A diamond stripping method, system and terminal based on MPCVD equipment
By using a nucleation transition layer and preset process gas in the MPCVD equipment to promote diamond growth and perform peeling treatment in a specific cooling environment, the problem of poor diamond peeling effect in the prior art is solved, and efficient and environmentally friendly separation of diamond from the substrate is achieved.
Patent Information
- Application Number
- CN202411766235.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-04
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2044-12-04
AI Technical Summary
In the prior art, diamond peeling effect is poor when peeling from the substrate, physical peeling requires a large thickness, otherwise it will easily break, and the use of strong acids in chemical peeling leads to environmental pollution and high costs.
The base material is nucleation and generation processed by using the target spin coating liquid in the MPCVD device to form a nucleation transition layer, and the diamond growth is promoted through preset process gas to obtain a polycrystalline diamond film. The initial and re-stripping treatment is then performed in a specific cooling environment to achieve lossless separation of diamond and substrate.
The peeling efficiency between diamond and substrate is improved, the loss of diamond during the peeling process is reduced, and environmental pollution and high costs are avoided due to the use of strong acids.
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Figure CN119243330B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of diamond growth, and in particular to a diamond stripping method, system, terminal and computer-readable storage medium based on MPCVD equipment. 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 High temperature), hot filament chemical vapor deposition method (HFCVD, hot filament chemical vapor deposition), etc. Among them, the microwave plasma chemical vapor deposition method (MPCVD, Microwave plasma chemical vapor deposition) 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.
[0003] However, when using MPCVD equipment to grow large-scale polycrystalline diamond films, after the diamond growth is completed, the diamond needs to be peeled off from the substrate (i.e., the base that supports the diamond). Commonly used peeling methods in the prior art include physical peeling and chemical peeling, but physical peeling in the prior art requires the diamond film to grow to a sufficient thickness (generally above 0.3 mm), otherwise it is easy to break. Chemical peeling requires the use of strong acid, causing environmental pollution, and the process is complex and costly.
[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 diamond stripping method, system, terminal and computer-readable storage medium based on MPCVD equipment, aiming to solve the problem of poor stripping effect when stripping diamond from a substrate (i.e., a base that supports diamond) in the prior art.
[0006] To achieve the above object, the present invention provides a diamond stripping method based on an MPCVD device, and the diamond stripping method based on an MPCVD device comprises the following steps:
[0007] Obtaining a target spin-coating liquid, a target substrate material, and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer;
[0008] Determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film;
[0009] Setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film;
[0010] A second cooling environment is set, and the initially stripped polycrystalline diamond film is subjected to a re-stripping process according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0011] Optionally, the diamond stripping method based on MPCVD equipment, wherein the step of obtaining a target spin-coating liquid, a target substrate material and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer, specifically comprises:
[0012] Determining a target nano-diamond powder and a target chemical dispersant, and performing a configuration process on the target nano-diamond powder and the target chemical dispersant to obtain a target spin-coating liquid;
[0013] Determine a target substrate material and a target molybdenum sheet, and place the target substrate material on the target molybdenum sheet;
[0014] Placing the target spin coating liquid on the target substrate material for spin coating to obtain a spin coating liquid film;
[0015] Performing a static treatment and an evaporation treatment on the spin-coated liquid film to obtain a target spin-coated liquid film;
[0016] A preset generating gas is determined, and a nucleation generating process is performed on the target spin-coated liquid film on the target substrate material according to the preset generating gas to obtain a target nucleation transition layer.
[0017] Optionally, the diamond stripping method based on MPCVD equipment, wherein the step of determining a preset generation gas and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain a target nucleation transition layer, specifically includes:
[0018] Determining a preset generation gas of a preset ratio, and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain an initial nucleation transition layer, wherein the preset generation gas includes hydrogen, methane, nitrogen and argon;
[0019] The nucleation state of the initial nucleation transition layer is monitored by a preset optical monitoring method, and when the nucleation state of the initial nucleation transition layer meets the preset requirements, a target nucleation transition layer is obtained.
[0020] Optionally, the diamond stripping method based on MPCVD equipment, wherein the step of determining a preset process gas and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film, specifically includes:
[0021] Acquiring a center temperature and an edge temperature of a growth surface of the target nucleation transition layer, and controlling a temperature difference between the center temperature of the growth surface and the edge temperature to be within a preset temperature difference, wherein the center temperature of the growth surface is greater than the edge temperature;
[0022] Turning on the microwave in the MPCVD device and filling the MPCVD device with a preset process gas;
[0023] The target nucleation transition layer is subjected to diamond growth treatment according to the preset process gas to obtain a polycrystalline diamond film.
