A graphite etching method, system and terminal without interrupting diamond growth
By etching the graphite on quartz in the MPCVD equipment, the problem of equipment shutdown caused by graphite deposition during single crystal diamond cultivation is solved, and the normal growth of diamond and the extension of single growth time are achieved.
Patent Information
- Application Number
- CN202411978371.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-04
- Estimated Expiration
- 2044-12-31
AI Technical Summary
During the cultivation of single crystal diamonds, a large amount of graphite deposits will appear above the quartz in the MPCVD equipment, causing abnormal shutdown of the equipment and affecting the normal growth of diamonds.
By adjusting the process gas ratio and cooling treatment in the first growth environment where the single crystal diamond is to be grown, a second growth environment is obtained, and the second stage of the diamond is grown in this environment, and the graphite on the quartz in the MPCVD device is etched under a low methane atmosphere.
It realizes effective removal of graphite deposition without interrupting diamond growth and equipment shutdown, ensuring the normal growth of diamonds, and improving the single growth time of diamonds.
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Figure CN119392209B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of diamond cultivation, and in particular to a graphite etching method, system, terminal and computer-readable storage medium without interrupting diamond growth. Background Art
[0002] Diamond has attracted everyone's attention due to its extremely excellent physical and chemical properties. However, the reserves of natural diamond are limited, so people have developed a variety of synthetic diamond methods, such as high temperature and high pressure method (HPHT, High pressure Hightemperature), hot filament chemical vapor deposition method (HFCVD, hot filament chemical vapor deposition), etc. Among them, microwave plasma chemical vapor deposition (MPCVD, Microwave plasma chemical vapordeposition) is a synthetic diamond method that can synthesize high-quality and large-area diamonds without the introduction of impurities. It has the advantages of no electrode discharge pollution, fast deposition rate, good stability, etc., and is considered to be the best method for preparing high-quality single-crystal diamonds.
[0003] However, in the existing single crystal diamond growth process, a large amount of graphite deposition will appear on the quartz in the MPCVD equipment, which will lead to poor quartz heat dissipation, excessive local temperature and inability to transmit microwaves normally. As a result, the reflected microwaves gradually increase during the growth of single crystal diamonds, which can easily lead to abnormal shutdown of the MPCVD equipment and affect the normal growth of diamonds.
[0004] Therefore, the prior art still needs to be improved and developed. Summary of the invention
[0005] The main purpose of the present invention is to provide a graphite etching method, system, terminal and computer-readable storage medium that do not interrupt diamond growth, aiming to solve the problem in the prior art that during the single crystal diamond cultivation process, a large amount of graphite deposition will appear above the quartz in the MPCVD equipment, which may easily cause the MPCVD equipment to shut down abnormally and affect the normal growth of diamond.
[0006] To achieve the above object, the present invention provides a graphite etching method without interrupting diamond growth, the graphite etching method without interrupting diamond growth comprising the following steps:
[0007] Determining a single crystal diamond to be grown and a first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment;
[0008] When the first stage growth process of the single crystal diamond to be grown is completed, the first growth environment is subjected to a process gas ratio adjustment process and a temperature reduction process to obtain a second growth environment;
[0009] The single crystal diamond to be grown is subjected to a second stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result.
[0010] Optionally, the graphite etching method without interrupting diamond growth, wherein the determining of the single crystal diamond to be grown and the first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment, specifically includes:
[0011] Determine a single crystal diamond to be grown and a first growth environment, wherein the first growth environment includes a first preset process gas at a first preset concentration ratio, a second preset process gas at a second preset concentration ratio, a third preset process gas at a third preset concentration ratio, a fourth preset process gas at a fourth preset concentration ratio, a fifth preset process gas at a fifth preset concentration ratio, a preset gas pressure range, a preset power range, and a first preset temperature range;
[0012] The single crystal diamond to be grown is placed in the first growth environment, and a first stage growth process is performed on the single crystal diamond to be grown according to the first growth environment.
[0013] Optionally, the graphite etching method without interrupting diamond growth, wherein when the first stage growth process of the single crystal diamond to be grown is completed, the first growth environment is subjected to process gas ratio adjustment and temperature reduction process to obtain a second growth environment, specifically comprising:
[0014] When the growth time of the single crystal diamond to be grown in the first growth environment reaches a first preset growth time range, it indicates that the first stage growth process of the single crystal diamond to be grown is completed;
[0015] The second preset process gas and the fourth preset process gas in the first growth environment are subjected to a process gas ratio adjustment process, and the first preset temperature range in the first growth environment is subjected to a temperature reduction process to obtain a second growth environment.
