CN214992009U - Airflow system structure for controlling diamond deposition rate - Google Patents
Airflow system structure for controlling diamond deposition rate Download PDFInfo
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- CN214992009U CN214992009U CN202121395948.3U CN202121395948U CN214992009U CN 214992009 U CN214992009 U CN 214992009U CN 202121395948 U CN202121395948 U CN 202121395948U CN 214992009 U CN214992009 U CN 214992009U
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Abstract
The utility model relates to the technical field of chemical vapor deposition, in particular to an airflow system structure for controlling the diamond deposition rate, which comprises an air inlet, an air outlet and a molybdenum support which are arranged on the wall of a microwave plasma reactor, wherein the air inlet and the horizontal plane form an angle theta; the gas outlets comprise a first gas outlet and a second gas outlet, and the first gas outlet is arranged at the bottom of the cavity of the microwave plasma reactor; the second air outlet is a central air hole which penetrates through the lifting deposition table at the central position of the lifting deposition table; the molybdenum support is provided with a gas diversion trench, the top of the molybdenum support is provided with a circular groove for placing a diamond growth base station, and the edge of the circular groove is provided with a circular chamfer. The gas can flow through the vicinity around the molybdenum support by adopting the air gas with a certain angle to enter and build a gas flow system structure, so that the number of gas molecules around the molybdenum support is increased, and more active groups for diamond growth are dissociated.
Description
Technical Field
The utility model relates to a chemical vapor deposition technical field, in particular to an air current system structure for controlling diamond deposition rate.
Background
The diamond has excellent performances such as high hardness, high thermal conductivity, high chemical inertness, high optical transparency, high forbidden bandwidth, high carrier concentration and the like, and has great application value in high-precision fields such as machining, high-power device radiating fins, high-power wave-transmitting windows, semiconductor devices, semiconductor chips and the like.
The Microwave Plasma Chemical Vapor Deposition (MPCVD) method has the advantages of electrodeless discharge, high energy conversion efficiency, pure plasma and the like, and is considered to be the first choice method for preparing large-area high-quality diamond films. However, the MPCVD method has some problems in terms of industrialization and mass production, that is, low deposition rate and high production cost. At present, most people adopt methods of increasing the concentration of a carbon source, increasing the air pressure or doping nitrogen and the like to improve the deposition rate of diamond so as to reduce the production cost; although the growth rate is fast and the cost is reduced, the quality of the produced diamond is poor and cannot meet the requirements of industrial application. At this time, how to effectively and rapidly grow diamonds in batch becomes a problem which needs to be solved urgently.
In the traditional method, the deposition rate of the diamond is improved by increasing the concentration of a carbon source, increasing the reaction pressure or doping nitrogen, and the like, although the growth rate is improved, the quality of the diamond is also deteriorated, and the requirement cannot be met.
Therefore, the technical personnel in the field need a device which can accelerate the growth of the diamond on the premise of not influencing the quality of the diamond, the utility model discloses a change the air current system structure, through changing the gas flow rate and the distribution around the molybdenum support, make the gas molecule quantity that is ionized by plasma in the diamond deposition process increase, the active group concentration that can be used for the diamond deposition increases, the deposition rate of the diamond promotes; and by controlling the angle of the air inlet, the distribution of a gas flow field in a reaction chamber of the microwave plasma reactor can be controlled, the gas flow field around the molybdenum support and the quantity of gas molecules ionized by plasma in the deposition process can be indirectly controlled, and the aim of controlling the deposition rate of the diamond can be achieved on the premise of ensuring the quality of the diamond.
The invention content is as follows:
in order to overcome the problems, the utility model aims to provide a through the angle of control air inlet and the position of gas outlet to and thereby the change of microwave plasma reactor reaction chamber interior gas flow field controls diamond deposition rate's air current system structure, can be under the prerequisite of guaranteeing the diamond quality, reach the mesh of control diamond's deposition rate.
