A polycrystalline diamond film generation method, system, terminal and storage medium
By optimizing the cavity cleaning, nucleation formula, and growth formula of the MPCVD equipment, the problems of low growth rate and large warpage of polycrystalline diamond films were solved, and efficient and stable polycrystalline diamond film generation was achieved.
Patent Information
- Application Number
- CN202511770963.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-28
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2045-11-28
AI Technical Summary
In the existing technology, the growth rate of high-quality, high-thermal-conductivity polycrystalline diamond films is relatively low, which cannot meet production requirements. Furthermore, the unevenness of the growth thickness leads to large film warpage, affecting stability.
By optimizing the cavity cleaning and start-up treatment of MPCVD equipment, setting target nucleation and growth formulations, including improvements to the heat dissipation device and adjustment of the gas concentration gradient, the growth environment and temperature differences of diamond films are controlled, thereby improving growth efficiency and quality stability.
It significantly improved the growth rate and quality of polycrystalline diamond films, reduced warpage, and enhanced the thermal conductivity and stability of the films.
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Figure CN121228197B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of diamond cultivation, in particular to a polycrystalline diamond film generation method, system, terminal and computer readable storage medium. BACKGROUND
[0002] Diamond has extremely excellent physical and chemical properties, but the reserves of natural diamond are limited, so people have developed various methods for synthesizing diamond, such as high pressure high temperature (HPHT), hot filament chemical vapor deposition (HFCVD), etc. Among them, the microwave plasma chemical vapor deposition (MPCVD) method for synthesizing diamond can synthesize high-quality and large-area diamond without the introduction of impurities, 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 diamond.
[0003] In the prior art, the MPCVD device is generally used to dissociate mixed gases such as methane and hydrogen under a predetermined high temperature condition to deposit high-quality polycrystalline diamond film on a substrate, but the growth rate of high-quality high-thermal-conductivity polycrystalline diamond film is low at present, which cannot meet the production needs of users for polycrystalline diamond film.
[0004] Therefore, the prior art still needs to be improved and developed. SUMMARY
[0005] The main purpose of the present application is to provide a polycrystalline diamond film generation method, system, terminal and computer readable storage medium, which aims to solve the problem of low growth rate of high-quality high-thermal-conductivity polycrystalline diamond film in the prior art.
[0006] To achieve the above-mentioned purpose, the present application provides a polycrystalline diamond film generation method, which comprises the following steps:
[0007] Determine a target MPCVD device, and perform cavity cleaning treatment and ignition treatment on the reaction cavity in the target MPCVD device to obtain a target reaction cavity;
[0008] Determine a target nucleation formula, and perform nucleation growth treatment on the target diamond placed in the target reaction cavity according to the target nucleation formula to obtain an initial diamond;
[0009] determining a target growth formula, and growing and cultivating the initial diamond according to the target growth formula to obtain a target polycrystalline diamond film.
[0010] Optionally, the polycrystalline diamond film generation method, wherein the cavity cleaning process comprises a vacuum pumping process and a gas replacement process.
[0011] The method further comprises determining a target MPCVD device, and performing a cavity cleaning process and a glow start process on a reaction cavity in the target MPCVD device to obtain a target reaction cavity, wherein the cavity cleaning process comprises:
[0012] determining a target MPCVD device, and performing a vacuum pumping process on a reaction cavity in the target MPCVD device by using a vacuum pump to obtain a vacuum-pumped reaction cavity;
[0013] filling the vacuum-pumped reaction cavity with hydrogen gas of a first preset concentration range, and performing a gas replacement process on the vacuum-pumped reaction cavity by using the hydrogen gas to obtain a replaced reaction cavity;
[0014] iterating the vacuum pumping process and the gas replacement process on the replaced reaction cavity, and when the iteration number reaches a preset iteration number, the cavity cleaning process is completed to obtain a cleaned cavity;
[0015] turning on a microwave, and obtaining microwave energy in the cleaned cavity, performing a breakdown process on the hydrogen gas in the cleaned cavity by using the microwave energy to obtain a plasma ball, and the glow start process is completed to obtain the target reaction cavity.
[0016] Optionally, the polycrystalline diamond film generation method, wherein the method further comprises determining a target nucleation formula, and performing a nucleation growth process on a target diamond placed in the target reaction cavity according to the target nucleation formula to obtain an initial diamond.