[0016] Optionally, the graphite etching method without interrupting diamond growth, wherein the process gas ratio adjustment process is performed on the second preset process gas and the fourth preset process gas in the first growth environment, and the first preset temperature range in the first growth environment is cooled to obtain the second growth environment, specifically comprising:
[0017] Within a first preset time range, reducing the second preset concentration ratio of the second preset process gas in the first growth environment to a sixth preset concentration ratio to obtain the second preset process gas of the sixth preset concentration ratio;
[0018] Within a second preset time range, reducing the fourth preset concentration ratio of the fourth preset process gas in the first growth environment to a seventh preset concentration ratio to obtain the fourth preset process gas of the seventh preset concentration ratio;
[0019] Lowering the first preset temperature range in the first growth environment to a second preset temperature range to obtain a second growth environment;
[0020] Among them, the second growth environment includes the first preset process gas at the first preset concentration ratio, the second preset process gas at the sixth preset concentration ratio, the third preset process gas at the third preset concentration ratio, the fourth preset process gas at the seventh preset concentration ratio, the fifth preset process gas at the fifth preset concentration ratio, the preset gas pressure range, the preset power range and the second preset temperature range.
[0021] Optionally, the graphite etching method without interrupting diamond growth, wherein the second stage growth treatment is performed on the single crystal diamond to be grown according to the second growth environment to obtain the target single crystal diamond, specifically comprising:
[0022] Performing a second stage growth process on the single crystal diamond to be grown according to the second growth environment;
[0023] When the growth time of the single crystal diamond to be grown in the second growth environment reaches a second preset growth time range, it indicates that the second stage growth process of the single crystal diamond to be grown is completed and the target single crystal diamond is obtained.
[0024] Optionally, the graphite etching method without interrupting diamond growth, wherein the etching process is performed on the graphite on the quartz in the MPCVD device according to the second growth environment to obtain the graphite etching result, specifically comprising:
[0025] performing an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment;
[0026] When the etching time of the graphite reaches the second preset growth time range, determining whether the graphite is completely etched;
[0027] If so, it is determined that the graphite etching process is completed and a graphite etching result is obtained.
[0028] Optionally, the graphite etching method without interrupting diamond growth, wherein the single crystal diamond to be grown is subjected to a second-stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result, and then further comprises:
[0029] When the second stage growth process of the single crystal diamond to be grown is completed and the etching process of the graphite is completed, restoring the second growth environment to the first growth environment within a third preset time range;
[0030] The target single crystal diamond is subjected to a third stage growth process according to the first growth environment to obtain a third stage single crystal diamond.
[0031] In addition, to achieve the above-mentioned purpose, the present invention also provides a graphite etching system without interrupting diamond growth, wherein the graphite etching system without interrupting diamond growth comprises:
[0032] A first stage growth processing module, used to determine the single crystal diamond to be grown and a first growth environment, and perform a first stage growth processing on the single crystal diamond to be grown according to the first growth environment;
[0033] A second growth environment generating module is used for, when the first stage growth process of the single crystal diamond to be grown is completed, performing a process gas ratio adjustment process and a temperature reduction process on the first growth environment to obtain a second growth environment;
[0034] The graphite etching module is used to perform a second stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond, and to perform an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result.
[0035] In addition, to achieve the above-mentioned purpose, the present invention also provides a terminal, wherein the terminal includes: a memory, a processor, and a graphite etching program for not interrupting diamond growth stored in the memory and runnable on the processor, wherein the graphite etching program for not interrupting diamond growth, when executed by the processor, implements the steps of the graphite etching method for not interrupting diamond growth as described above.
[0036] In addition, to achieve the above-mentioned purpose, the present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a graphite etching program without interrupting diamond growth, and when the graphite etching program without interrupting diamond growth is executed by a processor, the steps of the graphite etching method without interrupting diamond growth as described above are implemented.
