CN117535791B - MPCVD-based substrate for growing single crystal diamond material and method thereof - Google Patents
MPCVD-based substrate for growing single crystal diamond material and method thereof Download PDFInfo
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- CN117535791B CN117535791B CN202311670318.6A CN202311670318A CN117535791B CN 117535791 B CN117535791 B CN 117535791B CN 202311670318 A CN202311670318 A CN 202311670318A CN 117535791 B CN117535791 B CN 117535791B
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Abstract
The application provides a base station for growing single crystal diamond material based on MPCVD and a method for growing single crystal diamond material based on MPCVD; comprises a base station base for supporting the base station; the shielding base station is used for wrapping the side surface of the monocrystalline diamond substrate; the movable base station is embedded in the middle of the shielding base station and is used for bearing the monocrystalline diamond substrate and moving up and down relative to the shielding base station; when growing single crystal diamond, feeding microwave to excite hydrogen plasma from the lower part of the base station to grow single crystal diamond material; the control system moves the movable base table in real time according to the surface thickness change of the monocrystalline diamond substrate, the surface of the monocrystalline diamond substrate is kept flush with the upper surface of the shielding base table in real time, the side wall of the concave part of the shielding base table is close to the side surface of the monocrystalline diamond substrate, and the distribution of electric fields around the shielding base table is shielded to inhibit the growth of polycrystalline diamond; according to the technical scheme, the growth conditions can be kept stable all the time, and the preparation of high-quality large-size single crystal diamond is realized.
Description
Technical Field
The application relates to the technical field of microwave plasma chemical deposition, in particular to a base station for growing single crystal diamond material based on MPCVD and a method for growing single crystal diamond material based on MPCVD.
Background
Among various methods for synthesizing single crystal diamond, MPCVD (Microwave PLASMA CHEMICAL Vapor Deposition) is the preferred method for preparing high quality single crystal diamond because it can generate large-area, pure and stable plasma balls in a Deposition chamber. In the MPCVD apparatus structure, the base structure thereof is also subjected to various forms of improvement design, thereby improving the quality of the grown single crystal diamond. Particularly, a scalable structural design is introduced to realize temperature control and adjustment functions in some growth processes, for example, in the patent application of China patent publication No. CN113025997A, an MPCVD substrate table adaptable to thickness variation of a multi-size substrate is disclosed; in chinese patent publication No. CN218812081U, a compact lifting mechanism for MPCVD is disclosed; in chinese patent publication No. CN218860884U, a cavity structure for MPCVD apparatus is disclosed; in the patent application with the Chinese patent publication number of CN112647126A, an embedded water cooling table for the temperature-controlled continuous growth of large-particle MPCVD single crystal diamond and application thereof are disclosed, wherein two motors are used for driving the water cooling table to realize the constant temperature control, and as in the above disclosed technology, a lifting mechanism is introduced into an MPCVD device.
In a standard process for synthesizing single crystal diamond, a single crystal diamond substrate is placed on a flat substrate, and a series of conditions such as frequency and power of microwave, composition and flow rate of gas, pressure and temperature in a cavity, temperature of a surface of a base, etc. are strictly controlled so as to enable single crystal diamond to perform stable growth with high quality. However, when the single-crystal diamond grows gradually along the growth surface, the growth conditions around the growth surface change along with the increase of the thickness of the single-crystal diamond, so that the growth uniformity or thickness of the single-crystal diamond is affected; in the process of growing the single crystal diamond, the position of the surface of the single crystal diamond needs to be maintained at a certain temperature, and the thickness of the single crystal diamond grows to be large for a certain time, so that the distance from the plasma ball is reduced, and the temperature of the single crystal diamond is too high to be beneficial to growth; in addition, during the growth of single crystal diamond, the side polycrystalline diamond is grown due to the fact that the four non-growth-side sides of the diamond substrate are away from the central plasma region; meanwhile, because the hydrogen plasma cannot etch the growth of amorphous carbon in time, black substances grow on the side surfaces of the four non-growth surfaces of the diamond substrate in the diamond growth process, so that the growth of the growth surface of the diamond substrate is limited, and ineffective growth of the diamond substrate is caused; in order to solve the above problems, it is common to employ a lifting/lowering stage to adjust the distance between the plasma ball and the single crystal diamond, thereby stabilizing the temperature of the growth surface, or to employ a stage with grooves in which diamond is grown, and to replace the stages with different degrees of dishing during the multi-stage growth, so that the side walls of the grooves of the stage shield the electric fields of the respective non-growth sides, thereby preventing the growth of polycrystalline diamond around the single crystal diamond substrate, so that the single crystal diamond can be effectively grown continuously along the growth surface, thereby growing thicker single crystal diamond.
However, in the actual process, the inventor finds that in the growth process of the single crystal diamond, the temperature can be controlled to be stable by adjusting the distance between the base table and the plasma sphere, but the change of the distance between the surface of the single crystal diamond substrate and the base table can cause the change of the electric field on the surface of the single crystal diamond, so that the growth condition of the single crystal diamond is changed, and the uniformity of a single crystal diamond product is affected; in addition, the growth of polycrystalline diamond on the non-growth side of the monocrystalline diamond is limited, and the growth is continuously interrupted during the growth period to replace the base stations with different concave degrees, so that the preparation efficiency of the monocrystalline diamond is greatly reduced.