In order to realize the purpose, the utility model discloses a technical scheme is: a gas flow system structure for controlling the deposition rate of diamond comprises a gas inlet arranged on the wall of a microwave plasma reactor, a gas outlet externally connected with a mechanical pump and used for obtaining vacuum or maintaining air pressure, and a molybdenum support arranged on a lifting deposition table in the microwave plasma reactor, wherein the gas inlet and the horizontal plane form an angle theta; the gas outlets comprise a first gas outlet and a second gas outlet, and the first gas outlet is arranged at the bottom of the cavity of the microwave plasma reactor; the second air outlet is a central air hole which penetrates through the lifting deposition table at the central position of the lifting deposition table; the molybdenum support is provided with a gas diversion trench, the top of the molybdenum support is provided with a circular groove for placing a diamond growth base station, and the edge of the circular groove is provided with a circular chamfer.
In the above airflow system structure for controlling the diamond deposition rate, the gas guiding groove comprises a strip-shaped guiding groove and a circular guiding groove, which are arranged at the bottom of the molybdenum support, and the circular guiding groove is arranged right above the central air hole.
In the airflow system structure for controlling the diamond deposition rate, the depth of the circular groove is 0-5mm, and the radius R of the circular chamfer is 0.5-2 mm; the number of the strip-shaped diversion trenches is 4-16, and the groove diameter of the round diversion trench is 3-10 mm.
According to the structure of the gas flow system for controlling the diamond deposition rate, the lifting deposition table is internally provided with a cooling medium capable of circulating.
In the structure of the gas flow system for controlling the diamond deposition rate, the diameter of the second gas outlet is 3-10 mm.
In the airflow system structure for controlling the diamond deposition rate, the external mechanical pump is connected with the first air outlet and the second air outlet through pipelines, and a gas flowmeter for recording and controlling the gas flow is connected in the pipelines.
The gas flow system structure for controlling the diamond deposition rate described above, the theta angle ranges from 0 to 90 deg..
The utility model relates to an air current system structure for controlling diamond deposition rate's beneficial effect is: through the angle that sets up the air inlet and the gas tank structure on the molybdenum holds in the palm to and the position setting of gas outlet, abandon traditional level mode of admitting air, adopt the entering that has certain angle air gas, build the airflow system structure, near the gas can be followed the molybdenum and held in the palm around flowing through, make the gas molecule quantity around the molybdenum holds in the palm increase, dissociate more can supply in the active group that the diamond grows, thereby reach the purpose that improves diamond growth rate. And according to different air inlet angles, matching the gas flow proportion of the corresponding first air outlet and the second air outlet to control the growth rate of the diamond.
By changing the gas flow rate and distribution around the molybdenum support, the number of gas molecules ionized by plasma in the diamond deposition process is increased, the concentration of active groups for diamond deposition is increased, and the deposition rate of diamond is improved; and by controlling the angle of the air inlet, the distribution of a gas flow field in a reaction chamber of the microwave plasma reactor can be controlled, the gas flow field around the molybdenum support and the quantity of gas molecules ionized by plasma in the deposition process can be indirectly controlled, and the deposition rate of the diamond can be controlled on the premise of ensuring the quality of the diamond.
Drawings
FIG. 1 is a schematic view of the structure of the air flow system of the present invention;
FIG. 2 is a schematic view of the molybdenum support structure gas guiding groove of the present invention;
FIG. 3 is a schematic side view of the molybdenum support structure of the present invention;
FIG. 4 is a schematic perspective view of the molybdenum support structure of the present invention;
fig. 5 is a simulation diagram of the gas flow field distribution in the reaction chamber of the microwave plasma reactor of the present invention.
In the figure: 1 air inlet, 2 upper chambers, 3 lower chambers, 4 observation windows, 5 plasma balls, 6 diversion trenches, 7 molybdenum holders, 8 lifting deposition tables, 9 first air outlets, 10 second air outlets, 11 circular grooves, 12 strip diversion trenches, 13 circular diversion trenches and 14 circular chamfers.