[0024] Optionally, the diamond stripping method based on the MPCVD device, wherein the setting of a first cooling environment and performing an initial stripping treatment on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film, specifically comprises:
[0025] Setting a first cooling environment in the MPCVD device, wherein the first cooling environment includes a preset hydrogen concentration range and a first preset temperature range;
[0026] The polycrystalline diamond film is initially stripped according to the preset hydrogen concentration range and the first preset temperature range to obtain an initially stripped polycrystalline diamond film.
[0027] Optionally, the diamond stripping method based on the MPCVD device, wherein the initial stripping treatment is performed on the polycrystalline diamond film according to the preset hydrogen concentration range and the first preset temperature range to obtain the initially stripped polycrystalline diamond film, specifically comprises:
[0028] The first preset temperature range is lowered at every preset period until the first preset temperature range is lowered to a second preset temperature range, thereby obtaining a plurality of change temperatures;
[0029] The polycrystalline diamond film is initially stripped according to the plurality of the change temperatures and the preset hydrogen concentration range to obtain an initially stripped polycrystalline diamond film.
[0030] Optionally, the diamond stripping method based on the MPCVD device, wherein the second cooling environment is set, and the initially stripped polycrystalline diamond film is subjected to a re-stripping treatment according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped, specifically comprises:
[0031] Turning off the microwave in the MPCVD device, and obtaining a second cooling environment after the MPCVD device turns off the microwave;
[0032] The initially stripped polycrystalline diamond film is subjected to a re-stripping process according to the second temperature reduction environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0033] In addition, to achieve the above-mentioned purpose, the present invention further provides a diamond stripping system based on an MPCVD device, wherein the diamond stripping system based on an MPCVD device comprises:
[0034] A nucleation transition layer generation module is used to obtain a target spin-coating liquid, a target substrate material and a target molybdenum sheet, place the target substrate material on the target molybdenum sheet, and perform a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer;
[0035] A diamond growth module, used for determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film;
[0036] an initial stripping processing module, used for setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film;
[0037] The re-stripping processing module is used to set a second cooling environment and perform a re-stripping process on the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0038] 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 diamond stripping program based on MPCVD equipment stored in the memory and executable on the processor, wherein the diamond stripping program based on MPCVD equipment implements the steps of the diamond stripping method based on MPCVD equipment as described above when executed by the processor.
[0039] 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 diamond stripping program based on MPCVD equipment, and when the diamond stripping program based on MPCVD equipment is executed by a processor, the steps of the diamond stripping method based on MPCVD equipment as described above are implemented.
[0040] In the present invention, a target spin coating liquid, a target substrate material and a target molybdenum sheet are obtained, the target substrate material is placed on the target molybdenum sheet, and the target substrate material is subjected to a nucleation generation process according to the target spin coating liquid to obtain a target nucleation transition layer; a preset process gas is determined, and a diamond growth process is performed on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film; a first cooling environment is set, and the polycrystalline diamond film is subjected to an initial stripping process according to the first cooling environment to obtain an initially stripped polycrystalline diamond film; a second cooling environment is set, and the initially stripped polycrystalline diamond film is subjected to a re-stripping process according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped. The present invention generates a target nucleation transition layer on the target substrate material by configuring a spin coating liquid, and regulates the bonding strength between the polycrystalline diamond and the substrate by the target nucleation transition layer. Further, a certain cooling rate is set to separate the polycrystalline diamond from the substrate, which not only effectively improves the stripping efficiency of the diamond and the substrate, but also reduces the loss of diamond during the stripping process. BRIEF DESCRIPTION OF THE DRAWINGS
[0041] Figure 1 It is a first flow chart of a preferred embodiment of the diamond stripping method based on MPCVD equipment of the present invention;
[0042] Figure 2 is a second flow chart of a preferred embodiment of the diamond stripping method based on MPCVD equipment of the present invention;
[0043] Figure 3 It is a schematic diagram of polycrystalline diamond after growth and stripping according to a preferred embodiment of the diamond stripping method based on MPCVD equipment of the present invention;
[0044] Figure 4 It is a structural diagram of a preferred embodiment of a diamond stripping system based on MPCVD equipment of the present invention;
[0045] Figure 5 It is a structural diagram of a preferred embodiment of the terminal of the present invention. DETAILED DESCRIPTION
[0046] 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.
