300 ℃) is yellow is that a diamond synthesis system contains free nitrogen impurities or combined nitrogen impurity elements, and the nitrogen impurities enter diamond crystal lattices in the diamond crystallization process to further form nitrogen defects. Generally, the nitrogen defect concentration in the large diamond single crystal synthesized by the high temperature and high pressure method is about 300 ppm. In order to obtain a diamond large single crystal with a perfect lattice structure and better optical performance, a nitrogen removing agent (Ti/Cu or Zr) is required to be added into a synthesis cavity, so that the concentration of nitrogen impurity defects in the synthesized diamond large single crystal is less than 1ppm and the synthesized diamond large single crystal is colorless and transparent. After introduction of the nitrogen scavenger in the synthesis chamber (the synthesis assembly is shown in fig. 1), it is clearly equivalent to the introduction of new impurities inside the synthesis chamber. If the temperature gradient is not properly reduced, a large amount of metal inclusions can be generated in the prepared diamond, and the quality of the synthesized diamond is seriously influenced.
In the prior art, a graphite tube heating body as shown in figure 1 is adopted, and in order to ensure the quality of diamond without nitrogen impurities, an auxiliary heat source is added at the lower part of the graphite tube heating body in the prior art for reducing the temperature gradient. After the auxiliary heat source is added, the highest temperature of the graphite tube heating element is still located in the middle of the graphite tube heating element, the temperature of the bottom of the graphite tube is greatly improved compared with the temperature of the bottom of the graphite tube before the auxiliary heat source is not added, however, the distance from the middle of the graphite tube heating element to the bottom of the graphite tube is not changed, which means that the temperature gradient from the middle of the graphite tube heating element to the bottom of the graphite tube heating element is reduced, namely the temperature gradient in the synthesis cavity is reduced, and thus the quality of the IIa type diamond large single crystal can be.
However, the use of the auxiliary heat source chip causes a loss of pressure inside the synthesis chamber, about 0.8GPa, which means about 13.3% of the pressure is lost, and the system pressure must be increased to ensure the synthesis pressure of the large diamond single crystal, which inevitably causes an increase in the loss of the tungsten carbide anvil and other components of the high-pressure apparatus. In addition, the use of an auxiliary heat source is troublesome in the assembly process, and once the operation is careless, local overheating is generated near the synthesis auxiliary heat source, so that the circuit of a synthesis system is broken, even a cracking hammer phenomenon with larger loss is generated, and the production cost is increased.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a synthetic cavity of graphite tube heating member and big single crystal of diamond to solve the problem that proposes among the above-mentioned background art.
In order to achieve the above object, the utility model provides a following technical scheme:
the utility model provides a graphite pipe heating member, includes body A section and body B section, body A section with body B section is fashioned graphite material tubular structure as an organic whole, body B section is close to body A section's one side is peripheral forms the recess of annular structure through the cutting, the peripheral movable sleeve of recess is equipped with insulating ring.
Further, the length of the pipe body A section is larger than that of the pipe body B section.
Furthermore, the insulating ring is an integrally formed insulating ceramic ring.
Furthermore, the insulating ring is an insulating material ring formed by splicing two movably assembled parts.
Furthermore, the size of the insulating ring is movably matched with that of the groove, and the insulating ring is preferably made of an insulating ceramic material.
The utility model provides a synthetic cavity of big single crystal of diamond, include the graphite tube heating member, still including holding structure, holding structure establishes the graphite flake at quartz tube upper and lower both ends about the peripheral quartz tube of graphite tube heating member and laminating including the cover, quartz tube and graphite flake periphery are fixed through the embedding of pyrophyllite stone, and both ends all imbed about the pyrophyllite stone and are provided with the end plug, the end plug laminating graphite flake is fixed.
Further, the lower part is equipped with brilliant bed in the graphite tube heating body, it is equipped with the seed crystal to pack above the brilliant bed, just the seed crystal compresses tightly through the metal catalyst of cover establishing in the insulating tube, metal catalyst upper end center has cylindrical arch, and protruding peripheral cover is equipped with cyclic annular graphite carbon source, it is provided with ceramic end cap to pack in the graphite tube heating body of insulating tube, metal catalyst and graphite carbon source top.