Detailed Description
For better understanding of the present invention, the following embodiments are provided to further illustrate the technical solution, but the present invention is not limited to the following embodiments.
As shown in fig. 1-5, an airflow system structure for controlling diamond deposition rate includes an air inlet disposed on a wall of a microwave plasma reactor, the air inlet is disposed on an outer wall of an upper chamber of the microwave plasma reactor, an external mechanical pump is connected to obtain vacuum or maintain air pressure, the air outlet is disposed on an outer wall of a lower chamber of the microwave plasma reactor, a molybdenum support on a lifting deposition table in the microwave plasma reactor forms an angle θ with a horizontal plane, and the angle θ is 0-90 °; the air outlets comprise a first air outlet and a second air outlet, and the diameter of the second air outlet is 3-10 mm.
The first gas outlet is arranged at the bottom of the microwave plasma reactor chamber; the second air outlet is a central air hole which penetrates through the lifting deposition table at the central position of the lifting deposition table; the molybdenum support is provided with gas guide grooves, the gas guide grooves comprise strip-shaped guide grooves and circular guide grooves, the strip-shaped guide grooves and the circular guide grooves are arranged at the bottom of the molybdenum support, the number of the strip-shaped guide grooves is 4-16, the circular guide grooves are arranged right above the central air hole, and the groove diameter of the circular guide grooves is 3-10 mm. The top of the molybdenum holder is provided with a circular groove for placing diamond seed crystals, the depth of the circular groove is 0-5mm, the edge of the circular groove is provided with a circular chamfer, and the radius R of the circular chamfer is 0.5-2 mm.
A cooling medium which can be circulated is arranged in the lifting deposition table.
The external mechanical pump is connected with the first gas outlet and the second gas outlet through pipelines, and a gas flowmeter for recording and controlling gas flow is connected in the pipelines.
The lifting of the lifting deposition table uses magnetic fluid dynamic sealing, which is not described herein for the prior art.
The technical scheme mainly changes the flow velocity and distribution of gas around the molybdenum support, controls the number of gas molecules flowing around the molybdenum support by controlling the flow ratio of the gas of the first gas outlet and the second gas outlet, thereby controlling the growth rate of the diamond, changing the traditional horizontal gas inlet mode and methods for improving the deposition rate of the diamond by increasing the concentration of carbon atoms, improving the reaction pressure, doping nitrogen and the like, and increasing the number of gas molecules ionized by plasma in the deposition process of the diamond by changing the flow velocity and distribution of the gas around the molybdenum support, so that the concentration of active groups for depositing the diamond is increased, and the deposition rate of the diamond is improved; and by controlling the angle of the air inlet, the distribution of a gas flow field in a reaction chamber of the microwave plasma reactor can be controlled, the gas flow field around the molybdenum support and the quantity of gas molecules ionized by plasma in the deposition process can be indirectly controlled, and the aim of controlling the deposition rate of the diamond can be achieved on the premise of ensuring the quality of the diamond.
Example 1:
1. structural design of airflow system
The gas inlet and the horizontal plane form an angle of 45 degrees and are connected with the upper cavity in a welding way, the diameter of a gas pipe of the second gas outlet is 6mm, the depth of a circular groove on the top surface of the molybdenum holder is 0.2mm, and the radius R of a circular chamfer on the edge of the top surface of the molybdenum holder is 0.5 mm; the bottom surface of the molybdenum support is provided with strip-shaped guide grooves and round guide grooves, the number of the strip-shaped guide grooves is 8, the groove width is 1.5mm, and the radius of the round guide grooves is 3 mm;
2. growth of single crystal diamond
The method for controlling the diamond deposition rate by using the airflow system structure of the utility model comprises the following steps:
the method comprises the following steps: placing the treated 0.2mm monocrystal diamond seed crystal on a molybdenum support, opening a reaction chamber of a microwave plasma reactor, placing the molybdenum support into the reaction chamber of the microwave plasma reactor, and placing a circular guide groove of the molybdenum support right above an air hole at the center of a deposition table;
step two: closing the reaction chamber of the microwave plasma reactor, completely opening the first air outlet and the second air outlet, and vacuumizing the reaction chamber of the microwave plasma reactor until the background is vacuumized to be below 1 pa;
step three: introducing hydrogen, adjusting the gas flow of the first gas outlet and the second gas outlet, maintaining the reaction gas pressure at 1-3kPa, starting a microwave power supply, adjusting the microwave input power to 600-1000W, and exciting plasma;
step four; continuously increasing the microwave power, adjusting the gas flow of the first gas outlet and the second gas outlet to increase the reaction gas pressure, and stopping increasing the microwave power and the reaction gas pressure when the substrate is heated to the temperature of 800-;
step five; introducing methane, stabilizing for 30min, adjusting gas flow meters on the pipelines of the first gas outlet and the second gas outlet, controlling the gas flow ratio 1/30 of the second gas outlet and the first gas outlet, and keeping the reaction pressure stable;
step six: maintaining the gas flow ratio, and continuously carrying out the deposition growth of the diamond until the required time length is reached.
