CN216514120U - Substrate table for preparing diamond film based on MPCVD method - Google Patents

Substrate table for preparing diamond film based on MPCVD method Download PDF

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CN216514120U
CN216514120U CN202123132689.8U CN202123132689U CN216514120U CN 216514120 U CN216514120 U CN 216514120U CN 202123132689 U CN202123132689 U CN 202123132689U CN 216514120 U CN216514120 U CN 216514120U
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groove
annular
central
diamond film
annular groove
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李庆利
甄西合
赵丽媛
刘得顺
朱逢锐
徐悟生
刘畅
徐超
张钦辉
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Tianjin Benzuan Technology Co ltd
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Henan Micron Optical Technology Co ltd
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Abstract

The utility model relates to the technical field of crystal synthesis, in particular to a substrate table for preparing a diamond film based on an MPCVD method, which comprises a molybdenum support and a deposition negative film arranged on the molybdenum support, wherein the upper end surface of the molybdenum support is provided with a growth groove for placing the deposition negative film, the lower end surface of the molybdenum support is provided with an annular groove, the central position of the annular groove is provided with a central bulge, the height of the central bulge is the same as the height of the edge of the annular groove, at least one annular block with a central circular hole is arranged in the annular groove, the inner diameter of the central circular hole of the annular block is larger than the diameter of the central bulge, the outer diameter of the annular block is smaller than the inner diameter of the annular groove, and the height of the annular block is the same as the height of the central bulge. The matching of the bottom annular groove and the annular block is adopted, so that the surface temperature uniformity of the film is favorably improved, and the quality of the film is improved.