[0037] In the present invention, a single crystal diamond to be grown and a first growth environment are determined, and the single crystal diamond to be grown is subjected to a first stage growth treatment according to the first growth environment; when the first stage growth treatment of the single crystal diamond to be grown is completed, the first growth environment is subjected to a process gas ratio adjustment treatment and a temperature reduction treatment to obtain a second growth environment; the single crystal diamond to be grown is subjected to a second stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result. The present invention obtains a second growth environment by performing a process gas ratio adjustment treatment and a temperature reduction treatment on the first growth environment in which the single crystal diamond to be grown is located. On the basis of the second growth environment, the graphite on the quartz in the MPCVD device can be removed without interrupting the diamond growth and the equipment shutting down, which not only effectively ensures the normal growth of the diamond, but also effectively increases the single growth time of the diamond. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] Figure 1 It is a flow chart of a preferred embodiment of the graphite etching method without interrupting diamond growth of the present invention;
[0039] Figure 2 It is a structural diagram of a preferred embodiment of the graphite etching system without interrupting diamond growth of the present invention;
[0040] Figure 3 It is a structural diagram of a preferred embodiment of the terminal of the present invention. DETAILED DESCRIPTION
[0041] In order to make the purpose, technical solution and advantages of the present invention clearer and more specific, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0042] Diamond has attracted everyone's attention due to its extremely excellent physical and chemical properties. However, the reserves of natural diamonds are limited, so people have developed a variety of synthetic diamond methods, such as high temperature and high pressure method, hot wire chemical vapor deposition method, etc. Among them, microwave plasma chemical vapor deposition method, a synthetic diamond method, can synthesize high-quality and large-area diamonds without the introduction of impurities. It has the advantages of no electrode discharge pollution, fast deposition rate, good stability, etc., and is considered to be the best method for preparing high-quality single-crystal diamonds.
[0043] At present, the mainstream technology route for synthesizing diamonds by chemical vapor deposition is MPCVD (microwave plasma chemical vapor deposition), which is the most mature technology and the most widely used in the market. The advantages of MPCVD technology are: 1. The reaction chamber is larger, which is more suitable for cultivating large-grain diamonds; 2. No electrodes are required during the plasma generation process, and electrode impurities will not be introduced, making it easier to cultivate high-purity diamonds.
[0044] In the prior art, when using MPCVD cylindrical cavity equipment to grow single crystal diamond, a large amount of graphite deposition will appear on the quartz (after plasma decomposition, part of the carbon will be deposited on the quartz), resulting in poor quartz heat dissipation, excessive local temperature, and inability to transmit microwaves normally. As a result, the reflected microwaves gradually increase during the growth of single crystal diamond, and the equipment will eventually shut down abnormally due to quartz ablation, reflection jumps, or fireball jumps.
[0045] The graphite etching method without interrupting diamond growth described in the preferred embodiment of the present invention is as follows: Figure 1 As shown, the graphite etching method without interrupting diamond growth comprises the following steps:
[0046] Step S10, determining a single crystal diamond to be grown and a first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment.
[0047] The etching of graphite on the MPCVD equipment needs to be carried out after the diamond has grown for a period of time, that is, the etching of graphite needs to meet certain preset conditions. Prior to this, the diamond needs to be grown in a normal growth environment (i.e., the first growth environment in the present invention) for a period of time.
[0048] Specifically, determine a single crystal diamond to be grown and a first growth environment, wherein the first growth environment includes a first preset process gas at a first preset concentration ratio, a second preset process gas at a second preset concentration ratio, a third preset process gas at a third preset concentration ratio, a fourth preset process gas at a fourth preset concentration ratio, a fifth preset process gas at a fifth preset concentration ratio, a preset gas pressure range, a preset power range, and a first preset temperature range; place the single crystal diamond to be grown in the first growth environment, and perform a first stage growth treatment on the single crystal diamond to be grown according to the first growth environment.
[0049] First, it is necessary to grow the single crystal diamond to be grown in a normal formula (i.e., the first growth environment in the present invention) for 200-250 hours (i.e., the first preset growth time range in the present invention), wherein the normal formula is: 500 sccm of hydrogen (i.e., the first preset process gas of the first preset concentration ratio in the present invention), 0.02%-0.1% of nitrogen (i.e., the second preset process gas of the second preset concentration ratio in the present invention), 0.002%-0.006% of oxygen (i.e., the third preset process gas of the third preset concentration ratio in the present invention), 5%-10% of methane (i.e., the fourth preset process gas of the fourth preset concentration ratio in the present invention), about 1% of argon (i.e., the fifth preset process gas of the fifth preset concentration ratio in the present invention), constant gas pressure, constant power and constant temperature of 900-960°C (i.e., the first preset temperature range in the present invention).