Step seven: and closing the methane, adjusting the microwave power down, and simultaneously adjusting the gas flow of the first gas outlet and the second gas outlet to reduce the reaction gas pressure until the shutdown.
Under the above method, the deposition rate of the single crystal diamond is 10 to 15 μm/h.
Example 2:
1. structural design of airflow system
The gas inlet and the horizontal plane form an angle of 45 degrees and are connected with the upper cavity in a welding way, the diameter of a gas pipe of the second gas outlet is 6mm, the depth of a circular groove on the top surface of the molybdenum support is 3mm, and the radius R of a circular chamfer on the edge of the top surface of the molybdenum support is 0.5 mm; the bottom surface of the molybdenum support is provided with strip-shaped guide grooves and round guide grooves, the number of the strip-shaped guide grooves is 8, the groove width is 1.5mm, and the radius of the round guide grooves is 3 mm;
2. growth of polycrystalline diamond
The method for controlling the diamond deposition rate by using the airflow system structure of the utility model comprises the following steps:
the method comprises the following steps: placing the treated monocrystal diamond seed crystal with the thickness of 3mm on a molybdenum support, opening a reaction chamber of a microwave plasma reactor, placing the molybdenum support into the reaction chamber of the microwave plasma reactor, and placing a circular guide groove of the molybdenum support right above an air hole at the center of a deposition table;
step two: closing the reaction chamber of the microwave plasma reactor, completely opening the first air outlet and the second air outlet, and vacuumizing the reaction chamber of the microwave plasma reactor until the background is vacuumized to be below 1 pa;
step three: introducing hydrogen, adjusting the gas flow of the first gas outlet and the second gas outlet, maintaining the reaction gas pressure at 1-3kPa, starting a microwave power supply, adjusting the microwave input power to 600-1000W, and exciting plasma;
step four; continuously increasing the microwave power, adjusting the gas flow of the first gas outlet and the second gas outlet to increase the reaction gas pressure, and stopping increasing the microwave power and the reaction gas pressure when the substrate is heated to the temperature of 800-;
step five; introducing methane, stabilizing for 30min, adjusting gas flow meters on the pipelines of the first gas outlet and the second gas outlet, controlling the gas flow ratio 1/30 of the second gas outlet and the first gas outlet, and keeping the reaction pressure stable;
step six: maintaining the gas flow ratio, and continuously carrying out the deposition growth of the diamond until the required time length is reached.
Step seven: and closing the methane, adjusting the microwave power down, and simultaneously adjusting the gas flow of the first gas outlet and the second gas outlet to reduce the reaction gas pressure until the shutdown.
Under the above method, the deposition rate of the polycrystalline diamond film is 3 to 6 μm/h.