Description

Substrate table for preparing diamond film based on MPCVD method
Technical Field
The utility model relates to the technical field of crystal synthesis, in particular to a substrate table for preparing a diamond film based on an MPCVD method.
Background
Diamond has very high hardness, and has excellent properties of very high thermal conductivity, low thermal expansion coefficient, high chemical inertness and the like at room temperature, and the excellent physical and chemical properties make the diamond receive wide attention. It can be widely applied to the fields of cutters, coatings, optical windows, acoustic sensors, semiconductors, electronic devices and the like. Therefore, the research on the preparation technology of uniformly growing the diamond film with high speed, high quality and large area is particularly urgent.
The Microwave Plasma Chemical Vapor Deposition (MPCVD) is a high-quality and easy-to-control method for artificially preparing diamond, and the basic principle is to use microwaves to excite plasmas in a mixed gas of low-molecular carbon hydrocarbon gas (such as methane) and hydrogen, and in the high-temperature environment of the plasmas, carbon atoms are deposited on a deposition substrate placed on a substrate table, so as to realize the artificial growth of a diamond film. The MPCVD method for preparing the diamond film uses electromagnetic wave energy to excite reaction gas, has the advantages of no electrode pollution, plasma concentration, difficult diffusion and the like, has excellent performance, is very suitable for growing high-quality diamond, is one of the most promising methods for synthesizing diamond at present, and is also considered as the first method for preparing the high-quality diamond film.
Microwave Plasma Chemical Vapor Deposition (MPCVD) devices generally include a microwave system, a vacuum system, a gas supply system, a cooling system, and a plasma reaction chamber, wherein the plasma reaction chamber is a key component of the MPCVD device, and includes a microwave plasma reaction chamber, a water cooling table, a substrate table, and other components. In the MPCVD device, the substrate table is placed on a water cooling table in a microwave plasma reaction cavity, and the design of the substrate table has important influence on the distribution and uniformity of an electric field and plasma in the reaction cavity and plays an important role in preparing high-quality diamond.
Typical substrate table designs employ a simple disk configuration with the deposition substrate placed on a flat support surface of the disk. Due to the influence of the edge effect, the electric field at the outer edge of the deposition substrate is stronger than that at the central area, so that the density distribution uniformity of plasma in the reaction cavity is influenced, and the grown diamond film has uneven thickness. Meanwhile, when the substrate table is applied to a large-area diamond film, the temperature of the center and the edge of the film is high due to the distribution of the plasma field, so that the integral temperature distribution is uneven, the quality of the film is influenced, the large-area film has large stress, and cracks are generated. Improving the uniformity of diamond films is also one of the difficulties in large-area diamond growth.
Chinese patent CN 103911596B discloses a substrate table with a high temperature resistant metal ring, which is located at the lower half part of the inside of a plasma sphere above the substrate table, near the boundary of the plasma sphere, and can change the plasma density distribution, thereby improving the deposition uniformity of diamond film. The structure needs to arrange a high-temperature resistant non-metal bracket around the substrate table, and the high-temperature resistant metal ring is fixedly connected with the non-metal bracket through a tungsten wire or a tantalum wire. The substrate table structure has the disadvantages that additional components such as a non-metal bracket and the like are introduced, and the structure becomes complicated; in addition, in order to effectively improve the uniformity of the plasma ball, a positioning mechanism needs to be introduced to ensure that the bracket and the metal ring fixed on the bracket are accurately positioned, so that the complexity of the structure is further increased, the realization is difficult in practical application, and the positioning precision is difficult to ensure.
Chinese patent CN106929828A discloses a substrate table for preparing diamond film by microwave plasma chemical vapor deposition method. The substrate table improves the uniformity of a plasma field by the inclined plane or arc shape of the annular edge, and prevents impurities generated in a non-deposition area from being sputtered onto a deposited diamond film by the design of the annular groove. However, in practical application, when the diamond film is large, the plasma field causes the temperature of the diamond film at the center and the edge to be higher than that of the middle annular area due to the edge inclination, so that the diamond generates stress.
Accordingly, there is a need in the art for an apparatus that can solve the problem of the molybdenum holder being heated unevenly by the configuration of the substrate table itself.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a device capable of reducing a plasma edge effect of a plasma in a microwave plasma reactor on a molybdenum torr, improving temperature distribution uniformity of the molybdenum torr, and improving quality of a diamond film.
In order to achieve the above purposes, the technical scheme adopted by the utility model is as follows: a substrate table for preparing a diamond film based on an MPCVD method comprises a molybdenum support and a deposition film arranged on the molybdenum support, wherein a growth groove for placing the deposition film is arranged on the upper end surface of the molybdenum support, an annular groove is arranged on the lower end surface of the molybdenum support, a central bulge is arranged at the central position of the annular groove, the height of the central bulge is the same as the height of the edge of the annular groove, at least one annular block with a central circular hole is arranged in the annular groove, the inner diameter of the central circular hole of the annular block is larger than that of the central bulge, the outer diameter of the annular block is smaller than that of the annular groove, and the height of the annular block is the same as that of the central bulge.
