CN118028972A - TM multimode microwave plasma chemical vapor deposition device - Google Patents
TM multimode microwave plasma chemical vapor deposition device Download PDFInfo
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- CN118028972A CN118028972A CN202410120657.5A CN202410120657A CN118028972A CN 118028972 A CN118028972 A CN 118028972A CN 202410120657 A CN202410120657 A CN 202410120657A CN 118028972 A CN118028972 A CN 118028972A
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 73
- 238000000151 deposition Methods 0.000 claims abstract description 47
- 230000008021 deposition Effects 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010453 quartz Substances 0.000 claims abstract description 31
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- 238000000034 method Methods 0.000 claims abstract description 11
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- 239000010432 diamond Substances 0.000 claims description 48
- 229910003460 diamond Inorganic materials 0.000 claims description 48
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- 238000009826 distribution Methods 0.000 claims description 13
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- 238000009529 body temperature measurement Methods 0.000 claims description 2
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
A TM multimode microwave plasma chemical vapor deposition device belongs to the field of microwave plasma method chemical vapor deposition, and particularly relates to a TM multimode microwave plasma chemical vapor deposition device. Comprising the following steps: the microwave oven comprises a microwave power supply, a rectangular waveguide, a three-pin tuner, a short-circuit piston, a coaxial line mode converter, an annular quartz window, a non-cylindrical microwave resonant cavity, a temperature measuring window, an observation window, an air inlet, an air outlet, a cooling water gap, a deposition table, a lifting substrate table tuning structure and a bias electrode. The diameter of the upper cylindrical structure of the non-cylindrical microwave resonant cavity is smaller, so that a TM01 mode is generated; the lower cylindrical structure has a larger diameter for generating the TM02 mode. The TM01 and TM02 modes overlap at the substrate, exciting a large area, uniform plasma. The side surface of the cavity adopts an inclined plane structure, so that microwaves are focused at the substrate, and the electric field on the surface of the substrate is enhanced. Compared with the effective deposition area of 2 inches of a typical TM01 or TM02 single-mode device, the multi-mode device can realize plasma discharge with larger size, and the effective deposition area can be expanded to 4 inches.
Description
Technical Field
The invention belongs to the technical field of microwave plasma method chemical vapor deposition, and particularly relates to a TM multimode microwave plasma chemical vapor deposition device.
Technical Field
The diamond film prepared by the Microwave PLASMA CHEMICAL Vapor Deposition (MPCVD) method has excellent optical, electrical, mechanical and thermal properties, so that the diamond film has wide application prospect in the traditional and emerging industries. MPCVD devices can be classified into 915MHz and 2.45GHz devices according to the frequency at which the microwave source is used. Typical dimensions of polycrystalline diamond films currently produced in 2.45GHz devices areIt is difficult to meet the application requirements of large-sized windows and heat sinks. Meanwhile, the size of the polycrystalline diamond film prepared by the 915MHz device has reachedCan meet the requirements of large-size heat sinks, infrared and microwave windows and other applications. However, 915MHz devices are expensive, and equipment costs are more than 10 times that of the same type of 2.45GHz device, which severely limits the large-scale application of large-sized diamond films in the above-mentioned fields.
On the other hand, in order to exert the application advantages of diamond in the key fields of ultraviolet detector, irradiation detector, field effect transistor, etc., large-size single crystal diamond of inch grade is required. Heteroepitaxial growth is an effective technique for preparing high quality large size single crystal diamond. The biasing technique plays a key role in the growth of heteroepitaxial single crystal diamond. The charged particles in the bias acceleration plasma bombard the non-diamond substrate, causing high density nucleation of diamond, and thus preparing large-size heteroepitaxial single crystal diamond on the Ir (100) substrate. Therefore, in considering the development design of the 2.45GHz device, it is necessary to consider the bias electrode part.