[0047] 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 High temperature), hot filament chemical vapor deposition method (HFCVD, hot filament chemical vapor deposition), etc. Among them, the microwave plasma chemical vapor deposition method (MPCVD, Microwave plasma chemical vapor deposition) 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.
[0048] 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 growing large-grain diamonds; 2. No electrodes are required during the plasma generation process, and electrode impurities will not be introduced, making it easier to grow high-purity diamonds.
[0049] However, when using MPCVD equipment to grow large-scale polycrystalline diamond films, after the diamond growth is completed, the diamond needs to be peeled off from the substrate (i.e., the base that supports the diamond). Commonly used peeling methods in the prior art include physical peeling and chemical peeling, but physical peeling in the prior art requires the diamond film to grow to a sufficient thickness (generally above 0.3 mm), otherwise it is easy to break. Chemical peeling requires the use of strong acid, causing environmental pollution, and the process is complex and costly.
[0050] The diamond stripping method based on MPCVD equipment described in the preferred embodiment of the present invention is as follows: Figure 1 and Figure 2 As shown, the diamond stripping method based on MPCVD equipment includes the following steps:
[0051] Step S10, obtaining a target spin-coating liquid, a target substrate material and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer.
[0052] For diamond stripping, the commonly used stripping methods in the prior art include physical stripping and chemical stripping, but the stripping effects are not ideal, the process is complicated and the cost is high.
[0053] For heteroepitaxial nucleation of diamond on non-diamond substrates, the traditional means are scraping nucleation, spin coating nucleation, or in-situ bias nucleation of diamond nanocrystals. For scraping and bias nucleation methods, the polycrystalline diamond grown usually has a strong bonding force with the substrate, and it is usually necessary to use laser ring cutting and chemical etching methods on the adhesion part between the polycrystalline diamond and the substrate to complete the polycrystalline demolding (i.e., peeling the polycrystalline diamond off the substrate). It is difficult to use the difference in thermal expansion coefficients of the two materials (i.e., polycrystalline diamond and substrate) for in-situ stripping. At the same time, it is limited by the edge of the polycrystalline diamond and the substrate. The polycrystalline may be damaged during the demolding process. Although the bonding strength of the edge polycrystalline can be reduced as much as possible through the reasonable design of the molybdenum sheet, making the demolding easier, there is still a high probability that the polycrystalline will be greatly deformed during the demolding process.
[0054] The present invention aims to regulate the strength of the bonding force between diamond polycrystals and substrates, and through reasonable nucleation means and the growth of transition layers, after the growth of diamond polycrystals grown to a specific thickness, there is no need to take out the diamond polycrystals from the growth chamber for laser ring cutting or chemical etching to achieve polycrystal stripping. Instead, the in-situ polycrystals and the in-situ substrates are non-destructively stripped at a specific cooling rate, thereby reducing the cost of diamond growth and improving diamond stripping efficiency.
[0055] Specifically, a target nano-diamond powder and a target chemical dispersant are determined, and the target nano-diamond powder and the target chemical dispersant are configured to obtain a target spin-coating liquid; a target substrate material and a target molybdenum sheet are determined, and the target substrate material is placed on the target molybdenum sheet; the target spin-coating liquid is placed on the target substrate material for spin coating to obtain a spin-coating liquid film; the spin-coating liquid film is subjected to a static treatment and an evaporation treatment to obtain a target spin-coating liquid film; a preset generated gas of a preset proportion is determined, and a nucleation generation treatment is performed on the target spin-coating liquid film on the target substrate material according to the preset generated gas to obtain an initial nucleation transition layer, wherein the preset generated gas includes hydrogen, methane, nitrogen and argon; a preset optical monitoring method is used to monitor the nucleation state of the initial nucleation transition layer, and when the nucleation state of the initial nucleation transition layer meets the preset requirements, a target nucleation transition layer is obtained.
[0056] The spin coating liquid provided in the present invention (i.e., the target spin coating liquid in the present invention) is composed of: nano-diamond (i.e., the target nano-diamond powder in the present invention) and a dispersant (i.e., the target chemical dispersant in the present invention, which can be one of acetone, isopropanol, dimethyl sulfoxide, nonylphenol, and polyoxyethylene ether), wherein the size of the nano-diamond, the selection and ratio of the dispersant, the pH value, and the parameter control (rotation speed, temperature, etc.) during the spin coating process need to be preset.
