CN211771655U - High-quality diamond growth tray and growth system - Google Patents

High-quality diamond growth tray and growth system Download PDF

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CN211771655U
CN211771655U CN201922419930.1U CN201922419930U CN211771655U CN 211771655 U CN211771655 U CN 211771655U CN 201922419930 U CN201922419930 U CN 201922419930U CN 211771655 U CN211771655 U CN 211771655U
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diamond
growth
substrate table
hole
upper substrate
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彭国令
黄翀
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Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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Changsha New Material Industry Research Institute Co Ltd
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Abstract

The utility model relates to a high quality diamond growth tray and growth system. A high-quality diamond growth tray comprises an upper substrate table and a lower substrate table, wherein the upper substrate table is provided with a plurality of through holes; the through hole penetrates through the upper substrate table; the lower base plate table is provided with a lower base plate and a plurality of convex columns, and the convex columns correspond to the through holes one to one. Use this novel seed crystal tray that provides, can guarantee that diamond seed crystal growth environment is stable, reduce surface growth defect quantity, finally synthesize high-quality single crystal diamond piece, cooperate corresponding diamond growth method, newly-grown diamond grows with the stratiform, the diamond piece after cutting separation can reach optics level diamond.

Description

High-quality diamond growth tray and growth system
Technical Field
The utility model relates to a diamond growth field especially relates to a high quality diamond growth tray and growth system.
Background
The high-quality diamond has high forbidden band width and wide optical transmission spectrum, and simultaneously has ultrahigh hardness and thermal conductivity, excellent insulativity, excellent acid resistance, heat resistance, radiation resistance and other excellent physicochemical properties, and can be applied to the fields of precision machining, optical windows, gems, MEMS, chips and the like. However, the reserves of high quality natural diamond are limited, and thus various synthetic diamond methods such as high temperature and high pressure method, hot wire chemical vapor deposition method have been developed. In the method for synthesizing diamond by MPCVD (Microwave plasma chemical vapor deposition), diamond with high quality and large area can be synthesized theoretically because no impurities are introduced.
The quality of diamond synthesized by the MPCVD method is related to various factors, including carbon source concentration, gas flow, temperature, substrate table height, seed crystal tray shape, microwave power, synthesis temperature and the like. The temperature difference between the edge of the seed crystal tray and the diamond seed crystal is about 200 ℃ due to high temperature, and impurities such as carbon black and the like bonded by SP2 bonds are easily grown under the condition of plasma containing a carbon source. Along with the long-time running growth, the thickness of impurities at the edge of the seed crystal tray is increased, the bonding force of the seed crystal tray is poor, and the seed crystal tray is easy to warp from the tray and even peels off. The occurrence of the phenomenon has great harm to the stable growth of the diamond, and is mainly shown in the following aspects: firstly, the surface of diamond is seriously polluted by the peeling of impurities such as carbon black and the like to form surface defects, and further growth can form inclusion or polycrystal to influence the growth quality; secondly, when the impurities such as carbon black warp, the plasma distribution, the electric field distribution, the temperature distribution and the like in the vacuum cavity are influenced, so that the stress of the product is increased, the growth rate is reduced, the optical performance is reduced and other irreversible damages are caused.
The patent CN1296528C mentions that the rough river light improves the cavity and the seed crystal tray, the seed crystal can move up and down in the seed crystal tray after the improvement, the seed crystal is wrapped by the sheath, the seed crystal is gradually reduced along with the increase of the thickness, the heat dissipation efficiency of the seed crystal can be increased after the seed crystal is clamped by the edge of the sheath, but the proposal has good effect on the growth of the single crystal diamond, but is not suitable for the mass production of the diamond. The seed crystal tray is improved from an open type structure (open type) to a closed type structure (closed type), and the change of the mode can effectively increase the plasma density on the surface of the seed crystal, ensure that the epitaxial surface of the seed crystal has smooth appearance and obviously reduce the