[0017] determining a preset heat dissipation device in the target MPCVD device, and setting a temperature difference for the preset heat dissipation device to obtain a target heat dissipation device.
[0018] Optionally, the polycrystalline diamond film generation method, wherein the preset heat dissipation device comprises a silicon wafer, a molybdenum wafer, a molybdenum heat dissipation wafer, a substrate table, and a molybdenum cone table.
[0019] The silicon wafer is located at the top of the preset heat dissipation device and is used to carry the target diamond.
[0020] The molybdenum wafer is located below the silicon wafer and adjacent to the silicon wafer.
[0021] The molybdenum heat dissipation wafer is located below the molybdenum wafer and adjacent to the molybdenum wafer.
[0022] The substrate table is located at the lowermost part of the preset heat dissipation device and is adjacent to the molybdenum heat dissipation sheet.
[0023] The molybdenum cone table is connected to the silicon sheet and the substrate table, respectively.
[0024] Optionally, the polycrystalline diamond thin film generation method, wherein the temperature difference setting of the preset heat dissipation device to obtain a target heat dissipation device specifically includes:
[0025] A heat dissipation ring is arranged at the position where the molybdenum cone table contacts the substrate table, so that the edge temperature of the target diamond on the silicon sheet is increased to a first preset value;
[0026] The silicon sheet and the molybdenum sheet are suspended, so that the edge temperature of the target diamond on the silicon sheet is increased from the first preset value to a second preset value;
[0027] The center temperature of the target diamond on the silicon sheet is obtained, and a temperature difference between the second preset value and the center temperature is calculated;
[0028] When the temperature difference reaches a preset temperature difference, the temperature difference setting is completed, and a target heat dissipation device is obtained.
[0029] Optionally, the polycrystalline diamond thin film generation method, wherein the target nucleation formula is determined, and the target diamond placed in the target reaction cavity is subjected to nucleation growth treatment according to the target nucleation formula to obtain an initial diamond, specifically including:
[0030] The target nucleation formula is determined, and the target nucleation formula is filled into the target reaction cavity, wherein the nucleation formula includes hydrogen gas with a second preset concentration range, methane with a third preset concentration range, and nitrogen gas with a fourth preset concentration range;
[0031] The target reaction cavity is subjected to temperature rising treatment through the target nucleation formula, when the temperature rising time reaches a preset time, and the temperature in the cavity of the target reaction cavity is increased to a preset temperature, the initial growth treatment of the target diamond is performed through the preset temperature and the target nucleation formula to obtain an initial diamond.
[0032] Optionally, the polycrystalline diamond thin film generation method, wherein the target growth formula includes a first growth formula and a second growth formula;
[0033] The target growth formula is determined, and the initial diamond is subjected to growth cultivation treatment according to the target growth formula to obtain a target polycrystalline diamond thin film, specifically including:
[0034] An initial growth formula is determined, and the initial growth formula is adjusted according to a preset gradient value to obtain the first growth formula and the second growth formula;
[0035] The first growth formula consists of methane in a fifth preset concentration range, oxygen in a sixth preset concentration range, and nitrogen in a seventh preset concentration range.
[0036] The second growth formula consists of methane in the eighth preset concentration range, oxygen in the ninth preset concentration range, and nitrogen in the tenth preset concentration range.
[0037] A first growth time is determined, and within the first growth time range, the first growth formula is added to the target reaction chamber. The initial diamond is subjected to a first growth cultivation treatment using the first growth formula to obtain an initial polycrystalline diamond film.
[0038] A second growth time is determined. When the growth time of the initial polycrystalline diamond film reaches the second growth time, the initial polycrystalline diamond film is subjected to a second growth cultivation treatment using the second growth formula to obtain the target polycrystalline diamond film.
[0039] Furthermore, to achieve the above objectives, the present invention also provides a polycrystalline diamond thin film formation system, wherein the polycrystalline diamond thin film formation system comprises:
[0040] The cavity environment setting module is used to determine the target MPCVD equipment and perform cavity cleaning and ignition treatment on the reaction cavity in the target MPCVD equipment to obtain the target reaction cavity;
[0041] The nucleation growth processing module is used to determine the target nucleation formula and perform nucleation growth processing on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond;
[0042] The growth and cultivation module is used to determine the target growth formula and to grow and cultivate the initial diamond according to the target growth formula to obtain the target polycrystalline diamond film.