Compared with the prior art, the beneficial effects of the utility model are that: the resistance of the groove part will be increased, thus the temperature gradient in the synthetic cavity can be reduced, and the quality of IIa type diamond large single crystal is improved, therefore, an auxiliary heat source is not needed to be added at the lower part of the graphite tube heating body, and the height of the groove can be properly adjusted according to specific conditions; the design can ensure the effective transmission of the synthetic pressure and simultaneously avoid the damage of the groove part in the boosting process; through the design, when the synthesis cavity is used for preparing the diamond large single crystal by a high-temperature high-pressure method, the technical characteristics of the graphite tube heating body can be effectively utilized, the effective transmission of the synthesis pressure in the synthesis cavity is ensured, the increase of an auxiliary heat source can be reduced, the temperature gradient in the synthesis cavity can be reduced, the quality of the IIa type diamond large single crystal is improved, the volume in the cavity can be enlarged under the condition that the volume of the whole cavity is not changed, and the research and development directions of the diamond single crystal prepared by the high-temperature high-pressure method are compounded.
Drawings
Fig. 1 is a schematic structural diagram of a graphite tube heating body in the prior art.
Fig. 2 is a schematic structural diagram of a graphite tube heating body.
Fig. 3 is a schematic structural diagram of a diamond large single crystal synthesis cavity.
In the figure: 1-tube body A section, 2-tube body B section, 3-groove, 4-insulating ring, 5-pyrophyllite block, 6-quartz tube, 7-crystal bed, 8-crystal seed, 9-insulating tube, 10-metal catalyst, 11-graphite carbon source, 12-ceramic plug, 13-end plug and 14-graphite sheet.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Example 1
Referring to fig. 2, in an embodiment of the present invention, a graphite tube heating body includes a tube a section 1 and a tube B section, the tube a section 1 and the tube B section 2 may be an integrally formed graphite tube structure, the opening radii of the tube a section 1 and the tube B section 2 are the same, the length of the tube a section 1 is greater than the length of the tube B section 2, the tube B section 2 is close to the tube a section 1, a groove 3 of an annular structure is formed by cutting, when the total length of the tube a section 1 and the tube B section 2 is the same as the length of a conventional integrated graphite tube, the thickness of the cut groove 3 is thinner than that of the tube a section 1 and the tube B section 2, so that the resistance of the cut groove will increase, thereby also reducing the temperature gradient in a synthesis cavity, and further improving the quality of an IIa type diamond large single crystal, therefore, an auxiliary heat source is not needed to be added at the lower part of the graphite tube heating body.
Compare with integrative graphite pipe heating body among the prior art, traditional graphite pipe is because the reason of resistance, cause whole graphite pipe all to generate heat, and graphite pipe heating body central point puts to the temperature highest point, and by the temperature reduction gradually of center department to graphite pipe low temperature end, thereby produce a temperature difference T, the hypothesis has certain distance d from graphite pipe heating center to graphite pipe heating body both ends, thereby produce certain temperature gradient = T/d in vertical direction, when using traditional graphite pipe heating body to carry out the big single crystal preparation of IIa type diamond like this, just must increase auxiliary heat source on graphite pipe's basis, otherwise unable effectual completion processing.
However, gaps will appear around the cut part of the groove 3, which further affects the effective transmission of the synthetic pressure, and the reduction of the structural thickness of the part also affects the structural strength of the combination of the section a 1 of the tube body and the section B2 of the tube body, therefore, the periphery of the groove 3 is movably sleeved with an insulating ring 4, the insulating ring 4 is an integrally formed insulating ceramic ring or an insulating material ring formed by splicing two movably assembled parts, and the size of the insulating ring 4 is movably matched with that of the groove 3, so that the effective transmission of the synthetic pressure can be ensured, the breakage of the part of the groove 3 in the boosting process is also avoided, further the leakage is caused, the experiment and the production must be forcibly stopped, and the insulating ring is preferably made of insulating ceramic.
Example 2
Referring to fig. 3, in an embodiment of the present invention, a synthetic cavity of diamond large single crystal includes the graphite tube heating member as described in embodiment 1, and further includes an accommodating structure, the accommodating structure includes a quartz tube 6 sleeved on the periphery of the graphite tube heating member and a graphite sheet 14 attached to and fixed at the upper and lower ends of the quartz tube 6, the quartz tube 6 and the graphite sheet 14 are wrapped and fixed by a pyrophyllite block 5, and the upper and lower ends of the pyrophyllite block 5 are all embedded with end plugs 13, the end plugs 13 are attached to the graphite sheet 14 and fixed, so as to form limitation of movement.