defect density. But is not suitable for mass production of diamond. Shreya Nad and J.Asmussen et al, university of Michigan, by designing grooves of a seed tray, verify that a pocket type structure (pocket holder) has a better effect than a traditional open type structure (open type) in the aspects of surface morphology and sample quality of synthetic diamond, and is particularly reflected in the aspect of growth of diamond four-side polycrystal. The design mode of the substrate table can effectively inhibit the growth of diamond seed crystal four-edge/corner polycrystal by avoiding edge discharge and four-corner tip discharge to cause overlarge local plasma density, but is not suitable for mass production of diamond. The substrate table proposed by singapore IIA in patent SG11201406391YA can synthesize a plurality of single crystal diamonds, but this poses a great challenge to the problem of drift of the plurality of single crystals inside and the problem of temperature uniformity.
Thus, the prior art has shortcomings and needs to be improved and enhanced.
SUMMERY OF THE UTILITY MODEL
In view of the foregoing prior art, an object of the present invention is to provide a high quality diamond growth tray and growth system, which can reduce the formation of defects in the process of growing diamond, ensure the high quality growth of diamond, and perform batch production simultaneously.
In order to achieve the purpose, the utility model adopts the following technical proposal:
a high-quality diamond growth tray comprises an upper substrate table and a lower substrate table, wherein the upper substrate table is provided with a plurality of through holes; the through hole penetrates through the upper substrate table; the lower base plate table is provided with a lower base plate and a plurality of convex columns, and the convex columns correspond to the through holes one to one.
Preferably, the through hole has a first hole portion and a second hole portion, the first hole portion is in the shape of an inverted circular truncated cone or an inverted truncated cone, and the second hole portion is a cylinder having a cross section identical to the ground shape of the first hole portion.
Preferably, in the high quality diamond growth tray, the inner surface of the through hole and the outer surface of the convex column are of smooth design.
Preferably, the convex column and the second hole part have the same shape, the cross section of the convex column and the cross section of the second hole part are the same, and the height of the convex column is 1-2mm smaller than that of the through hole.
Preferably, in the high quality diamond growth tray, an angle between a side surface of the first hole portion of the through hole and an upper plane of the upper substrate table is 0 to 90 °.
Preferably, the high-quality diamond growth tray has an upper base on which the through-hole is provided.
Preferably, in the high quality diamond growth tray, an angle between a side surface of the upper stage and a surface of the upper substrate stage is 0 to 90 °.
Preferably, in the high quality diamond growth tray, the surface of the upper substrate table is roughened by sand blasting.
Preferably, the lower substrate table is fixedly arranged on a water cooling table.
A high quality diamond growth system uses the tray.
Compared with the prior art, the utility model provides a pair of high quality diamond growth tray and growth system uses this novel seed crystal tray that provides, can guarantee that diamond seed crystal growth environment is stable, reduces surface growth defect quantity, finally synthesizes high-quality single crystal diamond piece, cooperates corresponding diamond growth method, and the diamond of new growth grows with the stratiform to progressively grow thickly, the diamond piece after cutting separation can reach optics level diamond, the requirement of electron level even.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of a growth tray provided by the present invention;
fig. 2 is a schematic structural diagram of another embodiment of the growth tray provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the following description of the present invention will refer to the accompanying drawings and illustrate embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
Referring to fig. 1-2, the present invention provides a high quality diamond growth tray, which comprises an upper substrate table 1 and a lower substrate table 2, wherein the upper substrate table 1 has a plurality of through holes 11; the through hole 11 penetrates through the upper substrate table 1; the lower substrate table 2 has a lower substrate 21 and a plurality of protruding columns 22, and the protruding columns 22 correspond to the through holes 11 one by one.