To sum up, in order to realize low equipment cost preparation and industrialization application of large-size polycrystalline diamond film and large-size single crystal diamond, a multimode coupled 2.45GHz MPCVD apparatus with bias electrode structure was developed by equipment structure design and optimization, and the size of the depositable diamond film was changed fromExpand to/>Or even/> Is significant for the development of MPCVD technology.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a TM multimode microwave plasma chemical vapor deposition device which can realize the uniform preparation of a high-quality large-area diamond film under the condition of high microwave input power, and has the advantages of high film deposition rate, good large-area uniformity, simple structure, good vacuum property, stable operation and easy control of parameters. The apparatus is additionally provided with a bias electrode for nucleation during heteroepitaxial single crystal diamond nucleation. Since the non-cylindrical microwave resonant cavity of the device is formed by two cylinders with different diameters, the cylindrical structures with the two specific diameters are used for generating electromagnetic field distribution with different modes. The diameter of the upper cylindrical structure is smaller, and the upper cylindrical structure is used for generating a TM01 mode in the microwave resonant cavity; the diameter of the lower cylindrical structure is larger, so that TM02 mode is generated in the microwave resonant cavity. The TM01/TM02 multimode mixing not only enhances the microwave electric field and increases the plasma density, but also makes the plasma more uniformly distributed over the substrate surface. The side surface of the cavity adopts an inclined plane structure, so that microwaves are focused at the substrate, and the electric field on the surface of the substrate is enhanced. Compared with the effective deposition area of 2 inches of a typical TM01 or TM02 single-mode device, the multi-mode device can realize plasma discharge with larger size, and the effective deposition area can be expanded to 4 inches.
In addition, the device is used for vacuum sealing a quartz medium window positioned below the substrate table, so that the problem of impurity pollution caused by etching a quartz ring by hydrogen plasma is solved, and the device can be used for preparing an electronic grade diamond film or a single crystal. The prepared electronic grade diamond can be widely applied to the field of semiconductors, such as high-frequency electronic devices, millimeter wave devices and the like, as an ultra-wide band gap semiconductor material. The technical scheme of the invention is as follows:
a TM multimode microwave plasma chemical vapor deposition device comprises a 2.45GHz microwave power supply, a rectangular waveguide, a three-pin tuner, a short-circuit piston, a coaxial line mode converter, an annular quartz window, a non-cylindrical microwave resonant cavity, a temperature measuring window, an observation window, an air inlet, an air outlet, a cooling water gap, a deposition table, a lifting substrate table tuning structure and a bias electrode, and is characterized in that:
The non-cylindrical resonant cavity, the annular quartz window and the deposition table form a complete vacuum chamber; the annular quartz window is positioned below the deposition table, and a vacuum chamber is formed by sealing the deposition table and the non-cylindrical resonant cavity through the rubber ring; the air inlets are positioned above the non-cylindrical resonant cavity, and are arranged at intervals of 90 degrees along the axial direction, and the total number of the air inlets is 4; the exhaust port is positioned at the radial center of the deposition table, and is axially arranged at intervals of 60 degrees, and the total number of the exhaust ports is 6; the lifting substrate table tuning structure can move up and down and is used for real-time tuning of a microwave electric field and plasma.
A microwave power supply positioned below the resonant cavity generates microwaves with the frequency of 2.45GHz, the microwaves are converted into TM modes from TE modes by a rectangular waveguide through a coaxial converter, and the TM modes enter the resonant cavity after passing through an annular quartz window. A stable standing wave is formed within the non-cylindrical resonant cavity and a strong electric field region is formed above the deposition station. The reaction gas is ionized and excited under the action of a strong electric field to form plasma, and the bias electrode provides a bias electric field for the substrate to strengthen diamond nucleation on the substrate, so that the growth of heteroepitaxial single crystal diamond is realized.
Further, the non-cylindrical microwave resonant cavity is made of stainless steel and is composed of two cylinders with different diameters. The diameter of the upper cylinder is smaller, and the upper cylinder is used for generating a TM01 mode in the microwave resonant cavity; the diameter of the lower cylinder is larger, so that TM02 mode is generated in the microwave resonant cavity. Diameter ratio of two cylindersTo meet the requirements for generating multiple resonant modes. The TM01/TM02 multimode mixing not only enhances the microwave electric field and increases the plasma density, but also makes the plasma more uniformly distributed over the substrate surface.
Further, the middle part above the non-cylindrical microwave resonant cavity is provided with 1 bias electrode for providing a bias electric field in the growth process of heteroepitaxial monocrystalline diamond to enhance diamond nucleation.
Further, the non-cylindrical microwave resonant cavity and the coaxial line mode converter are made of stainless steel, the annular quartz window is made of quartz glass with a relative dielectric constant of 4.2, and the tuning structure of the liftable substrate table is made of copper.