[0043] In addition, to achieve the above objectives, the present invention also provides a terminal, wherein the terminal includes: a memory, a processor, and a polycrystalline diamond thin film generation program stored in the memory and executable on the processor, wherein when the polycrystalline diamond thin film generation program is executed by the processor, it implements the steps of the polycrystalline diamond thin film generation method as described above.
[0044] In addition, to achieve the above objectives, the present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a polycrystalline diamond thin film generation program, which, when executed by a processor, implements the steps of the polycrystalline diamond thin film generation method as described above.
[0045] In this invention, a target MPCVD device is identified, and the reaction chamber within the target MPCVD device undergoes chamber cleaning and scintillation treatment to obtain a target reaction chamber. A target nucleation formula is determined, and a target diamond placed in the target reaction chamber is nucleated and grown according to the target nucleation formula to obtain an initial diamond. A target growth formula is determined, and the initial diamond is grown and cultivated according to the target growth formula to obtain a target polycrystalline diamond film. This invention effectively improves the growth efficiency and quality stability of polycrystalline diamond films by constructing a favorable environment for diamond growth through chamber cleaning and scintillation treatment of the MPCVD device's reaction chamber, setting a target nucleation formula for nucleation and growth of the target diamond, and simultaneously setting a target growth formula for growth and cultivation of the initial diamond. Attached Figure Description
[0046] Figure 1 This is a flowchart of a preferred embodiment of the polycrystalline diamond thin film generation method of the present invention;
[0047] Figure 2 This is a schematic diagram of the overall implementation process of a preferred embodiment of the polycrystalline diamond thin film generation method of the present invention;
[0048] Figure 3 This is a structural diagram of a preferred embodiment of the polycrystalline diamond thin film formation system of the present invention;
[0049] Figure 4 This is a structural diagram of a preferred embodiment of the terminal of the present invention. Detailed Implementation
[0050] To make the objectives, technical solutions, and advantages of this invention clearer and more explicit, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
[0051] Diamond possesses exceptional physicochemical properties, but natural diamond reserves are limited. Therefore, various methods for synthesizing diamond have been developed, such as high-pressure high-temperature (HPHT) and hot-filament chemical vapor deposition (HFCVD). Among these, microwave plasma chemical vapor deposition (MPCVD) is considered the optimal method for producing high-quality, large-area diamonds because it avoids the introduction of impurities. It offers advantages such as no electrode discharge contamination, fast deposition rates, and good stability.
[0052] Diamond has a thermal conductivity of 1300-2200 W / (m·K), which is 3-5 times that of copper and 13 times that of silicon. Currently, the mainstream method for preparing diamond is chemical vapor deposition (CVD), especially microwave plasma CVD (MPCVD), which can deposit high-quality polycrystalline diamond films on substrates at temperatures of 900-950℃ by dissociating a mixture of gases such as methane and hydrogen.
[0053] High-quality polycrystalline diamond films obtained by controlling the gas ratio and temperature difference during deposition can typically achieve a thermal conductivity of over 1800 W / (m·K).
[0054] The existing technology has the following disadvantages:
[0055] 1. The growth rate of high-quality, high-thermal-conductivity polycrystalline diamond films is relatively low, only 2-3 μm / h.
[0056] 2. The deposition time required to grow films with a thickness of 500μm or more is relatively long, and the stability of the equipment is required to be high.
[0057] 3. The warpage of the grown film is highly sensitive to temperature control. Excessive temperature difference can easily cause stress release and cracking of the film during the cooling phase.
[0058] To address the above problems, this invention provides a method for generating polycrystalline diamond thin films, mainly comprising:
[0059] 1. Optimize gas ratio to improve growth quality stability: By adjusting the carbon source and other auxiliary gases, the growth efficiency can be improved while maintaining the original deposition quality.
[0060] 2. Optimize heat dissipation configuration and control the temperature difference between the edge and the center: Currently, diamond growth rates are lower at the edges than at the center, and the uneven thickness of the polycrystalline growth region leads to increased polycrystalline warpage. This invention controls the growth temperature difference between the central and edge regions of the diamond, enabling the growth rates of each region to become more consistent. In other words, by reducing the unevenness of diamond thickness, the polycrystalline warpage is reduced.