Specifically, the upper substrate table 1 and the lower substrate table 2 are used in combination, and the materials of the two are common materials in the art, and are not particularly limited. The through holes 11 are all arranged for bearing seed crystals for diamond growth, the shape of the through holes is set according to the requirement of diamond growth, for example, the through holes are required to be square, and end holes of the through holes 11 are square; generally, the tray can complete corresponding functions only by the upper substrate table 1, but if a diamond growth process is desired, the growth surface of the seed crystal is always in the optimal growth position, if the diamond growth method is an MPCVD method, the optimal growth position cannot be changed under the condition that all growth parameters are not changed, the optimal growth position can be determined as long as the position of the upper substrate table 1 is fixed, and at the moment, the growth surface of the seed crystal can be always in the optimal growth position only by adjusting the height of the seed crystal according to a certain rule; in the tray provided by the invention, the through hole 11 penetrates through the upper substrate table 1, meanwhile, the lower substrate table 2 is provided with the convex column 22, the convex column 22 is matched with the through hole 11, and the growth surface of the seed crystal can be ensured to be always in the optimal growth position by only ensuring the position of the upper substrate table 1 to be fixed and adjusting the height of the lower substrate table 2.
Specifically, the diameter of the through hole 11 is determined according to the effective growth area of the diamond to be grown, and the maximum diameter is not more than 55 mm. Auxiliary heat dissipation materials such as filaments and sheets can be firstly placed in the through hole 11, the filament sheets are made of high-temperature resistant (1400 degrees) materials such as molybdenum and nickel, and the purpose of placing the heat conduction materials is mainly to adjust the growth temperature of the seed crystal so as to be suitable for growth.
Preferably, in this embodiment, the through hole 11 includes a first hole 111 and a second hole 112, the first hole 111 is a circular truncated cone or an inverted circular truncated cone, and the second hole 112 is a column having a cross section identical to a ground surface of the first hole 111. For example, if the first hole portion 111 is rounded, the second hole portion 112 is cylindrical, and the cross-sectional area of the second hole portion 112 is the same as the area of the lower bottom surface of the first hole portion 111. The lower bottom surface of the inverted frustum of the first hole 111 is connected to the second hole 112, the first hole has a height of 1/3-1/2 of the total thickness of the upper substrate stage 1, and the second hole 112 has a height of 1/2-2/3 of the total thickness of the upper substrate stage 1. Preferably, the first hole 111 is a truncated cone or a regular polygonal frustum; the second hole 112 is a cylinder or a regular polygonal prism.
Preferably, in the present embodiment, the inner surface of the through hole 11 and the outer surface of the convex pillar 22 are designed to be smooth.
Preferably, in this embodiment, the shape of the protruding pillar 22 is the same as that of the second hole portion 112, and the cross section of the protruding pillar 22 is the same as that of the second hole portion 112, and the height of the protruding pillar 22 is 1-2mm smaller than that of the through hole 11. The cross sections are the same, and the shape and the area are the same. Further, the shape of the convex column 22 is the same as that of the second hole of the through hole, and the size of the convex column is slightly smaller than that of the second hole. Further, the distance between the convex column 22 and the upper surface of the upper base is less than 2mm after the convex column 22 is matched with the second hole part, and further preferably, the distance between the convex column 22 and the upper surface of the upper base is less than 1mm after the convex column 22 is matched with the second hole part. In this way, the height of the seed crystal can be better controlled.
Preferably, in this embodiment, an angle between a side surface of the first hole portion 111 of the through hole 11 and an upper plane of the upper substrate stage 1 is 0 to 90 °. The preferred angle is 30-60 °. When the angle between the side surface of the first hole 111 and the upper plane of the upper substrate stage 1 is 0, that is, the first hole 111 does not exist; when the angle between the side surface of the first hole 111 and the upper plane of the upper substrate stage 1 is 90 °, that is, the first hole 111 does not exist, the angle between the side surface of the first hole 111 and the upper plane of the upper substrate stage 1 is 0 to 90 °, excluding 0 ° and 90 °.
Preferably, in this embodiment, the upper substrate stage 1 has an upper base 12, the upper base 12 is in a circular truncated cone shape, and the plurality of through holes 11 are all provided on the upper base 12. The through hole is provided on the upper base 12. The upper substrate table 1 is circular in cross section. Specifically, the shape of the upper substrate table 1 may be designed according to specific production and processing conditions, and is preferably a circular shape, but may be a square shape.