[0050] Step S20: When the first stage growth process of the single crystal diamond to be grown is completed, the first growth environment is subjected to a process gas ratio adjustment process and a temperature reduction process to obtain a second growth environment.
[0051] When the first stage growth process of the single crystal diamond to be grown is completed, it is necessary to prepare the conditions for etching graphite without interrupting the diamond growth, that is, to construct a second growth environment, wherein the second growth environment needs to reduce the concentration ratio of nitrogen and methane relative to the first growth environment, so as to promote the hydrogen and oxygen therein to remove the graphite on the quartz in the MPCVD device. At the same time, the concentration ratio of methane will not drop to zero, but will remain at a low concentration, so that the diamond growth will not stop.
[0052] Specifically, when the growth time of the single crystal diamond to be grown in the first growth environment reaches a first preset growth time range, it indicates that the first stage growth process of the single crystal diamond to be grown is completed; within the first preset time range, the second preset concentration ratio of the second preset process gas in the first growth environment is reduced to a sixth preset concentration ratio to obtain the second preset process gas of the sixth preset concentration ratio; within the second preset time range, the fourth preset concentration ratio of the fourth preset process gas in the first growth environment is reduced to a seventh preset concentration ratio to obtain the fourth preset process gas of the seventh preset concentration ratio; the first preset temperature range in the first growth environment is reduced to a second preset temperature range to obtain a second growth environment; wherein the second growth environment includes the first preset process gas of the first preset concentration ratio, the second preset process gas of the sixth preset concentration ratio, the third preset process gas of the third preset concentration ratio, the fourth preset process gas of the seventh preset concentration ratio, the fifth preset process gas of the fifth preset concentration ratio, the preset gas pressure range, the preset power range and the second preset temperature range.
[0053] Most of the black deposits on top of the quartz in the MPCVD equipment are graphite, and graphite is easily etched by hydrogen or oxygen. Therefore, in order to extend the single-use time of the MPCVD equipment, a more reliable method is to etch the graphite without stopping the machine, that is, to interrupt the input of gases such as methane and nitrogen that directly affect the growth for a short time. However, if the input values of methane and nitrogen are directly set to 0, the atmosphere conditions in the reaction chamber of the MPCVD equipment will change too much in a short period of time, causing a sudden temperature change and being forced to shut down; and methane being 0 means that the normal growth of the growing diamond is directly interrupted, and the surface will be etched and destroyed by plasmas with etching effects such as hydrogen and oxygen. When the growing diamond resumes growth again, it needs to be re-nucleated, which will aggravate the defect expression on the crystal surface.
[0054] Based on the above considerations, the present invention slowly (slowly reducing nitrogen input, generally controlled within 10 minutes) interrupts nitrogen input (wherein, the input amount of nitrogen can be adjusted according to different processes, for example, from 0.02%-0.1% to 0 within 10 minutes, where the sixth preset concentration ratio in the present invention is 0) when the single crystal diamond (i.e., the diamond to be grown in the present invention) grows to about 200-250 hours (i.e., the first preset growth time range in the present invention) and reduces the input ratio of methane, which generally needs to be reduced to about 1% of the overall ratio (i.e., the seventh preset concentration ratio in the present invention). At this time, with the change in the ratio of nitrogen and methane, the growth temperature in the reaction chamber is also reduced by about 30-40°C (i.e., the second preset temperature range in the present invention, which is 900-960°C under normal circumstances), and the second growth environment is formed. In the low methane atmosphere of this second growth environment, the diamond to be grown is grown uninterruptedly, and the graphite on the quartz is etched under the low methane state (the etching time is about 2-3 hours).