Disclosure of Invention
The application aims to solve one of the technical defects, and provides a base station for growing single crystal diamond material based on MPCVD and a method for growing single crystal diamond material based on MPCVD, which improve the preparation efficiency of single crystal diamond.
A MPCVD-based submount for growing single crystal diamond material for use in an MPCVD deposition chamber, comprising:
the base station base is used for supporting the base station and serving as a coupling antenna, and maintaining the focusing distribution of the electric field intensity above the base station base;
The shielding base station is arranged in the middle of the base station base and used for wrapping the side surface of the monocrystalline diamond substrate and shielding electric field distribution around the side surface of the monocrystalline diamond substrate;
The movable base station is embedded in the middle of the shielding base station and is used for bearing the monocrystalline diamond substrate and moving up and down relative to the shielding base station;
When growing single crystal diamond, feeding microwaves from the lower part of the base table to enable the base table to form a strong electric field area, and exciting hydrogen plasma to grow single crystal diamond materials on the surface of the single crystal diamond substrate; the control system moves the movable base table in real time according to the surface thickness change of the single crystal diamond substrate, the surface of the single crystal diamond substrate is kept flush with the upper surface of the shielding base table in real time, so that the side wall of the concave part of the shielding base table is close to and wraps the side surface of the single crystal diamond substrate, and the peripheral electric field distribution is shielded to inhibit the growth of polycrystalline diamond.
In one embodiment, the shielding base is of a removable design;
the control system is also used for moving the shielding base table in real time according to the temperature change of the growth surface of the single crystal diamond substrate so as to adjust the distance between the growth surface of the single crystal diamond substrate and the plasma ball and maintain the growth condition of the growth surface of the single crystal diamond substrate stable.
In one embodiment, a molybdenum sheet is disposed on the upper surface of the movable base as a substrate tray; the single crystal diamond substrate is uniformly placed on the substrate tray;
and a metal gasket is arranged at the upper part of the shielding base station and used for fixing the monocrystalline diamond substrate.
In one embodiment, the movable base station is connected with a first servo motor, and the first servo motor is connected with a control system;
the shielding base station is connected with a second servo motor, and the second servo motor is connected with a control system;
And the control system controls the first servo motor to drive the movable base station to move and controls the second servo motor to drive the shielding base station to move according to the growth state and the temperature change of the surface of the monocrystalline diamond substrate monitored in real time.
In one embodiment, the lower part of the base station base is connected with a coaxial cable and is in sealing connection with a quartz ring of the MPCVD deposition cavity, and the MPCVD deposition cavity is vacuum-sealed;
Wherein the coaxial cable feeds microwaves to an area above a base station within the MPCVD deposition chamber.
In one embodiment, the movable base station is square in cross-section.
In one embodiment, the single crystal diamond substrate is uniformly placed on the upper surface of the movable base in a square layout.
In one embodiment, a camera is further arranged outside the observation window of the MPCVD deposition cavity, and the shooting direction of the camera is flush with the upper surface of the shielding base station;
the camera shoots a real-time image of the upper surface of the shielding base station and transmits the real-time image to the control system;
and the control system determines the alignment state of the surface of the monocrystalline diamond substrate and the upper surface of the shielding base station according to the pixel points of the monocrystalline diamond appearing in the real-time image, and outputs a related control signal to the first servo motor to drive the movable base station to move.
In one embodiment, the MPCVD-based submount for growing single crystal diamond material further comprises: a light detection device; wherein the light detection device comprises a microprocessor, a light emitting device and a light receiving device;
The light emitting device and the light receiving device are respectively arranged on two opposite observation windows of the MPCVD deposition cavity;
The microprocessor controls the light emitting device to emit light rays with set wavelength, and the light receiving device receives the light rays;
The microprocessor detects the intensity of the received light, and if the intensity of the light is smaller than a threshold value, outputs a relevant control signal to the linear driving structure to control the movable base station to move, so that the surface of the monocrystalline diamond substrate and the upper surface of the shielding base station are kept flush in real time.
In one embodiment, the movable base station has a first cooling chamber built therein, the first cooling chamber being connected to an air cooling system by an air cooling duct; wherein the air cooling system is connected to a control system;
The control system controls the gas flow rate of the gas cooling system to adjust the temperature of the movable base and the single crystal diamond substrate.
In one embodiment, the air-cooled conduit is a rigid conduit.
In one embodiment, the air cooling pipeline is movably connected with the first cooling cavity inside the movable base station in a nested manner;
The air inlet and the air outlet connected with the air cooling pipeline are centrally symmetrical in the first cooling cavity, so that the temperature distribution on the surface of the movable base station is uniform.
In one embodiment, an infrared thermometer is further arranged on the upper surface of the movable base station;
the infrared thermometer is used for detecting the real-time temperature of the surface of the monocrystalline diamond substrate;
the control system controls the gas flow of the gas cooling system according to the real-time temperature.
In one embodiment, the shielding base station is internally provided with a second cooling cavity, and the second cooling cavity is connected to a water cooling system through a water cooling pipeline; wherein the water cooling system is connected to a control system;
The control system controls the water flow of the water cooling system to radiate the shielding base station.