[0061] The preferred embodiment of the polycrystalline diamond thin film generation method of the present invention, such as... Figure 1 and Figure 2 As shown, the method for generating polycrystalline diamond thin films includes the following steps:
[0062] Step S10: Determine the target MPCVD equipment, and perform chamber cleaning and ignition treatment on the reaction chamber of the target MPCVD equipment to obtain the target reaction chamber. The chamber cleaning treatment includes vacuuming and gas replacement.
[0063] Both vacuuming and gas replacement processes are designed to ensure a pure growth environment for diamonds. Vacuuming is used to control the gas pressure inside the MPCVD equipment, while gas replacement involves filling the MPCVD equipment with hydrogen gas to remove impurity gases and ensure normal diamond growth.
[0064] Specifically, a target MPCVD device is identified, and the reaction chamber in the target MPCVD device is evacuated using a vacuum pump to obtain a evacuated reaction chamber. Hydrogen gas of a first preset concentration range is introduced into the evacuated reaction chamber, and the hydrogen gas is used to perform gas replacement treatment on the evacuated reaction chamber to obtain a replaced reaction chamber. The evacuation treatment and gas replacement treatment are iteratively performed on the replaced reaction chamber. When the number of iterations reaches a preset number of iterations, the chamber cleaning treatment is completed, and a cleaned chamber is obtained.
[0065] The microwave is turned on, and the microwave energy in the cleaned cavity is obtained. The hydrogen gas in the cleaned cavity is broken down by the microwave energy to obtain a plasma ball. The ignition process is completed, and the target reaction cavity is obtained.
[0066] The specific process of cavity cleaning and ignition treatment is as follows: First, start the target MPCVD equipment and perform the microwave power supply preheating program. At the same time, start the equipment vacuuming program and start the vacuum pump. The vacuum pump reduces the internal environment of the target MPCVD equipment from atmospheric pressure to 5-25 mTorr. After the vacuuming is completed, 5-20 Torr (i.e., the first preset concentration range in this invention) of hydrogen gas is introduced to perform gas replacement and plasma ball ignition program.
[0067] The specific process of gas replacement is as follows:
[0068] Hydrogen gas is introduced into the target MPCVD equipment to raise the gas pressure inside the chamber to 5-20 mTorr. Then, vacuuming is started to reduce the chamber pressure to 5-25 mTorr. This process is repeated 2-4 times (i.e., the preset number of iterations in this invention), which significantly improves the purity of the gas inside the chamber.
[0069] like Figure 2 As shown, the specific process of plasma sphere ignition is as follows:
[0070] 1. Vacuuming and Reaction Gas Preparation: The chamber environment of the target MPCVD equipment is evacuated to a vacuum, and a precisely proportioned reaction gas (such as hydrogen or methane) is introduced to create a pure and controllable environment for plasma excitation. Purpose: To ensure chamber sealing and prevent contamination by impurity gases.
[0071] 2. Microwave Energy Coupling and Gas Ionization: Microwave energy is transmitted into the cavity through a waveguide, accelerating electrons in the hydrogen atmosphere and causing them to collide with molecules, ionizing them into charged particles. The goal of this stage is to achieve initial breakdown of the gas. Purpose: To achieve efficient transmission and impedance matching of microwave power, and to avoid energy reflection damaging the microwave source.
[0072] 3. Plasma Formation and Stabilization: Initially ionized charged particles multiply avalanche-like, forming a high-density, stable plasma sphere (often a bright glow sphere). The goal at this stage is to maintain a stable and uniform plasma discharge. Purpose: To overcome plasma instabilities, such as scintillation, contraction, or erosion of the cavity walls, and to ensure that it is positioned optimally above the substrate.
[0073] Step S20: Determine the target nucleation formula, and perform nucleation growth treatment on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond.
[0074] Nucleation refers to the deposition of seed diamond crystals into a thin film.
[0075] In the nucleation growth process, a heat dissipation device is also required in this invention to control the temperature of the silicon wafer and the diamond on it. Generally, the temperature of the silicon wafer and the diamond on it is higher at the center than at the edge, which can cause excessive warping in the edge area and lead to cracks. Therefore, this invention improves the preset heat dissipation device to obtain a target heat dissipation device that can control the temperature of the center area and the edge area of the silicon wafer and the diamond on it within a preset range, thereby reducing the warping in the edge area and ensuring the normal growth of the polycrystalline diamond film.