[0055] It is understood that when the diamond to be grown is grown for 200-250 hours under the normal formula (i.e. the first preset growth time range in the present invention), nitrogen is preferentially and slowly removed under the conditions of constant pressure and constant power (because nitrogen will affect the color of the diamond blank), and the nitrogen flow rate is reduced from 0.02%-0.1% (i.e. the second preset concentration ratio in the present invention) to 0 (i.e. the sixth preset concentration ratio in the present invention) within 10 minutes (i.e. the first preset time range in the present invention), and the temperature is also increased within 20 minutes (i.e. the second preset time range in the present invention). The temperature will change, and generally the time for the temperature to change to stability is 20 minutes. The proportion of methane is slowly reduced from the original 5%-10% (i.e., the fourth preset concentration ratio in the present invention) to 1% (i.e., the seventh preset concentration ratio in the present invention), and the flow rates of other gases such as oxygen and hydrogen remain unchanged. During the atmosphere stabilization process (restoring normal growth atmosphere conditions within 5 minutes), the temperature will drop by about 30-40°C (i.e., the second preset temperature range in the present invention). Under this process condition (i.e., the second growth environment in the present invention), it will grow for about 2-3 hours (i.e., the second preset growth time range in the present invention).
[0056] Step S30, performing a second stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond, and etching the graphite on the quartz in the MPCVD equipment according to the second growth environment to obtain a graphite etching result.
[0057] When the second growth environment is constructed, diamond growth can continue based on the low concentration of methane in the second growth environment. At the same time, hydrogen and oxygen in the second growth environment will etch and remove graphite on the quartz in the MPCVD equipment to achieve graphite removal without interrupting diamond growth.
[0058] Specifically, the second stage growth treatment is performed on the single crystal diamond to be grown according to the second growth environment; when the growth time of the single crystal diamond to be grown in the second growth environment reaches a second preset growth time range, it indicates that the second stage growth treatment of the single crystal diamond to be grown is completed, and the target single crystal diamond is obtained.
[0059] The graphite on the quartz in the MPCVD device is etched according to the second growth environment; when the etching time of the graphite reaches the second preset growth time range, it is determined whether the graphite is completely etched; if so, it is determined that the graphite etching process is completed and a graphite etching result is obtained.
[0060] Furthermore, when the second stage growth treatment of the single crystal diamond to be grown is completed and the etching treatment of the graphite is completed, the second growth environment is restored to the first growth environment within a third preset time range; and the target single crystal diamond is subjected to a third stage growth treatment according to the first growth environment to obtain a third stage single crystal diamond.
[0061] When the graphite above the quartz in the MPCVD equipment is reduced to nothing (that is, the graphite etching process is completed), the normal formula is slowly restored (that is, the second growth environment is restored to the first growth environment) without changing the gas pressure and power. It is recommended that the time for restoring the nitrogen and methane concentration ratio is 10-20 minutes (that is, within the third preset time range of the present invention). When the atmosphere conditions are stable (that is, after returning to the first growth environment), growth is carried out at a constant temperature after about 20 minutes (that is, the third stage growth process of the target single crystal diamond is started).
[0062] During the normal growth process, the present invention increases the low methane growth time, which accounts for about 0.5%-0.6% of the total growth time, so as to achieve the purpose of uninterrupted diamond growth and etching quartz graphite. At the same time, it also effectively prolongs the entire single growth time of the single crystal diamond.
[0063] In summary, the present invention can effectively reduce the problem that diamond cannot grow for a long time due to graphite deposition. Through the graphite etching method of the present invention that does not interrupt diamond growth, the original single growth time of diamond (the original single growth time is 150-200 hours) can be extended to at least 400-500 hours.
[0064] Furthermore, if Figure 2 As shown, based on the above-mentioned graphite etching method without interrupting diamond growth, the present invention also provides a graphite etching system without interrupting diamond growth, wherein the graphite etching system without interrupting diamond growth includes:
[0065] The first stage growth processing module 51 is used to determine the single crystal diamond to be grown and the first growth environment, and perform the first stage growth processing on the single crystal diamond to be grown according to the first growth environment;
[0066] A second growth environment generating module 52 is used for, when the first stage growth process of the single crystal diamond to be grown is completed, adjusting the process gas ratio and cooling the first growth environment to obtain a second growth environment;
[0067] The graphite etching module 53 is used to perform a second stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond, and to perform an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result.
[0068] Furthermore, if Figure 3 As shown, based on the above-mentioned graphite etching method and system without interrupting diamond growth, the present invention also provides a terminal accordingly, and the terminal includes a processor 10, a memory 20 and a display 30. Figure 3 Only some components of the terminal are shown, but it should be understood that it is not required to implement all of the components shown, and more or fewer components may be implemented instead.