Example 3:
1. structural design of airflow system
The gas inlet and the horizontal plane form an angle of 60 degrees and are connected with the upper chamber in a welding way, the diameter of a gas pipe of the second gas outlet is 8mm, the depth of a circular groove on the top surface of the molybdenum holder is 0.2mm, and the radius R of a circular chamfer on the edge of the top surface of the molybdenum holder is 0.5 mm; the bottom surface of the molybdenum support is provided with strip-shaped guide grooves and circular guide grooves, the number of the strip-shaped guide grooves is 12, the groove width is 2mm, and the radius of the circular guide grooves is 3 mm;
2. growth of single crystal diamond
The method for controlling the diamond deposition rate by using the airflow system structure of the utility model comprises the following steps:
the method comprises the following steps: placing the treated 0.2mm monocrystal diamond seed crystal on a molybdenum support, opening a reaction chamber of a microwave plasma reactor, placing the molybdenum support into the reaction chamber of the microwave plasma reactor, and placing a circular guide groove of the molybdenum support right above an air hole at the center of a deposition table;
step two: closing the reaction chamber of the microwave plasma reactor, completely opening the first air outlet and the second air outlet, and vacuumizing the reaction chamber of the microwave plasma reactor until the background is vacuumized to be below 1 pa;
step three: introducing hydrogen, adjusting the gas flow of the first gas outlet and the second gas outlet, maintaining the reaction gas pressure at 1-3kPa, starting a microwave power supply, adjusting the microwave input power to 600-1000W, and exciting plasma;
step four; continuously increasing the microwave power, adjusting the gas flow of the first gas outlet and the second gas outlet to increase the reaction gas pressure, and stopping increasing the microwave power and the reaction gas pressure when the substrate is heated to the temperature of 800-;
step five; introducing methane, stabilizing for 30min, adjusting gas flow meters on the pipelines of the first gas outlet and the second gas outlet, controlling the gas flow ratio 1/50 of the second gas outlet and the first gas outlet, and keeping the reaction pressure stable;
step six: maintaining the gas flow ratio, and continuously carrying out the deposition growth of the diamond until the required time length is reached.
Step seven: and closing the methane, adjusting the microwave power down, and simultaneously adjusting the gas flow of the first gas outlet and the second gas outlet to reduce the reaction gas pressure until the shutdown.
Under the above method, the deposition rate of the single crystal diamond is 15 to 20 μm/h.
Example 4:
1. structural design of airflow system
The gas inlet and the horizontal plane form an angle of 60 degrees and are connected with the upper chamber in a welding way, the diameter of a gas pipe of the second gas outlet is 8mm, the depth of a circular groove on the top surface of the molybdenum support is 3mm, and the radius R of a circular chamfer on the edge of the top surface of the molybdenum support is 0.5 mm; the bottom surface of the molybdenum support is provided with strip-shaped guide grooves and circular guide grooves, the number of the strip-shaped guide grooves is 12, the groove width is 2mm, and the radius of the circular guide grooves is 3 mm;
2. growth of single crystal diamond
The method for controlling the diamond deposition rate by using the airflow system structure of the utility model comprises the following steps:
the method comprises the following steps: placing the processed single crystal diamond seed crystal with the thickness of 3mm on a molybdenum support, opening a reaction chamber of a microwave plasma reactor, placing the molybdenum support into the reaction chamber of the microwave plasma reactor, and placing a circular guide groove of the molybdenum support right above an air hole at the center of a deposition table when placing the molybdenum support;
step two: closing the reaction chamber of the microwave plasma reactor, completely opening the first air outlet and the second air outlet, and vacuumizing the reaction chamber of the microwave plasma reactor until the background is vacuumized to be below 1 pa;
step three: introducing hydrogen, adjusting the gas flow of the first gas outlet and the second gas outlet, maintaining the reaction gas pressure at 1-3kPa, starting a microwave power supply, adjusting the microwave input power to 600-1000W, and exciting plasma;
step four; continuously increasing the microwave power, adjusting the gas flow of the first gas outlet and the second gas outlet to increase the reaction gas pressure, and stopping increasing the microwave power and the reaction gas pressure when the substrate is heated to the temperature of 800-;
step five; introducing methane, stabilizing for 30min, adjusting gas flow meters on the pipelines of the first gas outlet and the second gas outlet, controlling the gas flow ratio 1/50 of the second gas outlet and the first gas outlet, and keeping the reaction pressure stable;
step six: maintaining the gas flow ratio, and continuously carrying out the deposition growth of the diamond until the required time length is reached.