[0076] Specifically, further, a preset heat dissipation device in the target MPCVD equipment is determined, and a temperature difference is set for the preset heat dissipation device to obtain the target heat dissipation device. The preset heat dissipation device includes a silicon wafer, a molybdenum wafer, a molybdenum heat sink, a substrate stage, and a molybdenum cone. The silicon wafer is located at the top of the preset heat dissipation device and is used to support the target diamond. The molybdenum wafer is located below the silicon wafer and is adjacent to it. The molybdenum heat sink is located below the molybdenum wafer and is adjacent to it. The substrate stage is located at the bottom of the preset heat dissipation device and is adjacent to the molybdenum heat sink. The molybdenum cone is connected to both the silicon wafer and the substrate stage.
[0077] A heat dissipation ring is provided at the contact position between the molybdenum cone and the substrate stage to raise the edge temperature of the target diamond on the silicon wafer to a first preset value; the silicon wafer and the molybdenum wafer are suspended in the air to raise the edge temperature of the target diamond on the silicon wafer from the first preset value to a second preset value; the center temperature of the target diamond on the silicon wafer is obtained, and the temperature difference between the second preset value and the center temperature is calculated; when the temperature difference reaches the preset temperature difference, the temperature difference setting is completed, and the target heat dissipation device is obtained.
[0078] Due to the influence of the plasma sphere shape (the distance from each point on the high-temperature plasma sphere to the silicon wafer surface is different, with the distance at the center being less than that at the edge, resulting in a temperature difference on the silicon wafer, i.e., the temperature at the center of the silicon wafer is higher than that at the edge), the temperature at the edge of the silicon wafer is naturally lower than that at the center. Furthermore, because the molybdenum cone is in contact with the silicon wafer, and the molybdenum wafer is in contact with the silicon wafer, the heat dissipation of the silicon wafer will be carried out through the direction of the molybdenum cone and the molybdenum wafer, resulting in the heat dissipation efficiency at the edge of the molybdenum wafer being higher than that at the center. Under the influence of the two layers, the diamond layer on the surface of the silicon wafer will also show a much lower growth rate at the edge than at the center due to the two influences, resulting in a decrease in the quality of diamond growth on the silicon wafer and a large warpage.
[0079] The optimization process of the heat dissipation configuration in this invention is as follows: 1. By adding different types of heat dissipation components (the number of molybdenum heat sinks can be 1 or 2-3, depending on the test data after the MPCVD equipment is turned on); 2. Introducing a heat dissipation ring configuration into the molybdenum cone to reduce the heat dissipation efficiency of the molybdenum cone (i.e., reducing contact with the substrate stage to reduce heat dissipation efficiency); 3. Introducing a suspended design (mainly suspending the molybdenum sheet and silicon wafer in the heat dissipation device), which increases the temperature at the edge of the top silicon wafer and reduces the temperature difference with the center. The temperature difference of the diamond on the silicon wafer during the growth process is reduced (the temperature difference is reduced to below 15°C, i.e., the preset temperature difference in this invention), so that the growth temperature of the diamond in different areas tends to be consistent, and the growth rate also tends to be consistent, thereby achieving the effect of reducing warpage and improving growth quality.
[0080] In this invention, heat dissipation is optimized by configuring a heat dissipation ring in the molybdenum cone, thereby increasing the temperature of the molybdenum cone and reducing the efficiency of heat conduction from the edge of the silicon wafer to the molybdenum cone.
[0081] The invention also incorporates a suspended design, which not only reduces the heat dissipation efficiency of the silicon wafer edge but also further increases the edge temperature, leveling the temperature difference between the edge and the center.
[0082] Further, a target nucleation formulation is determined and filled into the target reaction chamber. The nucleation formulation includes hydrogen in a second preset concentration range, methane in a third preset concentration range, and nitrogen in a fourth preset concentration range. The target reaction chamber is heated using the target nucleation formulation. When the heating time reaches a preset time and the internal temperature of the target reaction chamber rises to a preset temperature, the target diamond is subjected to initial growth treatment using the preset temperature and the target nucleation formulation to obtain an initial diamond.