[0069] In some embodiments, the memory 20 may be an internal storage unit of the terminal, such as a hard disk or memory of the terminal. In other embodiments, the memory 20 may also be an external storage device of the terminal, such as a plug-in hard disk, a smart media card (SMC), a secure digital (SD) card, a flash card, etc. equipped on the terminal. Further, the memory 20 may also include both an internal storage unit of the terminal and an external storage device. The memory 20 is used to store application software and various types of data installed in the terminal, such as the program code of the installation terminal. The memory 20 may also be used to temporarily store data that has been output or is to be output. In one embodiment, a graphite etching program 40 that does not interrupt diamond growth is stored on the memory 20, and the graphite etching program 40 that does not interrupt diamond growth can be executed by the processor 10, thereby realizing the graphite etching method that does not interrupt diamond growth in the present application.
[0070] In some embodiments, the processor 10 may be a central processing unit (CPU), a microprocessor or other data processing chip, used to run the program code or process data stored in the memory 20, such as executing the graphite etching method without interrupting diamond growth.
[0071] In some embodiments, the display 30 may be an LED display, a liquid crystal display, a touch-sensitive liquid crystal display, an OLED (Organic Light-Emitting Diode) touch device, etc. The display 30 is used to display information on the terminal and to display a visual user interface.
[0072] In one embodiment, when the processor 10 executes the graphite etching program 40 in the memory 20 without interrupting diamond growth, the following steps are implemented:
[0073] Determining a single crystal diamond to be grown and a first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment;
[0074] When the first stage growth process of the single crystal diamond to be grown is completed, the first growth environment is subjected to a process gas ratio adjustment process and a temperature reduction process to obtain a second growth environment;
[0075] The single crystal diamond to be grown is subjected to a second stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result.
[0076] The step of determining the single crystal diamond to be grown and a first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment, specifically includes:
[0077] Determine a single crystal diamond to be grown and a first growth environment, wherein the first growth environment includes a first preset process gas at a first preset concentration ratio, a second preset process gas at a second preset concentration ratio, a third preset process gas at a third preset concentration ratio, a fourth preset process gas at a fourth preset concentration ratio, a fifth preset process gas at a fifth preset concentration ratio, a preset gas pressure range, a preset power range, and a first preset temperature range;
[0078] The single crystal diamond to be grown is placed in the first growth environment, and a first stage growth process is performed on the single crystal diamond to be grown according to the first growth environment.
[0079] When the first stage growth process of the single crystal diamond to be grown is completed, the first growth environment is subjected to process gas ratio adjustment and temperature reduction process to obtain a second growth environment, specifically including:
[0080] When the growth time of the single crystal diamond to be grown in the first growth environment reaches a first preset growth time range, it indicates that the first stage growth process of the single crystal diamond to be grown is completed;
[0081] The second preset process gas and the fourth preset process gas in the first growth environment are subjected to a process gas ratio adjustment process, and the first preset temperature range in the first growth environment is subjected to a temperature reduction process to obtain a second growth environment.
[0082] The step of adjusting the ratio of the second preset process gas and the fourth preset process gas in the first growth environment and cooling the first preset temperature range in the first growth environment to obtain the second growth environment specifically includes:
[0083] Within a first preset time range, reducing the second preset concentration ratio of the second preset process gas in the first growth environment to a sixth preset concentration ratio to obtain the second preset process gas of the sixth preset concentration ratio;
[0084] Within a second preset time range, reducing the fourth preset concentration ratio of the fourth preset process gas in the first growth environment to a seventh preset concentration ratio to obtain the fourth preset process gas of the seventh preset concentration ratio;
[0085] Lowering the first preset temperature range in the first growth environment to a second preset temperature range to obtain a second growth environment;
[0086] Among them, the second growth environment includes the first preset process gas at the first preset concentration ratio, the second preset process gas at the sixth preset concentration ratio, the third preset process gas at the third preset concentration ratio, the fourth preset process gas at the seventh preset concentration ratio, the fifth preset process gas at the fifth preset concentration ratio, the preset gas pressure range, the preset power range and the second preset temperature range.
[0087] The step of performing a second-stage growth process on the single-crystal diamond to be grown according to the second growth environment to obtain a target single-crystal diamond specifically includes:
[0088] Performing a second stage growth process on the single crystal diamond to be grown according to the second growth environment;
[0089] When the growth time of the single crystal diamond to be grown in the second growth environment reaches a second preset growth time range, it indicates that the second stage growth process of the single crystal diamond to be grown is completed and the target single crystal diamond is obtained.