Step seven: and closing the methane, adjusting the microwave power down, and simultaneously adjusting the gas flow of the first gas outlet and the second gas outlet to reduce the reaction gas pressure until the shutdown.
Under the above method, the deposition rate of the polycrystalline diamond film is 5 to 10 μm/h.
The growth rate of diamond is related to the concentration of the carbon source in the reaction gas. The reaction gas flows around the molybdenum support, the number of gas molecules which can participate in dissociation around the molybdenum support is increased, and the concentration of carbon-containing active groups dissociated by the plasma is increased (namely, the carbon source concentration is increased by phase change), so that the growth rate of the diamond is improved. If the flow ratio of the gas flowing through the second gas outlet and the gas flowing through the first gas outlet is too small, the number of molecules of the gas flowing through the molybdenum support is small, and the effect of improving the growth rate of the diamond cannot be achieved; if the gas flow ratio of the second gas outlet and the first gas outlet is controlled to be too large, the number of gas molecules around the molybdenum support is too large, so that the reaction gas is not fully dissociated, the quality of the grown diamond is deteriorated, and the gas flow ratio of the second gas outlet and the first gas outlet needs to be adjusted properly. Through experiments, the gas flow ratio of the second gas outlet and the first gas outlet is controlled to be 1/100-1/10 optimally.
The above embodiments are only for illustrating the structural conception and the characteristics of the present invention, and the purpose thereof is to enable the person skilled in the art to understand the contents of the present invention and to implement the present invention, so as not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered by the protection scope of the present invention.
Claims (7)
1. The utility model provides a gas flow system structure for controlling diamond deposition rate, is used for acquireing the vacuum or maintain the atmospheric pressure gas outlet including setting up the air inlet on microwave plasma reactor wall, external mechanical pump, places the molybdenum on the lift deposit platform in microwave plasma reactor and holds in the palm, its characterized in that: the air inlet and the horizontal plane form an angle theta; the gas outlets comprise a first gas outlet and a second gas outlet, and the first gas outlet is arranged at the bottom of the cavity of the microwave plasma reactor; the second air outlet is a central air hole which penetrates through the lifting deposition table at the central position of the lifting deposition table; the molybdenum support is provided with a gas diversion trench, the top of the molybdenum support is provided with a circular groove for placing a diamond growth base station, and the edge of the circular groove is provided with a circular chamfer.
2. The gas flow system structure for controlling the diamond deposition rate according to claim 1, wherein: the gas diversion trench comprises a strip diversion trench and a circular diversion trench, wherein the strip diversion trench and the circular diversion trench are arranged at the bottom of the molybdenum support, and the circular diversion trench is arranged right above the central air hole.
3. The gas flow system structure for controlling the diamond deposition rate according to claim 2, wherein: the depth of the circular groove is 0-5mm, and the radius R of the circular chamfer is 0.5-2 mm; the number of the strip-shaped diversion trenches is 4-16, and the groove diameter of the round diversion trench is 3-10 mm.
4. The gas flow system structure for controlling the diamond deposition rate according to claim 1, wherein: and a cooling medium capable of circulating is arranged in the lifting deposition table.
5. The gas flow system structure for controlling the diamond deposition rate according to claim 1, wherein: the diameter of the second air outlet is 3-10 mm.
6. The gas flow system structure for controlling the diamond deposition rate according to claim 1, wherein: the external mechanical pump is connected with the first gas outlet and the second gas outlet through pipelines, and a gas flowmeter for recording and controlling gas flow is connected in the pipelines.
7. The gas flow system structure for controlling the diamond deposition rate according to claim 1, wherein: the theta angle ranges from 0 to 90 deg..
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