A method of growing single crystal diamond material based on MPCVD, applied to the MPCVD-based single crystal diamond material substrate, comprising:
placing a single crystal diamond substrate on the movable base station, and keeping the upper surface of the single crystal diamond substrate flush with the shielding base station;
depositing a single crystal diamond material on the surface of the single crystal diamond substrate;
The control system detects the alignment state of the surface of the single crystal diamond substrate and the upper surface of the shielding base table in real time, and controls the movable base table to move downwards, so that the surface of the single crystal diamond substrate and the upper surface of the shielding base table are kept flush in real time.
In one embodiment, the MPCVD-based method of growing single crystal diamond material further comprises:
The control system detects the real-time temperature of the surface of the monocrystalline diamond substrate in real time, the shielding base station is moved according to the real-time temperature, and the distance between the growth surface of the monocrystalline diamond substrate and the plasma ball is adjusted so that the surface temperature of the monocrystalline diamond substrate keeps a stable value.
The technical scheme of the embodiment is suitable for the lower feed type MPCVD deposition cavity of microwave fed in from the lower side, the growth surface of the monocrystalline diamond substrate is adjusted to move relative to the upper surface of the shielding base through the shielding base and the liftable movable base, in the growth process of the monocrystalline diamond material, the surface growth of the thickness of the monocrystalline diamond is monitored in real time, the growth surface of the monocrystalline diamond substrate is adjusted to be always kept flush with the upper surface of the shielding base, the side wall of the concave part of the shielding base is kept to be always close to the side surface of the monocrystalline diamond substrate, the electric field distribution around the monocrystalline diamond is shielded, the growth condition of the monocrystalline diamond material near the growth surface of the monocrystalline diamond material is always kept stable in the whole growth process, and therefore the growth of polycrystalline diamond is restrained, and the preparation of the monocrystalline diamond with higher quality, larger thickness and larger size is realized.
Further, the distance between the growth surface of the diamond substrate and the plasma ball is adjusted by lifting the shielding base table so as to control the temperature stability and ensure that the growth condition of the single crystal diamond is always kept stable.
Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.
Drawings
The foregoing and/or additional aspects and advantages of the application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic structural diagram of a submount of growing single crystal diamond material based on MPCVD according to one embodiment;
FIG. 2 is a schematic cross-sectional view of an exemplary movable base station;
Fig. 3 is a schematic structural view of another embodiment of a submount for growing single crystal diamond material based on MPCVD;
FIG. 4 is a schematic diagram of monitoring alignment based on a light detection device;
FIG. 5 is a schematic illustration of monitoring alignment status based on real-time images;
FIG. 6 is a schematic view of the structure of the air inlet and the air outlet in the first cooling chamber;
FIG. 7 is an electrical block diagram of an MPCVD deposition chamber of an embodiment;
Fig. 8 is a flow chart of a method of growing single crystal diamond material based on MPCVD in one embodiment.
Detailed Description
Embodiments of the present application are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the application.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless expressly stated otherwise, as understood by those skilled in the art. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, but do not preclude the presence or addition of one or more other features, integers, steps, operations.
It will be understood by those skilled in the art that all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless defined otherwise. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The application is directed to an improved scheme of MPCVD deposition cavity structure for growing single crystal diamond material based on MPCVD, which is applicable to MPCVD deposition cavity fed by microwaves from below; meanwhile, the surface growth environmental stability of the monocrystalline diamond substrate is improved, and the preparation of the monocrystalline diamond with higher quality and larger size is realized.
Referring to fig. 1, fig. 1 is a schematic structural view, illustrated as a cross-sectional view, of a submount of growing single crystal diamond material based on MPCVD according to an embodiment; the MPCVD-based submount of growing single crystal diamond material of the present embodiment may be used in an MPCVD deposition chamber 10, and the main structure includes: a base 01, a shielding base 02 and a movable base 03.
The base station base 01 is a basic structure and is used for supporting the whole base station, the fixed quartz ring 05 keeps the vacuum state of the deposition cavity 10, and microwaves are coupled as a coupling antenna, and the size of the base station base 01 is designed to meet the requirement and can maintain the focusing distribution of the electric field intensity above the base station base; the shielding base table 02 is arranged in the middle of the base table base 01, the shielding base table 02 is used for wrapping the side wall of the monocrystalline diamond substrate 11 and shielding electric field distribution around the side surface of the monocrystalline diamond substrate 11; the movable base 03 is embedded in the middle of the base 01 and the shielding base 02 and is used for bearing the monocrystalline diamond substrate 11 and moving up and down, when the monocrystalline diamond is high, the side wall of the concave part of the shielding base 02 is kept close to the side face of the monocrystalline diamond substrate 11 all the time, so that the side face of the monocrystalline diamond substrate 11 is wrapped to shield the peripheral electric field distribution of the monocrystalline diamond substrate 11, and the growth of polycrystalline diamond is restrained.
In this embodiment, the section of the movable base 03 is square, which can be determined by the arrangement of the diamond seeds therein; correspondingly, the single crystal diamond substrates 11 can be uniformly placed on the upper surface of the movable base 03 in a square layout, the single crystal diamond substrates 11 are closely arranged, and the side surfaces of the single crystal diamond substrates 11 are closely attached to the side walls of the recess of the shielding base 02.