Further, 4 air inlets are arranged above the non-cylindrical microwave resonant cavity, and 6 air outlets are arranged at the radial center of the deposition table along the axial direction, so that the uniformity of distribution of reaction gas in the cavity in the diamond growth process is ensured.
Further, the non-cylindrical microwave resonant cavity is connected with the rectangular waveguide through the coaxial line mode converter.
Further, the annular quartz window is arranged below the deposition table and far away from the plasma area, so that plasma etching on the quartz medium window is avoided.
Further, a sealing groove is formed at the joint of the annular quartz window, the stainless steel non-cylindrical resonant cavity and the deposition table, the annular quartz window is placed in the sealing groove, and a fixed rubber ring is arranged between the annular quartz window and the inner wall of the stainless steel non-cylindrical resonant cavity and between the annular quartz window and the inner wall of the deposition table structure.
Furthermore, the tuning structures of the non-cylindrical microwave resonant cavity, the deposition table and the liftable substrate table are all cooled by water, so that local overheating is avoided, and long-time operation of equipment is ensured.
Further, in the non-cylindrical microwave resonant cavity, the upper cylinder and the lower cylinder are connected by adopting inclined planes, and the inclined planes and the horizontal line form an included angle of 167+/-1 degrees so as to reflect microwaves and collect the microwaves at the substrate.
Further, the included angle between the outermost inclined plane of the non-cylindrical microwave resonant cavity and the horizontal line is 75+/-1 degrees, so that microwaves are reflected to be collected at the substrate.
Further, the lifting type substrate table tuning structure adopts a design of up-and-down movement adjustment, performs microwave electric field and plasma tuning, enhances the microwave electric field and plasma density, optimizes the distribution of the microwave electric field and the plasma density above the substrate, and realizes uniform deposition of diamond.
The key of the implementation process of the invention is as follows:
The invention provides a TM multimode microwave plasma chemical vapor deposition device. The microwave oven mainly comprises a 2.45GHz microwave power supply, a rectangular waveguide, a three-pin tuner, a short-circuit piston, a coaxial line mode converter, an annular quartz window, a non-cylindrical microwave resonant cavity, a temperature measuring window, an observation window, an air inlet, an air outlet, a cooling water gap, a deposition table, a lifting substrate table tuning structure and a bias electrode. The non-cylindrical microwave resonant cavity is formed by two cylinders with different diameters, and the cylindrical structures with the two specific diameters are used for generating electromagnetic field distribution with different modes. The diameter of the upper cylinder is smaller, and the upper cylinder is used for generating a TM01 mode in the microwave resonant cavity; the diameter of the lower cylinder is larger, so that TM02 mode is generated in the microwave resonant cavity. Diameter ratio of two cylinders To meet the requirements for generating multiple resonant modes. The TM01/TM02 multimode mixing not only enhances the microwave electric field and increases the plasma density, but also makes the plasma more uniformly distributed over the substrate surface. The bias electrode provides a bias electric field during heteroepitaxial growth of single crystal diamond to enhance diamond nucleation. The side surface of the cavity adopts an inclined plane structure, so that microwaves are focused at the substrate, and the electric field on the surface of the substrate is enhanced. Compared with the effective deposition area of 2 inches of a typical TM01 or TM02 single-mode device, the multi-mode device can realize plasma discharge with larger size, and the effective deposition area can be expanded to 4 inches.
The annular quartz window is arranged below the deposition table and far away from plasma, so that plasma etching on the quartz medium window is avoided. The lifting substrate table tuning structure can move up and down and is used for tuning a microwave electric field and plasma in real time. The device is mainly used for preparing heteroepitaxial monocrystalline diamond and polycrystalline diamond films, and can realize high-quality uniform deposition of diamond monocrystalline or large-area films under high power and high cavity pressure.