In the above substrate table for preparing a diamond film based on the MPCVD method, the molybdenum holder is a flat cylinder, the central axis of the central protrusion coincides with the central axis of the growth groove, the central axis of the central protrusion coincides with the central axis of the molybdenum holder, the height of the molybdenum holder is smaller than the height of the groove edge of the growth groove, and the diameter of the molybdenum holder is smaller than the inner diameter of the growth groove.
In the above substrate table for preparing a diamond film based on the MPCVD method, the outer diameter of the growth groove is smaller than the outer diameter of the annular groove.
In the substrate table for preparing the diamond film based on the MPCVD method, the outer edge of the groove edge at the outer side of the growth groove is provided with the fillet, and the width of the groove edge of the growth groove is larger than that of the groove edge of the annular groove.
The substrate table for preparing the diamond film based on the MPCVD method has the annular block as an integral structure.
The substrate table for preparing the diamond film based on the MPCVD method has the beneficial effects that: the cooperation of bottom ring channel and annular piece is adopted, be favorable to improving the equal nature of surface temperature of membrane, thereby improve the quality of membrane, the substrate platform is independent of cavity and the copper water-cooling dish of microwave plasma reactor, it is simple easy-to-use, be favorable to adjusting structure and size at any time, be favorable to preparing the diamond membrane of various not unidimensional, adopt the design of the outer annular surface edge radius angle of growth groove, the effectual plasma edge effect that has weakened, the effectual plasma ball subsection state that has improved in the MPCVD device, the homogeneity of its distribution has been improved, the homogeneity and the quality of the diamond membrane of preparation have been improved simultaneously.
Drawings
FIG. 1 is a schematic view of the overall cross-sectional structure of the present invention;
FIG. 2 is a schematic diagram of the structure of the present invention placed on a water cooling table;
FIG. 3 is a schematic diagram of the temperature distribution of a diamond film in a plasma;
FIG. 4 is a schematic view of the construction of the annular block of the present invention;
FIG. 5 is a schematic view of a single annular block placement position according to the present invention;
FIG. 6 is a schematic view of the placement of the double ring blocks of the present invention.
In the figure, a substrate table 1, a molybdenum support 2, a deposition negative plate 3, a growth groove 4, an annular groove 5, a central bulge 6, an annular block 7, a central round hole 8, a fillet 9, a water cooling table 10, an air exhaust pipeline 11, a plasma ball 12, a central area 13, a transition area 14, an edge area 15, an annular groove edge 16 and a growth groove edge 17.
Detailed Description
In order to make the technical solution better understood by those skilled in the art, the technical solution of the present invention is described below with reference to the specific embodiments and the accompanying drawings.
As shown in fig. 1-6, a substrate table for preparing a diamond film based on an MPCVD method comprises a molybdenum holder, the molybdenum holder is a flat cylinder, the outer edge of the outermost side above the molybdenum holder is provided with a rounded corner, a deposition negative is placed on the molybdenum holder, the deposition negative is also a flat cylinder, a growth groove for placing the deposition negative is dug inwards on the upper end surface of the molybdenum holder, the height of the deposition negative is less than or equal to the height of the groove edge of the growth groove, and the diameter of the deposition negative is less than the inner diameter of the growth groove.
The lower end surface of the molybdenum support is internally provided with an annular groove in a buckling manner, a central bulge is arranged at the central position of the annular groove, the height of the central bulge is the same as that of the groove edge of the annular groove, one or two or more than two annular blocks with a central round hole are arranged in the annular groove, the inner diameter of the central round hole of each annular block is larger than that of the central bulge, the outer diameter of each annular block is smaller than that of the annular groove, the height of each annular block is the same as that of the central bulge, according to different temperature requirements, each annular block can be provided with one or more than two annular blocks, when two annular blocks are arranged, each annular block is divided into an annular block with a large inner diameter and an annular block with a small inner diameter, the outer diameter of the annular block with a large inner diameter is tangent to the inner diameter of the annular groove, the inner diameter of the annular block with a small inner diameter is tangent to the outer diameter of the central bulge, a second annular groove area which is not filled with the annular blocks is formed between the two annular blocks, and the material of the molybdenum support is the same as that of the molybdenum support, each annular block is of an integral annular structure.
The central axis of the central bulge, the central axis of the growing groove and the central axis of the annular block are all superposed with the central axis of the molybdenum support, and the four central axes are positioned on the same central axis.
The outer diameter of a growing groove formed in the upper side of the molybdenum support is smaller than that of an annular groove formed in the lower side of the molybdenum support, and the width of the groove edge of the growing groove is the same as that of the groove edge of the annular groove.
Furthermore, in order to adjust and control the temperature of the transition region better, the width of the groove edge of the growth groove is larger than that of the groove edge of the annular groove.