As shown in fig. 2, fig. 2 is a schematic cross-sectional view of an exemplary movable base, in which the movable base 03 is designed as a square, and the single crystal diamond substrates 11 are distributed on the upper surface of the movable base 03 in a close arrangement, for example, the side length of the square of the movable base 03 may be selected to be 30mm, 40mm or 50mm, and correspondingly, 4×4×1mm 3,6×6×1mm3, or 8×8×1mm 3 single crystal diamond substrates 11 are uniformly placed on the movable base 03. The single crystal diamond substrates are closely arranged (the distance between the single crystal diamond substrates is smaller than 2 mm), so that the electric fields of the four non-growing sides of each single crystal CVD diamond are shielded by the adjacent single crystal CVD diamond, the growth of surrounding polycrystalline diamond is avoided, and a plurality of single crystal CVD diamond can effectively continue to grow along the growing surface, thereby growing into single crystal diamond with higher quality and thickness.
The surface of the single crystal diamond substrate 11 is kept flush with the upper surface of the shield base 02 throughout the growth of the single crystal diamond material; when growing single crystal diamond, feeding microwaves from below the base 01 of the base so as to form a strong electric field area above the base, and exciting hydrogen plasma to grow single crystal diamond material on the surface of the single crystal diamond substrate 11; the control system 04 moves the movable base 03 in real time according to the surface thickness variation or the temperature variation of the single crystal diamond substrate 11 so that the surface of the single crystal diamond substrate 11 is kept flush with the upper surface of the shielding base 02 in real time, thereby stabilizing the electric field around the single crystal diamond substrate 11.
For a more detailed clarity of the solution of the application, further embodiments are described below with reference to the accompanying drawings.
As shown in fig. 3, fig. 3 is a schematic structural view, schematically shown as a cross-sectional view, of another embodiment of a submount for growing single crystal diamond material based on MPCVD.
In one embodiment, a molybdenum sheet is provided on the upper surface of the movable base 03 as a substrate tray 37; the single crystal diamond substrate 11 is uniformly placed on the substrate tray 37; meanwhile, a metal gasket 27, typically a molybdenum metal sheet, is provided on the upper portion of the shielding base 02 for fixing the single crystal diamond substrate 11, and diamond material is grown on the shielding base 02, so that the upper portion of the shielding base 02 is uniform in heat dissipation and convenient to clean and replace.
In one embodiment, the shield base 02 is also of a removable design; as shown in fig. 3, the shield base 02 is movable in the up-and-down direction, and the movable base 03 and the single crystal diamond substrate 11 placed thereon are moved in the up-and-down direction as a whole. In this case, the control system 04 is further configured to move the shielding base 02 in real time according to a temperature change of the growth surface of the single crystal diamond substrate 11, so as to adjust a distance between the growth surface of the single crystal diamond substrate 11 and the plasma sphere, so that a growth condition of the growth surface of the single crystal diamond substrate 11 is maintained stable, and thus, a quality of the grown single crystal diamond can be improved.
For the control system 04, it mainly realizes the function of the control function part of the MPCVD deposition chamber 10, and for its specific structure, control driving devices such as an industrial personal computer, a processor, a driver, and the like may be included.
The technical solution of the above embodiment is suitable for the lower feeding type MPCVD deposition cavity 10 with microwave fed in, and the lower feeding type MPCVD deposition cavity 10 has smaller volume, which is convenient for cavity installation, replacement and overhaul.
The embodiment realizes a design scheme of a liftable compact base platform, through a shielding base platform 02 and a movable base platform 03 which are designed on a base platform base 01, the movable base platform 03 can move a loaded single crystal diamond substrate 11 up and down in the growth process of a single crystal diamond material, the growth surface of the single crystal diamond substrate 11 is always kept flush with the upper surface of the shielding base platform 02 through monitoring the surface growth thickness of the single crystal diamond in real time, so as to shield the electric field around the single crystal diamond substrate 11, the growth condition of the single crystal diamond material near the growth surface of the single crystal diamond material in the whole growth process is always kept stable, and the growth of polycrystalline diamond around the single crystal diamond substrate is prevented, thereby realizing the preparation of the single crystal diamond with high quality and large size.
The abutment for growing single crystal diamond material based on MPCVD of the present embodiment is applied in a down-feed type MPCVD deposition chamber 10, and microwaves are fed from below; accordingly, the coaxial cable 12 is connected to the lower part of the base station base 01, the coaxial cable 12 is hermetically connected with the quartz ring 05 of the MPCVD deposition chamber 10, and the MPCVD deposition chamber 10 is vacuum-sealed; thereby forming a deposition space of a vacuum environment.
The coaxial cable 12 feeds microwaves into the region above the base station in the MPCVD deposition chamber 10 to form a strong electric field region, producing a large-area, pure and stable plasma sphere, producing high quality single crystal diamond.
The movable base 03 may be driven by a motor or by other means.
In this embodiment, preferably, the movable base 03 is driven by the first servo motor 31, the movable base 03 is moved by the first servo motor 31 and the driving structure 311, the driving structure 311 may include a coupler, a linear bearing, a screw structure, etc., the driving structure 311 is connected to the lower part of the movable base 03, the connection control system 04 of the first servo motor 31, and the control system 04 may control the first servo motor 31 to drive the movable base 03 to move up and down according to the growth state of the surface of the single crystal diamond substrate 11 monitored in real time; more accurate movement control can be realized.