The lower part is equipped with brilliant bed 7 in the graphite tube heating body, it is equipped with seed crystal 8 to fill in 7 tops of brilliant bed, just seed crystal 8 compresses tightly through the metal catalyst 10 of cover establishing in insulating tube 9, metal catalyst 10 upper end center has cylindrical arch, and protruding peripheral cover is equipped with graphite carbon source 11, it is provided with ceramic end cap 12 to fill in the graphite tube heating body of insulating tube 9, metal catalyst 10 and graphite carbon source 11 top.
Through the design, when the synthesis cavity is used for preparing the diamond large single crystal by a high-temperature high-pressure method, the technical characteristics of the graphite tube heating body can be effectively utilized, the effective transmission of the synthesis pressure in the synthesis cavity is ensured, the increase of an auxiliary heat source can be reduced, the temperature gradient in the synthesis cavity can be reduced, the quality of the IIa type diamond large single crystal is improved, the volume in the cavity can be enlarged under the condition that the volume of the whole cavity is not changed, and the research and development direction of preparing the diamond single crystal by the high-temperature high-pressure method is met.
The utility model discloses the standard parts that use all can purchase from the market, and dysmorphism piece all can customize according to the record of the description with the drawing.
It is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The utility model provides a graphite pipe heating member, includes body A section (1) and body B section (2), its characterized in that, body A section (1) with body B section (2) is fashioned graphite material tubular structure as an organic whole, body B section (2) are close to body A section's (1) one side periphery forms annular structure's recess (3) through the cutting, the peripheral movable sleeve of recess (3) is equipped with insulating ring (4).
2. A graphite tube heating body as claimed in claim 1, characterised in that the length of the tube a section (1) is greater than the length of the tube B section (2).
3. A graphite tube heating body as claimed in claim 1, characterized in that the insulating collar (4) is an integrally formed ring of insulating ceramic material.
4. A graphite tube heating body as claimed in claim 1, characterized in that the insulating collar (4) is a movably mounted two-part split ring of insulating material.
5. A graphite tube heating body as claimed in claim 1, characterized in that the insulating collar (4) and the groove (3) are dimensionally matched, said insulating collar being made of insulating ceramic material.
6. A large diamond monocrystal synthesis cavity comprises a containing structure and is characterized by further comprising a graphite tube heating body according to any one of claims 1 to 5, wherein the containing structure comprises a quartz tube (6) sleeved on the periphery of the graphite tube heating body and graphite sheets (14) attached and fixed to the upper end and the lower end of the quartz tube (6), the peripheries of the quartz tube (6) and the graphite sheets (14) are wrapped and fixed through pyrophyllite blocks (5), end plugs (13) are embedded into the upper end and the lower end of each pyrophyllite block (5), and the end plugs (13) are attached and fixed to the graphite sheets (14).
7. The cavity for synthesizing the large single crystal of diamond according to claim 6, wherein a crystal bed (8) is arranged at the inner lower part of the graphite tube heating body, a seed crystal (7) is filled above the crystal bed (8), the seed crystal (7) is compressed by a metal catalyst (10) sleeved in an insulating tube (9), a cylindrical protrusion is arranged at the center of the upper end of the metal catalyst (10), a graphite carbon source (11) is sleeved at the periphery of the protrusion, and a ceramic plug (12) is filled in the graphite tube heating body above the insulating tube (9), the metal catalyst (10) and the graphite carbon source (11).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921000836.6U CN210875234U (en) | 2019-06-28 | 2019-06-28 | Graphite tube heating body and diamond large single crystal synthesis cavity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921000836.6U CN210875234U (en) | 2019-06-28 | 2019-06-28 | Graphite tube heating body and diamond large single crystal synthesis cavity |
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| Publication Number | Publication Date |
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| CN210875234U true CN210875234U (en) | 2020-06-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201921000836.6U Expired - Fee Related CN210875234U (en) | 2019-06-28 | 2019-06-28 | Graphite tube heating body and diamond large single crystal synthesis cavity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041100A (en) * | 2022-07-22 | 2022-09-13 | 中南钻石有限公司 | Diamond synthetic block cultivated by multilayer permeation type structure large-particle single crystal and preparation process thereof |
-
2019
- 2019-06-28 CN CN201921000836.6U patent/CN210875234U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041100A (en) * | 2022-07-22 | 2022-09-13 | 中南钻石有限公司 | Diamond synthetic block cultivated by multilayer permeation type structure large-particle single crystal and preparation process thereof |
| CN115041100B (en) * | 2022-07-22 | 2023-09-15 | 中南钻石有限公司 | Multilayer infiltration type structure large particle single crystal cultivation diamond synthetic block and preparation process thereof |
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| CF01 | Termination of patent right due to non-payment of annual fee |