Preferably, in this embodiment, an angle between the side surface of the upper base 12 and the upper substrate stage 1 is 0 to 90 °, and a preferable angle is 30 to 60 °. The inclination angle formed by the side surface of the upper base station 12 and the upper substrate station 1 can change the distribution of an electric field and plasma, the temperature distribution in the through hole 11 on the upper base station 12 is more uniform, the heat dissipation effect of the seed crystal tray is increased, the growth rate of impurities such as carbon black and the like at the position of the upper base station 12 is obviously reduced, and meanwhile, the shape of a plasma ball can be changed by an outer ring of the upper substrate station 1 after the upper base station 12 is removed, so that the density of the plasma is more uniform in the groove (namely above the seed crystal). In addition, when the angle between the side surface of the upper base 12 and the upper substrate stage is 90 °, that is, the upper base 12 is not a truncated cone and is cylindrical; when the angle between the side surface of the upper base 12 and the upper substrate stage is 0 °, that is, the upper base 12 does not exist, the angle between the side surface of the upper base 12 and the upper substrate stage is 0 ° to 90 °, excluding 0 °, but including 90 °.
Preferably, in this embodiment, the surface of the upper substrate stage 1 is roughened by sandblasting. The roughening treatment mode can be realized by sand blasting or machining (physical grinding), and the deposition of impurities such as carbon black at the position can be remarkably delayed.
Preferably, in this embodiment, the lower substrate stage 2 is fixedly mounted on the water-cooled stage 3. The total thickness of the tray provided by the present invention (the sum of the thicknesses of the upper substrate stage 1 and the lower substrate stage 2) is 8 to 12 mm. The diameter of the tray is consistent with that of the water cooling table 3.
To sum up, the utility model provides a tray has following effect:
1) through the newly designed seed crystal tray, the growth rate of impurities such as carbon black at the edge of the seed crystal tray can be obviously reduced, the stable growth time of a single time is longer, thicker products can be grown at one time, and the production efficiency is improved.
2) The newly designed seed crystal tray can repair the surface defects, reduce the number of the surface defects and finally synthesize high-quality single crystal diamond chips. The newly grown diamond grows in layers and grows gradually, and the diamond sheet after cutting and separation can meet the requirements of optical-grade diamond and even electronic grade diamond.
3) Through the newly designed seed crystal tray, a plurality of diamonds are produced in batch, the purposes of fixing a single-crystal diamond and adjusting the single-crystal diamond are achieved, meanwhile, the growth rate of the diamond is not reduced, the growth rate is still maintained at a high growth rate, and the method is very suitable for industrial stable production.
4) Through the newly designed seed crystal tray, the growth of edge polycrystal can be effectively inhibited, the accumulation of growth stress is reduced, and the seed crystal stress is released.
Example 2
A high-quality diamond growth system is based on the MPCVD normal growth system, and the tray for growing diamond is the tray provided by the invention. Wherein, the diamond is produced by the MPCVD method, the pretreatment process before the diamond synthesis is as follows, firstly, selecting the seed crystal with smooth surface, the growth surface is (100) surface, and polishing the surfaceAnd cleaning organic matters on the surface of the seed crystal by using acetone or absolute ethyl alcohol, carrying out acid cleaning treatment by using the prepared piranha solution to remove metal impurities on the surface of the seed crystal, washing away acid liquor by using deionized water, and then drying and putting the seed crystal into a cavity for growth. H is first introduced before growth2And under the pressure of 2-20mabr, introducing 300-1500KW glow starter to generate plasma, then gradually increasing the pressure and power to make the seed crystal stable at the temperature of 850-1000 ℃ and etching for 15-60 min. Introducing CH with a certain proportion after etching4And the seed crystal is stabilized at 900-1300 ℃ to start growing.
In the diamond growth process, firstly, the optimal position for diamond growth is determined, the upper substrate table 1 is fixed at the optimal position, then, in the diamond growth process, the height of the lower substrate table 2 is controlled to be reduced according to the diamond growth speed, and the growth surface of the diamond can be kept at the optimal growth surface at any time.
It should be understood that equivalent alterations and modifications can be made by those skilled in the art according to the technical solution of the present invention and the inventive concept thereof, and all such alterations and modifications should fall within the scope of the appended claims.