As for the method of monitoring the growth state of the surface of the single crystal diamond substrate 11, its accuracy and real-time property have an important influence on the movement control process, and therefore, it is necessary to design an accurate monitoring scheme to detect the growth state of the surface of the single crystal diamond substrate 11.
In one embodiment, the growth rate of the single crystal diamond in the MPCVD deposition chamber 10 may be obtained experimentally, the control system 04 may precisely calculate the surface thickness increase value of the single crystal diamond substrate 11 according to the determined growth rate, and the first control servo motor 31 may be moved according to the calculation result.
In one embodiment, the shielding base 02 is connected to a second servo motor 26, the second servo motor 26 being connected to the control system 04; the control system 04 controls the second servo motor 26 to drive the shielding base 02 to move up and down as a whole according to the temperature change of the surface of the single crystal diamond substrate 11 monitored in real time, and since the movable base 03 is embedded in the shielding base 02, at this time, the shielding base 02 and the movable base 03 and the single crystal diamond substrate 11 placed thereon move up and down as a whole, thereby realizing a temperature control function so that the temperature maintains a stable temperature value.
In one embodiment, a light detection solution may also be used; by providing a light detection means 13 outside the viewing window of the MPCVD deposition chamber 10; wherein the light detection means 13 comprises a microprocessor 131, light emitting means 132 and light receiving means 133; the light emitting device 132 and the light receiving device 133 are respectively disposed on two opposite viewing windows of the MPCVD deposition chamber 10; as shown in fig. 4, fig. 4 is a schematic view of monitoring alignment status based on a light detection device; the light is tightly attached to the upper surface of the shielding base 02, and during the growth process, the microprocessor 131 controls the light emitting device 132 to emit light, and the light receiving device 133 receives light; the microprocessor 131 detects the intensity of the light, in an initial state, the light is not blocked, the intensity of the light is greater than a threshold value, along with the growth of the surface of the monocrystalline diamond substrate 11 beyond the upper surface of the shielding base 02, the light is blocked, the intensity of the light is less than the threshold value, the control system 04 outputs a relevant control signal to the linear motor 31 to drive the movable base 03 to move downwards for a small distance, the height of the movable base 03 is gradually reduced along with the growth of the monocrystalline diamond, the growth surface of the monocrystalline diamond is always kept flush with the upper surface of the shielding base 02, and the cycle is repeated until the whole growth process is completed. Considering factors such as the influence of the transmittance of the single crystal diamond, etc., in consideration of the high temperature conditions in the hydrogen plasma ball and the deposition chamber, it is preferable that the light of this embodiment uses ultraviolet light of 300-400 nm.
As in the technical solution of the above embodiment, the structure is simple, the equipment cost is controllable, the alignment state of the surface of the single crystal diamond substrate 11 and the upper surface of the shielding base 02 can be monitored in real time, and the alignment state can be accurately predicted, so that accurate movement control is realized.
Further, since the movable stage 03 has a movement range d of about 5mm to 10mm, and the growth rate of single crystal diamond is generally several tens of micrometers/hour, the control system 04 needs more precise control of the movable stage 03 for high resolution movement control.
In one embodiment, it is preferable to provide the camera 14 outside the observation window of the MPCVD deposition chamber 10, and the shooting direction of the camera 14 is flush with the upper surface of the shielding base 02; capturing a real-time image of the upper surface of the shielding base 02 by the camera 14 and transmitting to the control system 04; the control system 04 determines the alignment state of the surface of the single crystal diamond substrate 11 and the upper surface of the shielding base 02 from the pixel points of the single crystal diamond appearing in the real-time image by the image processing technique; as shown in fig. 5, fig. 5 is a schematic diagram of monitoring alignment state based on real-time image, wherein real-time image is continuously shot through camera 14, in initial state, the upper surface of shielding base 02 in real-time image is a straight line, during growth process, the surface of monocrystalline diamond substrate 11 exceeds the upper surface of shielding base 02, at this time, a plurality of pixel points on the surface of monocrystalline diamond substrate 11 appear on the surface of monocrystalline diamond substrate 11 can be captured in real-time image, control system 04 outputs relevant control signal to first servo motor 31 to drive movable base 03 to move downwards for a slight distance, the height of movable base 03 gradually decreases along with growth of monocrystalline diamond, the growth surface of monocrystalline diamond is always kept flush with the upper surface of shielding base 02, and the whole growth process is circulated until completion.
As in the technical solution of the foregoing embodiment, the alignment state between the surface of the monocrystalline diamond substrate 11 and the upper surface of the shielding base 02 is monitored by an image processing technique, so that the accuracy of the growth rate affecting the monocrystalline diamond of various growth conditions can be avoided, the pixel level accuracy is realized, and the resolution is high, so that more accurate movement control is realized, compared with the method of calculating the growth rate.
In one embodiment, since temperature control over the movable stage 03 is critical to the quality of the growth of the single crystal diamond during the growth of the single crystal diamond, water cooling may be generally used for heat dissipation. In this embodiment, preferably, in order to more precisely control the temperature of the movable base 03, an air cooling method is used to cool the movable base 03; referring to fig. 3, in the cooling scheme using the air cooling method, the movable base 03 has a first cooling cavity 32 therein, and the first cooling cavity 32 is connected to an air cooling system 34 through an air cooling pipe 33, and an exemplary air source may be hydrogen; wherein the gas cooling system 34 is connected to the control system 04, the control system 04 controls the gas flow rate of the gas cooling system 34 to adjust the temperature of the movable stage 03 and the single crystal diamond substrate 11.