The molybdenum support is placed in the annular groove, the annular block is integrally placed on the water cooling table, the water cooling table can be made of copper, when the diamond film grows, in the plasma above the substrate table, the plasma is an oval sphere, the temperature of the central area is highest, the temperature of the edge area is second, the temperature of the transition area is lowest, the temperature distribution of the transition area is higher than that of the middle part of the transition area due to the fact that the edge fillet of the substrate table discharges, and the temperature of the transition area is lower, so when the large-size diamond film grows, the temperature difference between the central area, the edge area and the transition area of the diamond film is larger, and the quality of the diamond film grown in each area is different.
At the moment, the transition region at the bottom of the molybdenum support for placing the deposition film on the substrate table is dug into an annular inner groove, so that the contact between the transition region and the lower water-cooling copper table is reduced, the water-cooling heat dissipation effect is reduced, the water-cooling heat dissipation condition of the substrate table is adjusted, and the temperature of the region is increased. The temperature distribution of the transition area is high on two sides and low in the middle, the temperature difference of each area is smaller in order to enable the temperature of the diamond film to be more uniform, and the temperature of the diamond film can be more flexibly adjusted to be consistent through the annular block, so that the temperature uniformity of the diamond film can be adjusted.
The ring blocks are typically disposed at a location where the ring grooves are near the middle. The number is 6, and the three groups are divided into three groups (the three groups are different in the width of the annular block). According to the actual temperature distribution condition of the substrate table in the plasma, different annular blocks are flexibly used, so that the temperature is more uniform and consistent.
The larger the diamond film is, the higher the temperature of the central area is, the edge discharge phenomenon is weakened, at the moment, the annular block does not need to be added in the annular groove at the outer side of the molybdenum support growth groove, only the annular block needs to be added at the inner side of the annular groove, the water cooling and heat dissipation condition is adjusted, and the uniform and consistent effect of adjusting the temperature of the diamond film is achieved.
According to the utility model, the design of rounding the edge of the annular outer surface is adopted, so that the edge effect of the plasma is effectively weakened, the plasma spherical distribution state in the MPCVD device is effectively improved, the distribution uniformity is improved, and the uniformity and the quality of the prepared diamond film are improved.
The molybdenum support on the substrate table is independent of the cavity and the copper water-cooling disc, is simple and easy to use, is beneficial to adjusting the structure and the size at any time, and is beneficial to preparing diamond films with various sizes.
The design of the substrate table is suitable for MPCVD devices with various microwave frequencies (915MHz/2450MHz) and various reaction cavities, improves the distribution uniformity of electric fields and plasmas in large-size MPCVD devices, is suitable for preparing large-area diamond films, and improves the uniformity and quality of the prepared diamond films.
The cooperation of the bottom annular groove and the annular block is favorable for improving the surface temperature uniformity of the film, thereby improving the quality of the film.
The utility model has the advantages of ingenious design, simple structure and low cost, and is suitable for various MPCVD devices.
The method for preparing the diamond film by using the substrate table and adopting the microwave plasma chemical vapor deposition method comprises the following steps:
1. carrying out surface treatment on a deposition substrate (silicon wafer), and then carrying out ultrasonic cleaning;
2. opening an MPCVD reaction cavity cover, placing a proper annular block into an annular groove on a molybdenum support of a substrate table, placing the molybdenum support in the middle of a copper water cooling table, and placing a treated deposition substrate (silicon wafer) into a growth groove of the molybdenum support;
3. closing the reaction cavity cover, opening the mechanical pump, and vacuumizing until the vacuum in the reaction cavity is 0.01-0.4 pa;
4. measuring the air leakage rate in the reaction cavity, ensuring the air leakage rate to be 0.01-0.1pa/min, and recording the air leakage rate;
5. introducing high-purity hydrogen with the mass flow of 500sccm, starting the microwave when the air pressure of the reaction chamber is 200-3000pa, inputting and adjusting the power to be 1-3KW, and starting the glow to generate a plasma ball when the microwave frequency is 915MHZ/2.45 GHZ;
6. continuously introducing hydrogen with the mass flow of 500sccm, adjusting the air pressure in the reaction chamber to 10-13KPa, simultaneously adjusting the microwave input power to 6-30KW, and starting introducing hydrocarbon gas when the temperature of the deposition substrate reaches 800-;
7. adjusting various process parameters of the MPCVD device to prepare the diamond, wherein the microwave output power is 6-30KW, the air pressure of the reaction cavity is 10-20Kpa, and the temperature of the deposition substrate is 700-;
among the above process parameters. The deposition rate of the diamond film is 1-20 microns/hour, and the diamond film with the thickness of 0.1-2mm is obtained after 30-200 hours of growth.
8. And (5) after the diamond deposition is finished, taking out the sample, closing the reaction cover, and continuously vacuumizing.
The above-mentioned embodiments are only for illustrating the structural conception and the characteristics of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and to implement the present invention, and the protection scope of the present invention is not limited thereby. All equivalent changes or modifications made according to the spirit of the present disclosure should be covered within the scope of the present disclosure.