[0090] The etching of graphite on quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result specifically includes:
[0091] performing an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment;
[0092] When the etching time of the graphite reaches the second preset growth time range, determining whether the graphite is completely etched;
[0093] If so, it is determined that the graphite etching process is completed and a graphite etching result is obtained.
[0094] Wherein, the second growth environment is used to perform a second stage growth process on the single crystal diamond to be grown to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result, and then the following steps are further included:
[0095] When the second stage growth process of the single crystal diamond to be grown is completed and the etching process of the graphite is completed, restoring the second growth environment to the first growth environment within a third preset time range;
[0096] The target single crystal diamond is subjected to a third stage growth process according to the first growth environment to obtain a third stage single crystal diamond.
[0097] The present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a graphite etching program without interrupting diamond growth, and when the graphite etching program without interrupting diamond growth is executed by a processor, the steps of the graphite etching method without interrupting diamond growth as described above are implemented.
[0098] In summary, the present invention provides a graphite etching method and related equipment without interrupting diamond growth, the method comprising: determining a single crystal diamond to be grown and a first growth environment, and performing a first stage growth treatment on the single crystal diamond to be grown according to the first growth environment; when the first stage growth treatment of the single crystal diamond to be grown is completed, the first growth environment is subjected to a process gas ratio adjustment treatment and a temperature reduction treatment to obtain a second growth environment; the single crystal diamond to be grown is subjected to a second stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result. The present invention obtains a second growth environment by performing a process gas ratio adjustment treatment and a temperature reduction treatment on the first growth environment where the single crystal diamond to be grown is located. On the basis of the second growth environment, the graphite on the quartz in the MPCVD device can be removed without interrupting the diamond growth and the equipment being shut down, which not only effectively ensures the normal growth of the diamond, but also effectively increases the single growth time of the diamond.
[0099] It should be noted that, in this article, the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or terminal including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or terminal. In the absence of further restrictions, an element defined by the sentence "comprises a ..." does not exclude the presence of other identical elements in the process, method, article or terminal including the element.
[0100] Of course, those skilled in the art can understand that all or part of the processes in the above-mentioned embodiments can be implemented by instructing related hardware (such as a processor, a controller, etc.) through a computer program, and the program can be stored in a computer-readable storage medium that can be read by a computer, and the program can include the processes of the above-mentioned method embodiments when executed. The computer-readable storage medium can be a memory, a disk, an optical disk, etc.
[0101] It should be understood that the application of the present invention is not limited to the above examples. For ordinary technicians in this field, improvements or changes can be made based on the above description. All these improvements and changes should fall within the scope of protection of the claims attached to the present invention.
Claims
1. A graphite etching method without interrupting diamond growth, characterized in that: The graphite etching method without interrupting diamond growth comprises: Determining a single crystal diamond to be grown and a first growth environment, and performing a first stage growth process on the single crystal diamond to be grown according to the first growth environment; Wherein, the first growth environment includes a first preset process gas at a first preset concentration ratio, a second preset process gas at a second preset concentration ratio, a third preset process gas at a third preset concentration ratio, a fourth preset process gas at a fourth preset concentration ratio, a fifth preset process gas at a fifth preset concentration ratio, a preset gas pressure range, a preset power range, and a first preset temperature range; Wherein, the first preset process gas is hydrogen, the second preset process gas is nitrogen, the third preset process gas is oxygen, the fourth preset process gas is methane, and the fifth preset process gas is argon; When the growth time of the single crystal diamond to be grown in the first growth environment reaches a first preset growth time range, it indicates that the first stage growth process of the single crystal diamond to be grown is completed; Within a first preset time range, reducing the second preset concentration ratio of the second preset process gas in the first growth environment to a sixth preset concentration ratio to obtain the second preset process gas of the sixth preset concentration ratio; Within a second preset time range, reducing the fourth preset concentration ratio of the fourth preset process gas in the first growth environment to a seventh preset concentration ratio to obtain the fourth preset process gas of the seventh preset concentration ratio; Lowering the first preset temperature range in the first growth environment to a second preset temperature range to obtain a second growth environment; Wherein, the second growth environment includes the first preset process gas at the first preset concentration ratio, the second preset process gas at the sixth preset concentration ratio, the third preset process gas at the third preset concentration ratio, the fourth preset process gas at the seventh preset concentration ratio, the fifth preset process gas at the fifth preset concentration ratio, the preset gas pressure range, the preset power range and the second preset temperature range; The single crystal diamond to be grown is subjected to a second stage growth treatment according to the second growth environment to obtain a target single crystal diamond, and the graphite on the quartz in the MPCVD device is etched according to the second growth environment to obtain a graphite etching result.