As in the solution of the above embodiment, the movable base 03 uses gas as the cooling source, and the temperature of the movable base 03 can be controlled more precisely by adjusting the flow rate of the gas or the ratio of different gas types.
Since the movable base 03 moves within a certain range, if the air cooling pipe 33 is a hard cooling pipe, the position of the air inlet 33a inside the first cooling chamber 32 is changed; if the air cooling pipeline 33 is a soft cooling pipeline, the air inlet and outlet pipeline is deformed, so that the pipe diameter of the pipe wall is changed, the cooling effect of the movable base 03 is affected, and the surface temperature stability of the base is affected.
To achieve temperature stability, in one embodiment, referring to FIG. 6, FIG. 6 is a schematic diagram of the inlet and outlet structures in the first cooling chamber; the air cooling pipeline 33 adopts a hard pipeline, and as an embodiment, the air cooling pipeline 33 is movably connected with the first cooling cavity 32 inside the movable base 03 in a nested manner; the air inlet 33a and the air outlet 33b connected to the air cooling pipe 33 are centrally symmetrical in the first cooling chamber 32, so that the temperature distribution on the surface of the movable base 03 is uniform.
In the technical solution of the foregoing embodiment, in the design of the cooling pipe of the movable base 03, the hard cooling pipe is nested with the internal structure of the movable base 03, so as to ensure that the air inlet 33a and the air outlet 33b are centrosymmetric inside the movable base 03, and the temperature distribution on the surface of the base is uniform, thereby ensuring that the temperature value of the single crystal diamond of the movable base 03 is stable.
Further, as shown in fig. 6, since the movable base 03 moves within a certain range, the air inlet 33a and the air outlet 33b move up and down along the movable base 03 by a distance d, and the relative positions thereof are slightly changed, which may cause a change in the temperature of the growth surface of the single crystal diamond.
Accordingly, in this embodiment, an infrared thermometer 36 is further disposed above the movable base 03, the infrared thermometer 36 may be disposed above the infrared thermometer 36 and located on the outer surface of the MPCVD deposition chamber, the infrared thermometer 36 points to the upper position of the movable base 03, for detecting the real-time temperature of the surface of the single crystal diamond substrate 11, the infrared thermometer 36 may convert the power signal of the plasma radiation into a single crystal diamond growth surface temperature signal, the control system 04 may control the gas flow of the gas cooling system 34 according to the real-time temperature, and the control system 04 may also control the movable base to move according to the real-time temperature so as to adjust the distance between the single crystal diamond growth surface and the plasma ball, thereby ensuring the temperature stability of the single crystal diamond growth surface.
As shown, the infrared thermometer 36 is provided with two, real-time temperature detecting single crystal diamond growth surface, one side for measuring diamond growth area center temperature, and the other side for measuring boundary temperature; the control system 04 can control the movable base 03 to move according to the real-time temperature, and adjust the distance between the single crystal diamond growth surface and the plasma ball, so that the temperature of the single crystal diamond growth surface is kept stable.
In the above embodiment, the temperature above the base station is monitored in real time by the infrared thermometer, and the flow or the component of the cooling gas is accurately adjusted by the control system 04, so that the overall temperature can be kept stable.
In one embodiment, referring to FIG. 3, the abutment base 01 has a second cooling cavity 41 built therein, the second cooling cavity 41 being connected to a water cooling system 43 by a water cooling pipe 42; wherein the water cooling system 43 is connected to the control system 04; the control system 04 controls the water flow rate of the water cooling system 43 to dissipate heat from the base 01.
In the above embodiment, the heat dissipation is performed by adopting a water cooling mode for the relatively fixed base seat 01, so that the overall temperature of the base seat 01 can be reduced to a relatively stable temperature value, and the stability of the overall growth condition is maintained.
In summary, referring to fig. 7, fig. 7 is an electrical structure diagram of an MPCVD deposition chamber according to an embodiment, and as shown in the figure, a part of circuit structure is shown, a control system 04 of the MPCVD deposition chamber 10 controls a microwave source 06, and microwaves are fed into the chamber by a coaxial cable 12; the control camera 14 shoots a real-time image of the upper surface of the shielding base station 02 and performs image analysis, and outputs a relevant control signal to the digital piezoelectric controller of the first servo motor 31 to precisely control the movable base station 03 to move downwards; controlling the gas flow of the gas cooling system 34, and precisely controlling the temperature of the single crystal diamond substrate 11 on the movable base 03; the flow rate of the water cooling system 43 is controlled, and a control signal is outputted to control the second servo motor 26 to move the shielding base 02, so that the overall temperature is controlled to maintain a stable temperature value.
According to the technical scheme of the embodiments, the base station comprises functional parts such as microwave conveying, base station structure and control, base station cooling and the like, compact base station design for growing single crystal diamond can be carried out, and a liftable base station suitable for an MPCVD deposition cavity 10 fed by microwaves from the lower side is designed; meanwhile, the position of the single crystal diamond substrate 11 can be adjusted in real time in the growth process, the growth surface of the single crystal diamond substrate can be kept flush with the upper surface of the base table along with the thickness growth of the single crystal diamond, and the temperature of the surface of the base table can be controlled more accurately by combining the gas cooling structure design of the movable base table 03, so that the growth condition of the single crystal diamond substrate 11 near the growth surface in the growth process is kept stable all the time, and the preparation of the single crystal diamond with higher quality and larger size is realized.