[0057] like Figure 2 As shown, the present invention first configures nano-diamond powder and chemical dispersant to obtain a target spin-coating liquid, and then spin-coats, stands and evaporates the target spin-coating liquid on a target substrate material to generate a uniform matte film, which is then transferred to a target molybdenum sheet for growth to obtain a nucleation transition layer.
[0058] In an embodiment of the present invention, the spin coating nucleation method is to use a spin coating liquid prepared with nano diamond powder of a specific size (preferably 10-50 nanometers in the present invention) and a chemical dispersant, and use a spin coater to form a uniform spin coating liquid film of a specific thickness (i.e., the spin coating liquid film in the present invention) on a substrate material (i.e., the target substrate material in the present invention) of a preset size (which can be 2 inches / 3 inches / 4 inches / 6 inches / 8 inches) at a certain rotation speed (first use a low rotation speed of 200-500 r / s to evenly disperse the spin coating liquid on the substrate material, and then use a high rotation speed of 1800-2000 r / s to form a uniform spin coating liquid film with a thickness of approximately 50-150 nanometers), and let it stand under a certain environment (temperature 25°C / humidity 60-70%RH) to allow the dispersant in the spin coating liquid to fully evaporate, thereby forming a uniform matte film (i.e., the target spin coating liquid film in the present invention) on the surface of the substrate.
[0059] The configuration process of nano-diamond powder and chemical dispersant is as follows (taking NP-10 as an example of dispersant): 1. Use a clean beaker to measure a quantitative diamond suspension (suspension: dispersant NP-10=100:1.5); 2. Place a magnetic stirrer into the suspension, turn on the rotary switch, set the speed to medium speed (turn the knob to the middle), and rotate the rotor in the beaker; 3. Use a graduated dropper to absorb the corresponding proportion of dispersant NP-10, and slowly drip it into the suspension drop by drop, with a dripping speed of about one drop every 2 seconds; 4. After dripping, cover the mouth of the beaker with a clean plastic wrap and continue stirring for 3 hours; 5. After stirring, pour the suspension into a clean suspension bottle and let it stand for 24 hours.
[0060] like Figure 2As shown, the obtained uniform matte film (i.e., the target spin-coated liquid film in the present invention) is placed on a specially designed molybdenum sheet (i.e., the target molybdenum sheet in the present invention, located in the MPCVD device) through the target substrate material, and a certain proportion of hydrogen, methane, nitrogen and argon (i.e., the generated gas in the present invention, preferably 400-600 SccmH2, 20-40 SccmCH4, 5-20 SccmN2, Sccm is the volume flow unit) is introduced into the MPCVD device, and nucleation growth is carried out at a certain temperature (preferably 600-800°C), and the nucleation growth time is set. In this process, it is necessary to monitor the nucleation state of the nucleation transition layer by optical means (i.e., the preset optical monitoring method in the present invention, preferably the laser reflection interference method in the present invention) to determine the timing of switching the process (i.e., stopping the nucleation growth and entering the diamond growth process).
[0061] Among them, the process parameters of the nucleation transition layer include the ratio of hydrogen and methane and the ratio of nitrogen and argon addition. At the same time, a key parameter needs to be set as the timing of adding methane and nitrogen. Furthermore, by controlling the surface temperature and the thickness of the nucleation transition layer, the bonding force between the polycrystalline diamond film and the substrate can be effectively regulated, thus laying the foundation for in-situ film stripping in the later stage. At the same time, during the growth of the nucleation transition layer, it is necessary to combine effective optical means to carry out real-time in-situ film growth dynamics monitoring to determine the timing of process switching.
[0062] Step S20, determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film.
[0063] After obtaining the target nucleation transition layer, the present invention can place the target nucleation transition layer in an MPCVD device to grow diamond (preset process gas will be filled into the MPCVD device) to obtain a polycrystalline diamond film (the spin coating liquid in the target nucleation transition layer contains nano-diamond powder, so the preset process gas can promote the growth of nano-diamond powder in the target nucleation transition layer to obtain a polycrystalline diamond film).
[0064] Specifically, the center temperature and edge temperature of the growth surface of the target nucleation transition layer are obtained, and the temperature difference between the center temperature of the growth surface and the edge temperature is controlled to be within a preset temperature difference, wherein the center temperature of the growth surface is greater than the edge temperature; microwaves in the MPCVD device are turned on, and a preset process gas is filled into the MPCVD device; diamond growth treatment is performed on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film.