2. The graphite etching method without interrupting diamond growth according to claim 1, characterized in that: The step of performing a second stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond specifically includes: Performing a second stage growth process on the single crystal diamond to be grown according to the second growth environment; When the growth time of the single crystal diamond to be grown in the second growth environment reaches a second preset growth time range, it indicates that the second stage growth process of the single crystal diamond to be grown is completed and the target single crystal diamond is obtained.
3. The graphite etching method without interrupting diamond growth according to claim 2, characterized in that: The etching of graphite on quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result specifically includes: performing an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment; When the etching time of the graphite reaches the second preset growth time range, determining whether the graphite is completely etched; If so, it is determined that the graphite etching process is completed and a graphite etching result is obtained.
4. The graphite etching method without interrupting diamond growth according to claim 1, characterized in that: The method further comprises: performing a second-stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond, and etching the graphite on the quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result, and then further comprising: When the second stage growth process of the single crystal diamond to be grown is completed and the etching process of the graphite is completed, restoring the second growth environment to the first growth environment within a third preset time range; The target single crystal diamond is subjected to a third stage growth process according to the first growth environment to obtain a third stage single crystal diamond.
5. A graphite etching system without interrupting diamond growth, characterized in that: The graphite etching system without interrupting diamond growth comprises: A first stage growth processing module, used to determine the single crystal diamond to be grown and a first growth environment, and perform a first stage growth processing on the single crystal diamond to be grown according to the first growth environment; Wherein, the first growth environment includes a first preset process gas at a first preset concentration ratio, a second preset process gas at a second preset concentration ratio, a third preset process gas at a third preset concentration ratio, a fourth preset process gas at a fourth preset concentration ratio, a fifth preset process gas at a fifth preset concentration ratio, a preset gas pressure range, a preset power range, and a first preset temperature range; Wherein, the first preset process gas is hydrogen, the second preset process gas is nitrogen, the third preset process gas is oxygen, the fourth preset process gas is methane, and the fifth preset process gas is argon; When the growth time of the single crystal diamond to be grown in the first growth environment reaches a first preset growth time range, it indicates that the first stage growth process of the single crystal diamond to be grown is completed; Within a first preset time range, reducing the second preset concentration ratio of the second preset process gas in the first growth environment to a sixth preset concentration ratio to obtain the second preset process gas of the sixth preset concentration ratio; Within a second preset time range, reducing the fourth preset concentration ratio of the fourth preset process gas in the first growth environment to a seventh preset concentration ratio to obtain the fourth preset process gas of the seventh preset concentration ratio; Lowering the first preset temperature range in the first growth environment to a second preset temperature range to obtain a second growth environment; Wherein, the second growth environment includes the first preset process gas at the first preset concentration ratio, the second preset process gas at the sixth preset concentration ratio, the third preset process gas at the third preset concentration ratio, the fourth preset process gas at the seventh preset concentration ratio, the fifth preset process gas at the fifth preset concentration ratio, the preset gas pressure range, the preset power range and the second preset temperature range; The graphite etching module is used to perform a second stage growth process on the single crystal diamond to be grown according to the second growth environment to obtain a target single crystal diamond, and to perform an etching process on the graphite on the quartz in the MPCVD device according to the second growth environment to obtain a graphite etching result.
6. A terminal, characterized in that: The terminal includes: a memory, a processor, and a graphite etching program without interrupting diamond growth stored in the memory and executable on the processor. When the graphite etching program without interrupting diamond growth is executed by the processor, the steps of the graphite etching method without interrupting diamond growth as described in any one of claims 1 to 4 are implemented.
7. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores a graphite etching program without interrupting diamond growth, and when the graphite etching program without interrupting diamond growth is executed by a processor, the steps of the graphite etching method without interrupting diamond growth as described in any one of claims 1-4 are implemented.
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