Claims (10)

1. A high-quality diamond growth tray is characterized by comprising an upper substrate table and a lower substrate table, wherein the upper substrate table is provided with a plurality of through holes; the through hole penetrates through the upper substrate table; the lower base plate table is provided with a lower base plate and a plurality of convex columns, and the convex columns correspond to the through holes one to one.
2. A high quality diamond growth tray according to claim 1 wherein said through hole has a first hole portion which is in the shape of an inverted truncated cone or inverted truncated cone and a second hole portion which is a cylinder having the same cross section as the ground of said first hole portion.
3. A high quality diamond growth tray according to claim 2 wherein the inner surface of the through hole and the outer surface of the post are of smooth design.
4. A high quality diamond growth tray according to claim 3 wherein said post is the same shape as said second aperture and said post has the same cross section as said second aperture and a height less than 1-2mm of the height of said through hole.
5. A high quality diamond growth tray according to claim 2 wherein the angle between the side of the first hole section of the through hole and the upper plane of the upper substrate table is 0-90 °.
6. A high quality diamond growth tray according to claim 1 wherein said upper substrate table has an upper base platform, said upper base platform being in the shape of a circular truncated cone, and a plurality of said through holes being provided on said upper base platform.
7. A high quality diamond growth tray according to claim 6 wherein the angle between the side of the upper abutment and the surface of the upper substrate table is 0-90 °.
8. A high quality diamond growth tray according to claim 7 wherein the surface of the upper substrate table is roughened by grit blasting.
9. A high quality diamond growth tray according to claim 1 wherein the lower substrate table is fixedly mounted on a water cooled table.
10. A high quality diamond growth system using the tray of any one of claims 1 to 9.
CN201922419930.1U 2019-12-27 2019-12-27 High-quality diamond growth tray and growth system Active CN211771655U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112609240A (en) * 2020-12-11 2021-04-06 哈尔滨工业大学 Method for improving heterogeneous epitaxial large-size nucleation uniformity of diamond based on composite structure sample stage
CN112831835A (en) * 2021-02-25 2021-05-25 廊坊西波尔钻石技术有限公司 Substrate table structure for diamond growth and use method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112609240A (en) * 2020-12-11 2021-04-06 哈尔滨工业大学 Method for improving heterogeneous epitaxial large-size nucleation uniformity of diamond based on composite structure sample stage
CN112609240B (en) * 2020-12-11 2022-05-24 哈尔滨工业大学 Method for improving heterogeneous epitaxial large-size nucleation uniformity of diamond based on composite structure sample platform
CN112831835A (en) * 2021-02-25 2021-05-25 廊坊西波尔钻石技术有限公司 Substrate table structure for diamond growth and use method thereof
CN112831835B (en) * 2021-02-25 2023-09-05 廊坊西波尔钻石技术有限公司 Substrate table structure for diamond growth and use method thereof

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Address after: 7th Floor, Building B8, Lugu Enterprise Plaza, Yuelu District, Changsha City, Hunan Province, 410000

Patentee after: Aerospace Science and Industry (Changsha) New Materials Research Institute Co.,Ltd.

Address before: 7 / F, building B8, luguyuyuan, 27 Wenxuan Road, high tech Development Zone, Changsha City, Hunan Province, 410205

Patentee before: CHANGSHA ADVANCED MATERIALS INDUSTRIAL RESEARCH INSTITUTE Co.,Ltd.