[0065] When the target nucleation transition layer is generated, the normal diamond growth process is switched to. At the same time, in order to compensate for the additional stress caused by the edge effect during the growth process, the temperature difference between the center and the edge of the growth surface (the central high-temperature constant temperature point and the edge annular low-temperature zone) is maintained at 40~70°C (i.e., the preset temperature difference in the present invention) through the combination of the heat dissipation molybdenum sheet below, thereby ensuring that the diamond polycrystals are prevented from breaking during the cooling and demolding process.
[0066] Among them, for the design of the molybdenum sheet used in the diamond growth process: in order to effectively compensate for the additional stress caused by the edge effect, an effective molybdenum tray heat dissipation design can be used to maintain a certain temperature difference between the temperature center and the edge of the polycrystalline growth surface during the growth process (the temperature difference is preferably set to 40~70°C, and the specific temperature difference depends on the thickness of the polycrystalline film to be grown). In addition, the special design of the molybdenum tray also needs to consider reducing or avoiding the growth of polycrystalline film on the side of the substrate, so as to reduce the additional bonding force generated during the automatic film stripping process and avoid polycrystalline fragmentation.
[0067] Step S30, setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film.
[0068] After the diamond growth is completed, the diamond needs to be cooled by setting a certain cooling rate, so that the growing polycrystalline film can be separated from the substrate within a specific temperature range, thereby achieving the initial separation of the polycrystalline film and the substrate.
[0069] Specifically, a first cooling environment is set in the MPCVD device, wherein the first cooling environment includes a preset hydrogen concentration range and a first preset temperature range; the first preset temperature range is lowered at preset intervals until the first preset temperature range is lowered to a second preset temperature range, thereby obtaining a plurality of variable temperatures; and the polycrystalline diamond film is initially stripped according to the plurality of variable temperatures and the preset hydrogen concentration range to obtain an initially stripped polycrystalline diamond film.
[0070] After the growth of the polycrystalline diamond film is completed, the present invention further controls the temperature change by controlling the methane content in the MPCVD equipment, thereby reducing the bonding strength between the polycrystalline film and the substrate, further reducing the difficulty of polycrystalline diamond film stripping, and achieving the initial separation of the polycrystalline film and the substrate in the polycrystalline diamond film.
[0071] In a specific embodiment of the present invention, after the growth of the polycrystalline diamond film is completed, the introduction of methane and oxygen is closed, and then pure hydrogen is introduced into the reaction chamber, and the pure hydrogen is used for slight etching at 500-800°C (i.e., the first preset temperature range in the present invention) for 5-25 minutes, and the temperature of the polycrystalline substrate is cooled to 200-300°C (i.e., the second preset temperature range in the present invention) at a cooling rate of 3-5°C / min (total cooling time of 2-6 hours). During this period, due to the change of residual methane gas in the reaction chamber, the temperature of the substrate will suddenly change, so that the polycrystalline film and the silicon substrate (i.e., the preset substrate material in the present invention, the preset substrate material used in the present invention can be one of silicon, molybdenum, quartz glass, and sapphire, and a silicon substrate is preferably used in the embodiment) are slightly separated.
[0072] The first cooling environment set in the present invention controls the temperature by controlling the amount of methane, and the thermal expansion coefficients of diamond and silicon substrate (i.e., the base in the present invention) are different. Therefore, the initial separation of diamond and silicon substrate can be achieved by controlling the temperature. At this time, the separation is only slightly peeled off and not thorough (the temperature in the first cooling environment drops slowly).
[0073] The present invention can control the polycrystalline diamond to achieve effective non-destructive automatic film stripping (i.e., separation of the polycrystalline film from the substrate in the polycrystalline diamond) in a specific temperature range at a certain cooling rate (the cooling rate depends on the thickness of the polycrystalline film) by setting the cooling process control parameters (cooling rate and air pressure inside the cavity, etc.) after the diamond growth is completed.
[0074] Step S40, setting a second cooling environment, and re-stripping the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0075] Specifically, the microwaves in the MPCVD device are turned off, and a second cooling environment is obtained after the microwaves in the MPCVD device are turned off; the initially stripped polycrystalline diamond film is re-stripped according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0076] After the initial stripping process is completed, the microwave is turned off to extinguish the plasma, which will further promote a large deformation of the silicon substrate (the silicon substrate may remain intact or broken), so that the polycrystalline film is completely separated from the silicon substrate (that is, the target polycrystalline diamond film and target substrate after the polycrystalline diamond stripping are obtained). During the cooling process of the polycrystalline diamond in the present invention, the polycrystalline film and the substrate will be naturally stripped due to the difference in stress between the two. The diamond crystal obtained after stripping is of high quality, with low material loss and is not limited by the material size.