An example of a method of growing single crystal diamond material based on MPCVD is set out below.
Referring to fig. 8, fig. 8 is a flowchart of a method of growing single crystal diamond material based on MPCVD, applied to a single crystal diamond material substrate based on MPCVD, comprising the steps of:
Step (1): in the initial state, the single crystal diamond substrate 11 is placed on the movable base 03, and the upper surface of the single crystal diamond substrate 11 is kept flush with the shielding base 02.
Illustratively, in arranging the single crystal diamond substrates 11, if thicker growth in the growth direction of the single crystal diamond is required, the diamond substrates may be closely arranged, for example, the distance between the single crystal diamond substrates 11 is less than 2mm, and the height of the movable stage 03 is adjusted so that the growth surface of the single crystal diamond is flush with the upper surface of the shielding stage 02; if the surface of the single crystal diamond grows along the periphery at the same time, the arrangement tightness degree of the diamond substrates is required to be reasonably adjusted, the compact arrangement is not required, and meanwhile, the movable base 03 is adjusted so that the growth surface of the single crystal diamond and the surface of the shielding base 02 are kept horizontal.
Illustratively, as in fig. 2, the side length of the square of the movable base 03 may be selected to be 30mm, 40mm or 50mm, and correspondingly, the single crystal diamond substrate 11 of 4×4×1mm3,6×6×1mm3, or 8×8×1mm3 is uniformly placed on the movable base 03.
In this embodiment, prior to step (1), the pretreatment of the single crystal diamond substrate 11, the start-up of the deposition apparatus, the etching of the substrate surface, and the methane gas injection may be further included.
Step (2): depositing single crystal diamond material on the surface of the single crystal diamond substrate 11; specifically, microwaves are fed in through a coaxial line by a microwave source, hydrogen plasma is excited on the surface of the single crystal diamond substrate 11, and a reaction gas is introduced to grow the single crystal diamond material.
Step (3): the control system 04 detects the alignment state of the surface of the single crystal diamond substrate 11 with the upper surface of the shield base 02 in real time, and controls the movable base 03 to move downward so that the surface of the single crystal diamond substrate 11 is kept flush with the upper surface of the shield base 02 in real time.
Illustratively, in the initial state, the diamond wafer of the movable stage 03 is uniformly placed on the movable stage 03, and the movable stage 03 is held flush with the shield stage 02 and fixed using a molybdenum plate. Then, a growth process is carried out, and along with the gradual growth of the surface of the single crystal diamond, a real-time image of the growth of the single crystal diamond is captured through a camera 14 on an observation window of a deposition cavity wall, the alignment state of the surface of the single crystal diamond and the upper surface of the shielding base 02 is determined, and the height of the movable base 03 is adjusted, so that the growth surface of the single crystal diamond is flush with the upper surface of the shielding base 02.
Further, the step (3) may further include:
Step (4): the control system 04 detects the real-time temperature of the surface of the single crystal diamond substrate 11 in real time, moves the shielding base 02 in real time according to the real-time temperature control, and adjusts the distance between the growth surface of the single crystal diamond substrate 11 and the plasma ball so that the surface temperature of the single crystal diamond substrate 11 keeps a stable value.
Illustratively, during single crystal diamond growth, the temperature of the growth surface is detected in real time using an infrared thermometer, and the surface temperature is maintained at a steady value by moving the shield base 02, in combination with adjusting the gas cooling system 34 and the water cooling system 43 to maintain the growth surface temperature steady.
According to the technical scheme of the embodiment, the position of the single crystal diamond substrate 11 can be adjusted in real time in the thickness growth process of the single crystal diamond, so that the growth surface of the single crystal diamond substrate is always kept flush with the upper surface of the shielding base 02, meanwhile, the electric fields of four non-growth side surfaces are shielded, and the growth condition near the growth surface is always kept stable; meanwhile, the surface temperature of the monocrystalline diamond substrate 11 can be controlled more accurately by moving the shielding base 02, so that the growth condition of the monocrystalline diamond near the growth surface is always kept stable in the growth process, and the preparation of the monocrystalline diamond with higher quality and larger size is realized.
The foregoing is only a partial embodiment of the present application, and it should be noted that it will be apparent to those skilled in the art that modifications and adaptations can be made without departing from the principles of the present application, and such modifications and adaptations are intended to be comprehended within the scope of the present application.
Claims (10)
1. A MPCVD-based submount for growing single crystal diamond material for use in an MPCVD deposition chamber, comprising:
the base station base is used for supporting the base station and serving as a coupling antenna, and maintaining the focusing distribution of the electric field intensity above the base station base;
The shielding base station is arranged in the middle of the base station base and used for wrapping the side surface of the monocrystalline diamond substrate and shielding electric field distribution around the side surface of the monocrystalline diamond substrate;
The movable base station is embedded in the middle of the shielding base station and is used for bearing the monocrystalline diamond substrate and moving up and down relative to the shielding base station;
When growing single crystal diamond, feeding microwaves from the lower part of the base table to enable the base table to form a strong electric field area, and exciting hydrogen plasma to grow single crystal diamond materials on the surface of the single crystal diamond substrate; the control system moves the movable base table in real time according to the surface thickness change of the single crystal diamond substrate, the surface of the single crystal diamond substrate is kept flush with the upper surface of the shielding base table in real time, so that the side wall of the concave part of the shielding base table is close to and wraps the side surface of the single crystal diamond substrate, and the peripheral electric field distribution is shielded to inhibit the growth of polycrystalline diamond.