[0083] like Figure 2 As shown, during the heating stage, the nucleation formulation (target nucleation formulation) is introduced, namely, a certain proportion of hydrogen, methane, nitrogen, and argon (wherein, preferably, hydrogen is set to 200-800 Sccm (i.e., the second preset concentration range in this invention), methane is set to 5-35 Sccm (i.e., the third preset concentration range in this invention), and nitrogen is set to 1-30 Sccm (i.e., the fourth preset concentration range in this invention, Sccm is a unit of volumetric flow rate), the heating time is set to 5-120 min (i.e., the preset time in this invention), and the target heating temperature is 600-750℃ (i.e., the preset temperature in this invention). This reduces the etching effect of the pure hydrogen environment in the original heating process on the spin-coated seed crystal surface to the weakest point, and increases the speed and density of diamond nucleation.
[0084] In gas optimization formulation, MPCVD deposition of polycrystalline diamond films typically involves seeding diamond crystals on a substrate, nucleating them at a low temperature of 600-750℃, and then cultivating them at 800-1000℃. Before nucleation, since the seed crystals are usually nanometer-sized, the traditional approach is to extend the heating time (to 120-180 min) before reaching the appropriate temperature. However, the short heating time and the excessively rapid heating rate lead to uneven temperatures between the seed crystals, further causing some areas of the seed crystals to be too hot and resulting in ablation, ultimately leading to diamond nucleation failure. The nucleation formulation of this invention introduces growth from the heating process, combining the heating process with nucleation, which can effectively reduce the impact of hydrogen ablation on the silicon wafer surface.
[0085] Step S30: Determine the target growth formula, and grow the initial diamond according to the target growth formula to obtain a target polycrystalline diamond film. The target growth formula includes a first growth formula and a second growth formula.
[0086] After the nucleation process is completed, diamond growth and cultivation can be carried out. In order to improve the growth efficiency, the growth formula has been improved in this invention and a gradient configuration has been set. That is, different growth formulas are set at different growth time periods, which can effectively improve the growth efficiency of diamond.
[0087] Specifically, an initial growth formula is determined and adjusted according to a preset gradient value to obtain a first growth formula and a second growth formula; wherein, the first growth formula is methane within a fifth preset concentration range, oxygen within a sixth preset concentration range, and nitrogen within a seventh preset concentration range; the second growth formula is methane within an eighth preset concentration range, oxygen within a ninth preset concentration range, and nitrogen within a tenth preset concentration range; a first growth time is determined, and within the first growth time range, the first growth formula is added to the target reaction chamber, and the initial diamond is subjected to a first growth cultivation treatment using the first growth formula to obtain an initial polycrystalline diamond film; a second growth time is determined, and when the growth time of the initial polycrystalline diamond film reaches the second growth time, the initial polycrystalline diamond film is subjected to a second growth cultivation treatment using the second growth formula to obtain a target polycrystalline diamond film.
[0088] like Figure 3 As shown, the present invention improves the diamond growth formula: In order to solve the problem of slow diamond film growth rate and long growth time during the growth process, the present invention introduces gradient adjustment in the growth formula. The specific adjustment process is as follows: the methane concentration is adjusted to 20-60 Sccm (i.e., the fifth preset concentration range in the present invention), the oxygen concentration is adjusted to 0.5-10 Sccm (i.e., the sixth preset concentration range in the present invention), and the nitrogen concentration is adjusted to 0.5-20 Sccm (i.e., the seventh preset concentration range in the present invention).
[0089] It is understood that this invention sets up a gradient adjustment of the gas ratio to improve crystal quality, and changes the growth environment at different time periods. The specific implementation steps are as follows:
[0090] 1. The growth time is 0-100h (i.e., the first growth time in this invention): methane (methane concentration adjusted to 20-60 Sccm, i.e. the fifth preset concentration range in this invention), oxygen (oxygen concentration adjusted to 0.5-10 Sccm, i.e. the sixth preset concentration range in this invention), and nitrogen (nitrogen concentration adjusted to 0.5-20 Sccm, i.e. the seventh preset concentration range in this invention) are introduced.
[0091] 2. The growth time is 100-200h (i.e., the second growth time in this invention): the methane concentration is adjusted to 5-40 Sccm (i.e., the eighth preset concentration range in this invention), and the oxygen and nitrogen concentrations are adjusted to 0-15 Sccm (i.e., the ninth preset concentration range in this invention, wherein the ninth preset concentration range and the tenth preset concentration range are equal).