[0077] like Figure 3 As shown, Figure 3 In order to grow the polycrystalline diamond after peeling (i.e., the target polycrystalline diamond film in the present invention), the second cooling environment set in the present invention is to turn off the microwave source of the MPCVD equipment. At this time, the separation of the diamond and the silicon substrate is complete (the temperature in the second cooling environment drops quickly, and the temperature difference between the diamond and the silicon substrate is large).
[0078] The present invention aims to adjust the strength of the bonding force between polycrystalline diamond and substrate by setting the growth of nucleation transition layer, so as to realize effective separation of polycrystalline diamond and substrate by utilizing the difference of thermal expansion coefficient between materials during the cooling process. Based on this idea, the schemes for deforming the nucleation transition layer are as follows: 1. By depositing a coating (specific metal or non-metallic material) on the substrate or performing graphic processing on the coating, the strength of nucleation and the effective area of nucleation are controlled, and the bonding force between the polycrystalline film grown above and the substrate or transition coating below is controlled by combining the two, so as to realize the regulation of interface bonding force; 2. By adopting other nucleation pretreatment means, because spin coating nucleation is to make nano-diamond particles bond to the surface of the substrate through weak chemical bonding by spin coating liquid, based on this cognition, nano-diamond particles can be bonded to the substrate by adopting similar methods such as electrospraying to achieve the same in-situ film stripping function.
[0079] Furthermore, if Figure 4 As shown, based on the above-mentioned diamond stripping method based on MPCVD equipment, the present invention also provides a diamond stripping system based on MPCVD equipment, wherein the diamond stripping system based on MPCVD equipment includes:
[0080] A nucleation transition layer generation module 51 is used to obtain a target spin coating liquid, a target substrate material and a target molybdenum sheet, place the target substrate material on the target molybdenum sheet, and perform a nucleation generation process on the target substrate material according to the target spin coating liquid to obtain a target nucleation transition layer;
[0081] The diamond growth module 52 is used to determine a preset process gas, and perform a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film;
[0082] An initial stripping processing module 53 is used to set a first cooling environment and perform an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film;
[0083] The re-stripping processing module 54 is used to set a second cooling environment and perform a re-stripping process on the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0084] Furthermore, if Figure 5 As shown, based on the above-mentioned diamond stripping method and system based on MPCVD equipment, the present invention also provides a terminal accordingly, and the terminal includes a processor 10, a memory 20 and a display 30. Figure 5 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.
[0085] 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 memory card (Smart Media Card, SMC), a secure digital (SecureDigital, SD) card, a flash card (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 on 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 diamond stripping program 40 based on an MPCVD device is stored on the memory 20, and the diamond stripping program 40 based on the MPCVD device can be executed by the processor 10, thereby realizing the diamond stripping method based on the MPCVD device in the present application.
[0086] 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 diamond stripping method based on the MPCVD device.
[0087] 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.
[0088] In one embodiment, when the processor 10 executes the diamond stripping program 40 based on the MPCVD device in the memory 20, the following steps are implemented:
[0089] Obtaining a target spin-coating liquid, a target substrate material, and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer;
[0090] Determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film;
[0091] Setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film;
[0092] A second cooling environment is set, and the initially stripped polycrystalline diamond film is subjected to a re-stripping process according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0093] The step of obtaining a target spin-coating liquid, a target substrate material, and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer specifically includes:
[0094] Determining a target nano-diamond powder and a target chemical dispersant, and performing a configuration process on the target nano-diamond powder and the target chemical dispersant to obtain a target spin-coating liquid;
[0095] Determine a target substrate material and a target molybdenum sheet, and place the target substrate material on the target molybdenum sheet;
[0096] Placing the target spin coating liquid on the target substrate material for spin coating to obtain a spin coating liquid film;
[0097] Performing a static treatment and an evaporation treatment on the spin-coated liquid film to obtain a target spin-coated liquid film;
[0098] A preset generating gas is determined, and a nucleation generating process is performed on the target spin-coated liquid film on the target substrate material according to the preset generating gas to obtain a target nucleation transition layer.