The key point of generating plasma and carrying out heteroepitaxial single crystal diamond deposition is that: placing the substrate on a liftable substrate table, vacuumizing the chamber to 1.0X10 -1 Pa, introducing hydrogen and methane into the chamber after vacuumizing to a preset vacuum, and keeping the chamber pressure at 3000-16000Pa. And starting a 2.45GHz microwave power supply, and adjusting the output power to 0.6-5kW. The bias electrode provides a bias electric field to the substrate during nucleation. The tuning structure of the three pin tuner, the shorting piston and the liftable substrate table is adjusted to minimize the microwave reflection coefficient. The ideal plasma discharge state in the film deposition process is achieved. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Compared with the prior art, the invention has the following beneficial effects:
The invention provides a TM multimode microwave plasma chemical vapor deposition device, and compared with the traditional microwave plasma chemical vapor deposition device, the non-cylindrical microwave resonant cavity is formed by two cylinders with different diameters, and the cylinders with the specific diameters are used for generating electromagnetic field distribution with different modes. The diameter of the upper cylinder is smaller, and the upper cylinder is used for generating a TM01 mode in the microwave resonant cavity; the diameter of the lower cylinder is larger, so that TM02 mode is generated in the microwave resonant cavity. Diameter ratio of two cylinders To meet the requirements for generating multiple resonant modes. The TM01/TM02 multimode mixing not only enhances the microwave electric field and increases the plasma density, but also makes the plasma more uniformly distributed over the substrate surface. A tungsten bias electrode is located in the upper portion of the reactor chamber for providing a bias electric field during the growth of heteroepitaxial single crystal diamond to enhance nucleation of diamond on a heterogeneous substrate (e.g., ir, YSZ, or sapphire). The side surface of the cavity adopts an inclined plane structure, so that microwaves are focused at the substrate, and the electric field on the surface of the substrate is enhanced. Compared with the effective deposition area of 2 inches of a typical TM01 or TM02 single-mode device, the multi-mode device can realize plasma discharge with larger size, and the effective deposition area can be expanded to 4 inches.
The annular quartz window is arranged below the deposition table and far away from the plasma area, so that plasma etching on the quartz medium window is avoided. The film deposition rate is high, the large-area uniformity is good, the device is simple in structure, the vacuum property is good, the stable operation can be realized, and the parameters are easy to control. In addition, an inclined plane structure is adopted on the side surface of the resonant cavity, so that microwaves are focused at the substrate, and the electric field intensity of the surface of the substrate is enhanced. Meanwhile, the device introduces the bias electrode, and the bias electrode provides a bias electric field in the process of heteroepitaxial growth of single crystal diamond, so that nucleation of diamond at the substrate is enhanced, and the device can be used for preparing large-size heteroepitaxial single crystal diamond. The prepared heteroepitaxial single crystal diamond can be widely applied to the field of semiconductors such as ultraviolet detectors, irradiation detectors, field effect transistors and the like as an ultra-wide band gap semiconductor material.
Drawings
FIG. 1 is a schematic illustration of a TM multimode microwave plasma chemical vapor deposition apparatus;
Wherein: 1-2.45GHz microwave power supply; 2-rectangular waveguide; 3-three pin adapter; a 4-coaxial line mode converter; 5-shorting the piston; 6-an annular quartz window; 7-a deposition station structure; 8-a liftable substrate table tuning structure; 9-a non-cylindrical microwave resonant cavity; 10-viewing window; 11-a temperature measurement window; 12-bias electrodes; 13-air inlet; 14-exhaust port; 15-plasma.
FIG. 2 shows the result of the numerical simulation of the electric field intensity distribution of the TM multimode device according to the present invention, the substrate diameter is
FIG. 3 shows the result of numerical simulation of the electron density distribution of plasma based on the TM multimode device according to the present invention, the substrate diameter isThe potential of the bias electrode is +100deg.V, and the substrate and the metal resonant cavity are grounded.
FIG. 4 shows the result of numerical simulation of the electron density distribution of plasma based on the TM multimode device according to the present invention, the substrate diameter is
FIG. 5 is a comparison of results of numerically simulated electric field intensity distribution at a location above the substrate surface based on the TM multimode device proposed in the present invention and a typical TM01 mode and TM02 mode microwave plasma chemical vapor deposition device, with a simulation condition of microwave power 8000W. Numerical simulation results show that compared with typical TM01 mode and TM02 mode cylindrical microwave plasma chemical vapor deposition devices, the TM multimode device provided by the invention is characterized in thatThe electric field intensity distribution above the substrate surface was improved by 80% and 50%.