[0092] Possible design changes or modifications to this invention:
[0093] 1. The size of the silicon wafer can be reduced so that the molybdenum cone does not come into contact with the silicon wafer, thus reducing the impact of the molybdenum cone on the silicon wafer;
[0094] 2. By setting a protruding molybdenum cone on the silicon wafer, the plasma sphere edge effect is directly applied to the edge of the silicon wafer, thereby increasing the edge temperature of the silicon wafer;
[0095] 3. The substrate stage is designed to allow direct heating in different areas, resulting in different heat transfer efficiencies at different contact surfaces.
[0096] Furthermore, such as Figure 4 As shown, based on the above-described method for generating polycrystalline diamond films, the present invention also provides a polycrystalline diamond film generation system, wherein the polycrystalline diamond film generation system comprises:
[0097] The cavity environment setting module 51 is used to determine the target MPCVD equipment and perform cavity cleaning and ignition treatment on the reaction cavity in the target MPCVD equipment to obtain the target reaction cavity;
[0098] The nucleation growth processing module 52 is used to determine the target nucleation formula and perform nucleation growth processing on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond.
[0099] The growth and cultivation processing module 53 is used to determine the target growth formula and to grow and cultivate the initial diamond according to the target growth formula to obtain the target polycrystalline diamond film.
[0100] Furthermore, such as Figure 4As shown, based on the above-described method and system for generating polycrystalline diamond thin films, the present invention also provides a terminal, which includes a processor 10, a memory 20, and a display 30. Figure 4 Only some of the terminal components are shown; however, 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.
[0101] In some embodiments, the memory 20 may be an internal storage unit of the terminal, such as a hard disk or memory. In other embodiments, the memory 20 may be an external storage device of the terminal, such as a plug-in hard disk, smart media card (SMC), secure digital card (SD), flash card, etc. Further, the memory 20 may include both internal and external storage devices. The memory 20 is used to store application software and various types of data installed on the terminal, such as the program code installed on the terminal. The memory 20 can also be used to temporarily store data that has been output or will be output. In one embodiment, the memory 20 stores a polycrystalline diamond thin film generation program 40, which can be executed by the processor 10 to implement the polycrystalline diamond thin film generation method of this application.
[0102] In some embodiments, the processor 10 may be a central processing unit (CPU), a microprocessor, or other data processing chip, used to run program code stored in the memory 20 or process data, such as executing the polycrystalline diamond thin film generation method.
[0103] In some embodiments, the display 30 may be an LED display, a liquid crystal display, a touch-sensitive liquid crystal display, or an OLED (Organic Light-Emitting Diode) touchscreen. The display 30 is used to display information on the terminal and to display a visual user interface.
[0104] In one embodiment, when the processor 10 executes the polycrystalline diamond thin film generation program 40 in the memory 20, the following steps are performed:
[0105] The target MPCVD equipment is identified, and the reaction chamber in the target MPCVD equipment is subjected to chamber cleaning and ignition treatment to obtain the target reaction chamber.
[0106] Determine the target nucleation formula, and perform nucleation growth treatment on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond;
[0107] A target growth formula is determined, and the initial diamond is grown and cultivated according to the target growth formula to obtain a target polycrystalline diamond film.
[0108] The cavity cleaning process includes vacuuming and gas replacement.
[0109] The process of identifying the target MPCVD equipment and performing chamber cleaning and ignition treatment on the reaction chamber within the target MPCVD equipment to obtain the target reaction chamber specifically includes:
[0110] The target MPCVD equipment is identified, and the reaction chamber in the target MPCVD equipment is evacuated using a vacuum pump to obtain the evacuated reaction chamber.
[0111] Hydrogen gas within a first preset concentration range is introduced into the vacuumed reaction chamber, and the hydrogen gas is used to perform gas replacement treatment on the vacuumed reaction chamber to obtain a replaced reaction chamber.
[0112] The vacuuming process and the gas replacement process are iteratively performed on the replaced reaction chamber. When the number of iterations reaches the preset number of iterations, the chamber cleaning process is completed, and a cleaned chamber is obtained.
[0113] The microwave is turned on, and the microwave energy in the cleaned cavity is obtained. The hydrogen gas in the cleaned cavity is broken down by the microwave energy to obtain a plasma ball. The ignition process is completed, and the target reaction cavity is obtained.
[0114] The process of determining the target nucleation formula and performing nucleation growth treatment on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond includes, prior to:
[0115] The preset heat dissipation device in the target MPCVD equipment is identified, and the temperature difference of the preset heat dissipation device is set to obtain the target heat dissipation device.