Claims (5)

1. A substrate table for preparing a diamond film based on an MPCVD method comprises a molybdenum holder and a deposition negative film placed on the molybdenum holder, wherein the upper end surface of the molybdenum holder is provided with a growth groove for placing the deposition negative film, and the substrate table is characterized in that: the molybdenum support is characterized in that an annular groove is formed in the lower end face of the molybdenum support, a central bulge is formed in the center of the annular groove, the height of the central bulge is the same as that of the edge of the annular groove, at least one annular block with a central circular hole is arranged in the annular groove, the inner diameter of the central circular hole of each annular block is larger than the diameter of the central bulge, the outer diameter of each annular block is smaller than the inner diameter of the annular groove, and the height of each annular block is the same as that of the central bulge.
2. The substrate stage for producing a diamond film according to claim 1, which comprises: the deposition negative plate is in a flat cylindrical shape, the central axis of the central bulge coincides with the central axis of the growth groove, the central axis of the central bulge coincides with the central axis of the deposition negative plate, the central axis of the central bulge coincides with the central axis of the molybdenum support, the height of the deposition negative plate is smaller than the height of the groove edge of the growth groove, and the diameter of the deposition negative plate is smaller than the inner diameter of the growth groove.
3. The substrate stage for producing a diamond film according to claim 1, which comprises: the outer diameter of the growing groove is smaller than that of the annular groove.
4. The substrate stage for producing a diamond film according to claim 1, which comprises: the outer edge of the outer side groove edge of the growth groove is provided with a fillet, and the width of the groove edge of the growth groove is larger than that of the groove edge of the annular groove.
5. The substrate stage for producing a diamond film according to claim 1, which comprises: the annular block is of an integrated structure.
CN202123132689.8U 2021-09-02 2021-12-14 Substrate table for preparing diamond film based on MPCVD method Active CN216514120U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115506014A (en) * 2022-09-27 2022-12-23 四川本钻科技有限公司 Substrate table for single crystal diamond crystal growth and use method thereof
CN115558902A (en) * 2022-10-26 2023-01-03 武汉莱格晶钻科技有限公司 Substrate table suitable for diamond growth and use method thereof
CN116180057A (en) * 2023-03-07 2023-05-30 成都沃特塞恩电子技术有限公司 MPCVD system

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115506014A (en) * 2022-09-27 2022-12-23 四川本钻科技有限公司 Substrate table for single crystal diamond crystal growth and use method thereof
CN115558902A (en) * 2022-10-26 2023-01-03 武汉莱格晶钻科技有限公司 Substrate table suitable for diamond growth and use method thereof
CN116180057A (en) * 2023-03-07 2023-05-30 成都沃特塞恩电子技术有限公司 MPCVD system

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Effective date of registration: 20240112

Address after: 300380 102, R & D building, Digital Science Park, No. 27, Xingguang Road, Zhongbei Town, Xiqing District, Tianjin

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