FIG. 6 is a comparison of results of numerical simulation of plasma electron density distribution at a location above a substrate surface based on a TM multimode device and typical TM01 mode and TM02 mode microwave plasma chemical vapor deposition devices according to the present invention, with simulation conditions of microwave power at 800W, 15000Pa. Numerical simulation results show that compared with typical TM01 mode and TM02 mode cylindrical microwave plasma chemical vapor deposition devices, the TM multimode device provided by the invention is characterized in that The plasma electron density above the substrate surface was increased by 72% and 23% and the uniformity was increased by 48% and 115%, respectively.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and specific embodiments:
As shown in the figure, the invention provides a TM multimode microwave plasma chemical vapor deposition device, and the mechanical structures of a microwave resonant cavity and a vacuum chamber are axisymmetrically distributed. Microwave energy generated by a 2.45GHz microwave power supply (1) propagates along a rectangular waveguide (2), is coupled through a coaxial line mode converter (4) and an annular quartz window (6) and enters a non-cylindrical microwave resonant cavity (9), and a three-pin tuner (3), a short-circuit piston (5) and a liftable substrate table tuning structure (8) are adjusted to minimize the microwave reflection coefficient. An air inlet (13) is arranged at the center above the non-cylindrical microwave resonant cavity (9), and 6 air outlets (14) are axially arranged at the radial center of the deposition table structure. The temperature measuring window (11) is used for measuring the temperature in real time in the diamond growth process, and the observation window (10) is used for observing the states of the plasma and the substrate.
Example 1
And placing the phi 60mm monocrystalline silicon substrate on a lifting substrate table tuning structure (8), vacuumizing a cavity to 1.0 multiplied by 10 -1 Pa, introducing H 2 serving as working gas into the resonant cavity after vacuumizing to a preset vacuum, and adjusting the cavity pressure to 2000Pa. And starting a 2.45GHz microwave power supply (1), gradually adjusting output power to 8000W, synchronously raising cavity pressure to 23kPa, and adjusting a three-pin tuner (3), a short-circuit piston (5) and a lifting substrate table tuning structure (8) to minimize the microwave reflection coefficient. And introducing CH 4 to deposit the diamond film. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Example 2
Will beThe monocrystalline silicon substrate is placed on a tuning structure (8) of a liftable substrate table, the chamber is vacuumized to 1.0 multiplied by 10 -1 Pa, H 2 is introduced into the resonant cavity after the chamber is vacuumized to a preset vacuum to serve as working gas, and the cavity pressure is adjusted to be 2000Pa. And starting a 2.45GHz microwave power supply (1), gradually adjusting output power to 8000W, synchronously raising cavity pressure to 20kPa, and adjusting a three-pin tuner (3), a short-circuit piston (5) and a lifting substrate table tuning structure (8) to minimize the microwave reflection coefficient. And introducing CH 4 to deposit the diamond film. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Example 3
Will beThe monocrystalline silicon substrate is placed on a tuning structure (8) of a liftable substrate table, the chamber is vacuumized to 1.0 multiplied by 10 -1 Pa, H 2 is introduced into the resonant cavity after the chamber is vacuumized to a preset vacuum to serve as working gas, and the cavity pressure is adjusted to be 2000Pa. And starting a 2.45GHz microwave power supply (1), gradually adjusting output power to 9000W, synchronously raising cavity pressure to 16kPa, and adjusting a three-pin tuner (3), a short-circuit piston (5) and a lifting substrate table tuning structure (8) to minimize the microwave reflection coefficient. And introducing CH 4 to deposit the diamond film. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Example 4
Placing the MgO substrate with the Ir film plated at 3inch on a tuning structure (8) of a liftable substrate table, vacuumizing a cavity to 1.0 multiplied by 10 -1 Pa, introducing H 2 into a resonant cavity after vacuumizing to a preset vacuum as working gas, and adjusting the cavity pressure to 2000Pa. And starting a 2.45GHz microwave power supply (1), gradually adjusting output power to 4500W, synchronously raising cavity pressure to 18kPa, and adjusting a three-pin tuner (3), a short-circuit piston (5) and a lifting substrate table tuning structure (8) to minimize microwave reflection coefficient. And (3) introducing CH 4, turning on a bias power supply to enable the potential of the bias electrode (12) to be 300V, and applying bias to the substrate to nucleate. After nucleation for 30min, the bias power supply is turned off, and the heteroepitaxial growth of the monocrystalline diamond is carried out. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Example 5
36 HTHP diamond seed crystal substrates with the diameter of 10mm multiplied by 10mm are arranged on a lifting substrate table tuning structure (8) according to the arrangement of 6 multiplied by 6, the chamber is vacuumized to 1.0 multiplied by 10 -1 Pa, H 2 is introduced into the resonant cavity as working gas after the chamber is vacuumized to the preset vacuum, and the cavity pressure is regulated to 2000Pa. And starting a 2.45GHz microwave power supply (1), gradually adjusting the output power to 5500W, synchronously raising the cavity pressure to 20kPa, and adjusting a three-pin tuner (3), a short-circuit piston (5) and a lifting substrate table tuning structure (8) to minimize the microwave reflection coefficient. And introducing CH 4 to perform homoepitaxial growth of the monocrystalline diamond. And after the film deposition is finished, the power supply is turned off, the gas is turned off, and the vacuum is pumped to the limit and then the power is turned off.