[0099] The step of determining a preset generation gas and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain a target nucleation transition layer specifically includes:
[0100] Determining a preset generation gas of a preset ratio, and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain an initial nucleation transition layer, wherein the preset generation gas includes hydrogen, methane, nitrogen and argon;
[0101] The nucleation state of the initial nucleation transition layer is monitored by a preset optical monitoring method, and when the nucleation state of the initial nucleation transition layer meets the preset requirements, a target nucleation transition layer is obtained.
[0102] The step of determining a preset process gas and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film specifically includes:
[0103] Acquiring a center temperature and an edge temperature of a growth surface of the target nucleation transition layer, and controlling a temperature difference between the center temperature of the growth surface and the edge temperature to be within a preset temperature difference, wherein the center temperature of the growth surface is greater than the edge temperature;
[0104] Turning on the microwave in the MPCVD device and filling the MPCVD device with a preset process gas;
[0105] The target nucleation transition layer is subjected to diamond growth treatment according to the preset process gas to obtain a polycrystalline diamond film.
[0106] The step of setting a first cooling environment and performing an initial stripping treatment on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film specifically includes:
[0107] Setting a first cooling environment in the MPCVD device, wherein the first cooling environment includes a preset hydrogen concentration range and a first preset temperature range;
[0108] The polycrystalline diamond film is initially stripped according to the preset hydrogen concentration range and the first preset temperature range to obtain an initially stripped polycrystalline diamond film.
[0109] The performing of an initial stripping treatment on the polycrystalline diamond film according to the preset hydrogen concentration range and the first preset temperature range to obtain an initially stripped polycrystalline diamond film specifically includes:
[0110] The first preset temperature range is lowered at every preset period until the first preset temperature range is lowered to a second preset temperature range, thereby obtaining a plurality of change temperatures;
[0111] The polycrystalline diamond film is initially stripped according to the plurality of the change temperatures and the preset hydrogen concentration range to obtain an initially stripped polycrystalline diamond film.
[0112] The setting of the second cooling environment and re-stripping the initially stripped polycrystalline diamond film according to the second cooling environment to obtain the target polycrystalline diamond film and the target substrate after the polycrystalline diamond film is stripped specifically includes:
[0113] Turning off the microwave in the MPCVD device, and obtaining a second cooling environment after the MPCVD device turns off the microwave;
[0114] The initially stripped polycrystalline diamond film is subjected to a re-stripping process according to the second temperature reduction environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
[0115] The present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a diamond stripping program based on an MPCVD device, and when the diamond stripping program based on an MPCVD device is executed by a processor, the steps of the diamond stripping method based on an MPCVD device as described above are implemented.
[0116] In summary, the present invention provides a diamond stripping method based on MPCVD equipment and related equipment, the method comprising: obtaining a target spin-coating liquid, a target substrate material and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer; determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film; setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film; setting a second cooling environment, and performing a re-stripping process on the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped. The present invention generates a target nucleation transition layer on a target substrate material by configuring a spin coating liquid, and regulates the strength of the bonding force between the polycrystalline diamond and the substrate through the target nucleation transition layer. Furthermore, the polycrystalline diamond and the substrate are separated by setting a certain cooling rate, which not only effectively improves the stripping efficiency of the diamond and the substrate, but also reduces the loss of the diamond during the stripping process.
[0117] 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.
[0118] 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.