2. A submount for growing single crystal diamond material based on MPCVD according to claim 1, wherein the shield submount is of a removable design;
the control system is also used for moving the shielding base table in real time according to the temperature change of the growth surface of the single crystal diamond substrate so as to adjust the distance between the growth surface of the single crystal diamond substrate and the plasma ball and maintain the growth condition of the growth surface of the single crystal diamond substrate stable.
3. A base station for growing single crystal diamond material based on MPCVD according to claim 1, wherein a molybdenum sheet is provided on the upper surface of the movable base station as a substrate tray; the single crystal diamond substrate is uniformly placed on the substrate tray;
and a metal gasket is arranged at the upper part of the shielding base station and used for fixing the monocrystalline diamond substrate.
4. A stage for MPCVD-based growth of single crystal diamond material according to claim 2, wherein the movable stage is connected to a first servo motor, the first servo motor being connected to a control system;
the shielding base station is connected with a second servo motor, and the second servo motor is connected with a control system;
And the control system controls the first servo motor to drive the movable base station to move and controls the second servo motor to drive the shielding base station to move according to the growth state and the temperature change of the surface of the monocrystalline diamond substrate monitored in real time.
5. The MPCVD-based single crystal diamond material growth submount of claim 1, wherein a camera is further provided outside the viewing window of the MPCVD deposition chamber, the camera being oriented flush with the upper surface of the shield submount;
the camera shoots a real-time image of the upper surface of the shielding base station and transmits the real-time image to the control system;
and the control system determines the alignment state of the surface of the monocrystalline diamond substrate and the upper surface of the shielding base station according to the pixel points of the monocrystalline diamond appearing in the real-time image, and outputs a related control signal to the first servo motor to drive the movable base station to move.
6. A submount for growing single crystal diamond material based on MPCVD as described in claim 1 further comprising: a light detection device; wherein the light detection device comprises a microprocessor, a light emitting device and a light receiving device;
The light emitting device and the light receiving device are respectively arranged on two opposite observation windows of the MPCVD deposition cavity;
The microprocessor controls the light emitting device to emit light rays with set wavelength, and the light receiving device receives the light rays;
The microprocessor detects the intensity of the received light, and if the intensity of the light is smaller than a threshold value, outputs a relevant control signal to the linear driving structure to control the movable base station to move, so that the surface of the monocrystalline diamond substrate and the upper surface of the shielding base station are kept flush in real time.
7. A stage for MPCVD-based growth of single crystal diamond material according to claim 1, wherein the movable stage has a first cooling chamber built-in, the first cooling chamber being connected to an air cooling system by an air cooling duct; wherein the air cooling system is connected to a control system;
The control system controls the gas flow of the gas cooling system to adjust the temperatures of the movable base station and the monocrystalline diamond substrate;
The shielding base is internally provided with a second cooling cavity which is connected to a water cooling system through a water cooling pipeline; wherein the water cooling system is connected to a control system;
The control system controls the water flow of the water cooling system so as to radiate the shielding base station.
8. A base station for MPCVD-based growth of single crystal diamond material according to claim 7, wherein the air-cooled tube is a hard tube; an infrared thermometer is also arranged above the movable base station;
the air cooling pipeline is movably connected with a first cooling cavity in the movable base station in a nested mode;
The air inlet and the air outlet connected with the air cooling pipeline are centrally symmetrical in the first cooling cavity, so that the temperature distribution on the surface of the movable base station is uniform;
the infrared thermometer is used for detecting the real-time temperature of the surface of the monocrystalline diamond substrate;
the control system controls the gas flow of the gas cooling system according to the real-time temperature.
9. A method of MPCVD-based growing single crystal diamond material for use in a MPCVD-based growing single crystal diamond material substrate according to any one of claims 1 to 8, comprising:
placing a single crystal diamond substrate on the movable base station, and keeping the upper surface of the single crystal diamond substrate flush with the shielding base station;
depositing a single crystal diamond material on the surface of the single crystal diamond substrate;
The control system detects the alignment state of the surface of the single crystal diamond substrate and the upper surface of the shielding base table in real time, and controls the movable base table to move downwards, so that the surface of the single crystal diamond substrate and the upper surface of the shielding base table are kept flush in real time.
10. A method of growing single crystal diamond material based on MPCVD according to claim 9, further comprising:
The control system detects the real-time temperature of the surface of the monocrystalline diamond substrate in real time, the shielding base station is moved according to the real-time temperature, and the distance between the growth surface of the monocrystalline diamond substrate and the plasma ball is adjusted so that the surface temperature of the monocrystalline diamond substrate keeps a stable value.
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| CN202311670318.6A CN117535791B (en) | 2023-12-06 | MPCVD-based substrate for growing single crystal diamond material and method thereof |
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| CN202311670318.6A CN117535791B (en) | 2023-12-06 | MPCVD-based substrate for growing single crystal diamond material and method thereof |
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