Claims (14)
1. A TM multimode microwave plasma chemical vapor deposition device comprises a 2.45GHz microwave power supply, a rectangular waveguide, a three-pin tuner, a short-circuit piston, a coaxial line mode converter, an annular quartz window, a non-cylindrical microwave resonant cavity, a temperature measuring window, an observation window, an air inlet, an air outlet, a cooling water gap, a deposition table, a lifting substrate table tuning structure and a bias electrode, and is characterized in that:
The non-cylindrical resonant cavity, the annular quartz window and the deposition table form a complete vacuum chamber; the annular quartz window is arranged below the deposition table and forms a vacuum cavity with the deposition table and the non-cylindrical resonant cavity through rubber ring sealing; the air inlets are positioned above the non-cylindrical resonant cavity, and are arranged at intervals of 90 degrees along the axial direction, and the total number of the air inlets is 4; the exhaust port is positioned at the radial center of the deposition table structure, and is arranged at intervals of 60 degrees along the axial direction, and the total number of the exhaust ports is 6; the lifting substrate table tuning structure can move up and down and is used for real-time tuning of a microwave electric field and plasma.
2. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the non-cylindrical microwave resonant cavity is made of stainless steel and is formed by two cylinders with different diameters; the diameter of the upper cylinder is smaller, and the upper cylinder is used for generating a TM01 mode in the microwave resonant cavity; the diameter of the lower cylinder is larger, so that TM02 mode is generated in the microwave resonant cavity; diameter ratio of two cylindersTo meet the requirement of generating multiple resonance modes; the TM01/TM02 multimode mixing not only can enhance the microwave electric field and improve the plasma density, but also can lead the plasma to be distributed more uniformly above the surface of the large-size substrate.
3. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein 4 air inlets are disposed above the non-cylindrical microwave resonant cavity, and 6 air outlets are disposed along the axial direction at the radial center of the deposition table, so as to ensure uniformity of distribution of the reaction gas in the chamber during the diamond growth process.
4. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein a bias electrode made of tungsten is disposed in the middle above the non-cylindrical microwave resonant cavity, and is used to provide a bias electric field during the growth of heteroepitaxial single crystal diamond, so as to enhance nucleation of diamond.
5. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the non-cylindrical microwave resonant cavity is made of stainless steel, and is connected to the rectangular waveguide through a coaxial line mode converter.
6. The TM multimode microwave plasma chemical vapor deposition device of claim 1, wherein the annular quartz window is disposed below the deposition table, away from the plasma region, and etching of the quartz dielectric window by the plasma is avoided.
7. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein a sealing groove is formed at a joint of the annular quartz window, the stainless steel non-cylindrical cavity and the deposition table, the annular quartz window is placed in the sealing groove, and a fixed rubber ring is arranged between the annular quartz window and the stainless steel inner wall and between the annular quartz window and the deposition table inner wall.
8. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the viewing window is located at a side of the non-cylindrical microwave resonant cavity, and is configured to view a plasma state in real time in use.
9. The TM multimode microwave plasma chemical vapor deposition device of claim 1, wherein the temperature measurement window is located on top of the non-cylindrical microwave resonant cavity for measuring the substrate temperature in real time.
10. The TM multimode microwave plasma chemical vapor deposition device of claim 1, wherein the annular quartz window has a relative dielectric constant of 4.2.
11. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the tuning structures of the non-cylindrical microwave resonant cavity, the deposition table, and the liftable substrate table are all water cooled, so as to avoid local overheating and ensure long-term operation of the apparatus.
12. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the non-cylindrical microwave resonant cavity, the upper cylinder and the lower cylinder are connected by a bevel, and the bevel forms an angle of 167±1° with respect to the horizontal line, so as to reflect the microwaves to collect at the substrate.
13. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein an angle between an outermost inclined plane of the non-cylindrical microwave resonant cavity and a horizontal line is 75±1°, so as to reflect microwaves to be collected at the substrate.
14. The TM multimode microwave plasma chemical vapor deposition apparatus of claim 1, wherein the liftable substrate table tuning structure is designed to be movable up and down, perform microwave electric field and plasma tuning, enhance microwave electric field and plasma density, and optimize distribution of both above the substrate, so as to achieve uniform deposition of diamond.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305816A (en) * | 2012-03-14 | 2013-09-18 | 北京科技大学 | High power microwave plasma chemical vapor deposition device for diamond film |
| CN103695865A (en) * | 2013-12-13 | 2014-04-02 | 北京科技大学 | TM021 modal high-power microwave plasma diamond film deposition device |
| US20140230729A1 (en) * | 2010-12-23 | 2014-08-21 | Element Six Limited | Microwave plasma reactor for manufacturing synthetic diamond material |
| CN104164658A (en) * | 2014-08-06 | 2014-11-26 | 北京科技大学 | Ellipsoidal high-power microwave plasma diamond film deposition device |
| CN108624870A (en) * | 2018-07-05 | 2018-10-09 | 成都纽曼和瑞微波技术有限公司 | A kind of tunable circle throwing cavate high power microwave plasma chemical vapor deposition unit |
| US20200105504A1 (en) * | 2017-04-14 | 2020-04-02 | Taiyuan University Of Technology | Plasma chemical vapor deposition reactor with a microwave resonant cavity |
| CN113481595A (en) * | 2021-06-07 | 2021-10-08 | 北京科技大学 | M-shaped coaxial antenna 915MHz microwave plasma chemical vapor deposition device |
| CN114959631A (en) * | 2022-04-24 | 2022-08-30 | 北京科技大学 | Double-end feed-in microwave electron cyclotron resonance plasma chemical vapor deposition device |
| CN115132561A (en) * | 2022-06-02 | 2022-09-30 | 北京科技大学 | Annular ladder coaxial antenna type microwave plasma chemical vapor deposition device |
| CN115799793A (en) * | 2022-11-29 | 2023-03-14 | 郑州磨料磨具磨削研究所有限公司 | Novel microwave resonant cavity and microwave plasma chemical vapor deposition device |
-
2024
- 2024-01-29 CN CN202410120657.5A patent/CN118028972A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140230729A1 (en) * | 2010-12-23 | 2014-08-21 | Element Six Limited | Microwave plasma reactor for manufacturing synthetic diamond material |
| CN103305816A (en) * | 2012-03-14 | 2013-09-18 | 北京科技大学 | High power microwave plasma chemical vapor deposition device for diamond film |
| CN103695865A (en) * | 2013-12-13 | 2014-04-02 | 北京科技大学 | TM021 modal high-power microwave plasma diamond film deposition device |
| CN104164658A (en) * | 2014-08-06 | 2014-11-26 | 北京科技大学 | Ellipsoidal high-power microwave plasma diamond film deposition device |
| US20200105504A1 (en) * | 2017-04-14 | 2020-04-02 | Taiyuan University Of Technology | Plasma chemical vapor deposition reactor with a microwave resonant cavity |
| CN108624870A (en) * | 2018-07-05 | 2018-10-09 | 成都纽曼和瑞微波技术有限公司 | A kind of tunable circle throwing cavate high power microwave plasma chemical vapor deposition unit |
| CN113481595A (en) * | 2021-06-07 | 2021-10-08 | 北京科技大学 | M-shaped coaxial antenna 915MHz microwave plasma chemical vapor deposition device |
| CN114959631A (en) * | 2022-04-24 | 2022-08-30 | 北京科技大学 | Double-end feed-in microwave electron cyclotron resonance plasma chemical vapor deposition device |
| CN115132561A (en) * | 2022-06-02 | 2022-09-30 | 北京科技大学 | Annular ladder coaxial antenna type microwave plasma chemical vapor deposition device |
| CN115799793A (en) * | 2022-11-29 | 2023-03-14 | 郑州磨料磨具磨削研究所有限公司 | Novel microwave resonant cavity and microwave plasma chemical vapor deposition device |
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