[0119] 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 diamond stripping method based on MPCVD equipment, characterized in that: The diamond stripping method based on MPCVD equipment includes: Obtaining a target spin-coating liquid, a target substrate material, and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer; Determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film, specifically comprising: obtaining a growth surface center temperature and an edge temperature of the target nucleation transition layer, and controlling the temperature difference between the growth surface center temperature and the edge temperature to be within a preset temperature difference, wherein the growth surface center temperature is greater than the edge temperature; Turning on the microwave in the MPCVD device and filling the MPCVD device with a preset process gas; Performing diamond growth processing on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film; Through the effective molybdenum tray heat dissipation design, a certain temperature difference is maintained between the temperature center and the edge of the polycrystalline growth surface during the growth process; The molybdenum support considers reducing or avoiding the growth of polycrystalline film on the side of the substrate, reducing the extra bonding force generated during the automatic film stripping process, and avoiding the fragmentation of polycrystalline; Setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film, specifically comprising: setting a first cooling environment in the MPCVD device, wherein the first cooling environment includes a preset hydrogen concentration range and a first preset temperature range; Performing an initial stripping process on the polycrystalline diamond film according to the preset hydrogen concentration range and the first preset temperature range to obtain an initially stripped polycrystalline diamond film, specifically comprising: reducing the first preset temperature range at each preset period until the first preset temperature range is reduced to a second preset temperature range to obtain a plurality of variable temperatures; performing an initial stripping process on the polycrystalline diamond film according to the plurality of variable temperatures and the preset hydrogen concentration range to obtain an initially stripped polycrystalline diamond film; The first cooling environment is set to control the temperature by controlling the amount of methane, and the initial separation of diamond and substrate is achieved by controlling the temperature; Setting a second cooling environment, and re-stripping the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped, specifically comprising: Turning off the microwaves in the MPCVD device and obtaining a second cooling environment after the MPCVD device turns off the microwaves; performing a re-stripping process on the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped; When the initial stripping process is completed, the microwave is turned off to extinguish the plasma, promoting the deformation of the silicon substrate, so that the polycrystalline film is completely separated from the silicon substrate.
2. The diamond stripping method based on MPCVD equipment according to claim 1, characterized in that: The step of obtaining a target spin coating liquid, a target substrate material, and a target molybdenum sheet, placing the target substrate material on the target molybdenum sheet, and performing a nucleation generation process on the target substrate material according to the target spin coating liquid to obtain a target nucleation transition layer specifically includes: Determining a target nano-diamond powder and a target chemical dispersant, and performing a configuration process on the target nano-diamond powder and the target chemical dispersant to obtain a target spin-coating liquid; Determine a target substrate material and a target molybdenum sheet, and place the target substrate material on the target molybdenum sheet; Placing the target spin coating liquid on the target substrate material for spin coating to obtain a spin coating liquid film; Performing a static treatment and an evaporation treatment on the spin-coated liquid film to obtain a target spin-coated liquid film; A preset generating gas is determined, and a nucleation generating process is performed on the target spin-coated liquid film on the target substrate material according to the preset generating gas to obtain a target nucleation transition layer.
3. The diamond stripping method based on MPCVD equipment according to claim 2, characterized in that: The step of determining a preset generation gas and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain a target nucleation transition layer specifically includes: Determining a preset generation gas of a preset ratio, and performing a nucleation generation process on the target spin-coated liquid film on the target substrate material according to the preset generation gas to obtain an initial nucleation transition layer, wherein the preset generation gas includes hydrogen, methane, nitrogen and argon; The nucleation state of the initial nucleation transition layer is monitored by a preset optical monitoring method, and when the nucleation state of the initial nucleation transition layer meets the preset requirements, a target nucleation transition layer is obtained.
4. A diamond stripping system based on an MPCVD device based on the diamond stripping method based on an MPCVD device according to any one of claims 1 to 3, characterized in that: The diamond stripping system based on MPCVD equipment includes: A nucleation transition layer generation module is used to obtain a target spin-coating liquid, a target substrate material and a target molybdenum sheet, place the target substrate material on the target molybdenum sheet, and perform a nucleation generation process on the target substrate material according to the target spin-coating liquid to obtain a target nucleation transition layer; A diamond growth module, used for determining a preset process gas, and performing a diamond growth process on the target nucleation transition layer according to the preset process gas to obtain a polycrystalline diamond film; an initial stripping processing module, used for setting a first cooling environment, and performing an initial stripping process on the polycrystalline diamond film according to the first cooling environment to obtain an initially stripped polycrystalline diamond film; The re-stripping processing module is used to set a second cooling environment and perform a re-stripping process on the initially stripped polycrystalline diamond film according to the second cooling environment to obtain a target polycrystalline diamond film and a target substrate after the polycrystalline diamond film is stripped.
5. A terminal, characterized in that: The terminal includes: a memory, a processor, and a diamond stripping program based on an MPCVD device stored in the memory and executable on the processor. When the diamond stripping program based on the MPCVD device is executed by the processor, the steps of the diamond stripping method based on the MPCVD device as described in any one of claims 1 to 3 are implemented.
6. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores a diamond stripping program based on an MPCVD device, and when the diamond stripping program based on an MPCVD device is executed by a processor, the steps of the diamond stripping method based on an MPCVD device as described in any one of claims 1 to 3 are implemented.
Citation Information
Patent Citations
Close-packed nano-diamond film and preparation method thereof
CN115852331A
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CN117328032A
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