[0116] The preset heat dissipation device includes a silicon wafer, a molybdenum sheet, a molybdenum heat sink, a substrate stage, and a molybdenum cone.
[0117] The silicon wafer is located at the top of the preset heat dissipation device and is used to support the target diamond.
[0118] The molybdenum sheet is located below and adjacent to the silicon wafer;
[0119] The molybdenum heat sink is located below and adjacent to the molybdenum sheet;
[0120] The substrate stage is located at the bottom of the preset heat dissipation device and is adjacent to the molybdenum heat sink;
[0121] The molybdenum cone is connected to the silicon wafer and the substrate stage, respectively.
[0122] Specifically, setting a temperature difference for the preset heat dissipation device to obtain the target heat dissipation device includes:
[0123] A heat dissipation ring is provided at the position where the molybdenum cone contacts the substrate stage, so that the edge temperature of the target diamond on the silicon wafer is raised to a first preset value;
[0124] The silicon wafer and the molybdenum wafer are suspended in the air, so that the edge temperature of the target diamond on the silicon wafer increases from the first preset value to the second preset value;
[0125] Obtain the center temperature of the target diamond on the silicon wafer, and calculate the temperature difference between the second preset value and the center temperature;
[0126] When the temperature difference reaches the preset temperature difference, the temperature difference setting is completed, and the target heat dissipation device is obtained.
[0127] Specifically, determining the target nucleation formula and performing nucleation growth treatment on the target diamond placed in the target reaction chamber according to the target nucleation formula to obtain the initial diamond includes:
[0128] A target nucleation formulation is determined, and the target nucleation formulation is filled into the target reaction chamber, wherein the nucleation formulation includes hydrogen in a second preset concentration range, methane in a third preset concentration range, and nitrogen in a fourth preset concentration range.
[0129] The target reaction chamber is heated using the target nucleation formula. When the heating time reaches a preset time and the internal temperature of the target reaction chamber rises to a preset temperature, the target diamond is subjected to initial growth treatment using the preset temperature and the target nucleation formula to obtain an initial diamond.
[0130] The target growth formula includes a first growth formula and a second growth formula;
[0131] The process of determining the target growth formula and growing the initial diamond according to the target growth formula to obtain the target polycrystalline diamond film specifically includes:
[0132] An initial growth formula is determined, and the initial growth formula is adjusted according to a preset gradient value to obtain the first growth formula and the second growth formula;
[0133] The first growth formula consists of methane in a fifth preset concentration range, oxygen in a sixth preset concentration range, and nitrogen in a seventh preset concentration range.
[0134] The second growth formula consists of methane in the eighth preset concentration range, oxygen in the ninth preset concentration range, and nitrogen in the tenth preset concentration range.
[0135] A first growth time is determined, and within the first growth time range, the first growth formula is added to the target reaction chamber. The initial diamond is subjected to a first growth cultivation treatment using the first growth formula to obtain an initial polycrystalline diamond film.
[0136] A second growth time is determined. When the growth time of the initial polycrystalline diamond film reaches the second growth time, the initial polycrystalline diamond film is subjected to a second growth cultivation treatment using the second growth formula to obtain the target polycrystalline diamond film.
[0137] The present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a polycrystalline diamond thin film generation program, which, when executed by a processor, implements the steps of the polycrystalline diamond thin film generation method as described above.
[0138] In summary, this invention provides a method, system, terminal, and storage medium for generating polycrystalline diamond films. The method includes: identifying a target MPCVD device and performing chamber cleaning and sintering treatment on the reaction chamber of the target MPCVD device to obtain a target reaction chamber; identifying a target nucleation formula and performing nucleation growth treatment on a target diamond placed in the target reaction chamber according to the target nucleation formula to obtain an initial diamond; and identifying a target growth formula and performing growth cultivation treatment on the initial diamond according to the target growth formula to obtain a target polycrystalline diamond film. This invention effectively improves the growth efficiency and growth quality stability of polycrystalline diamond films by performing chamber cleaning and sintering treatment on the reaction chamber of the MPCVD device to create a favorable environment for diamond growth, setting a target nucleation formula for nucleation growth of the target diamond, and simultaneously setting a target growth formula for growth cultivation treatment of the initial diamond.
[0139] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or terminal. Unless otherwise specified, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or terminal that includes that element.
[0140] Of course, those skilled in the art will understand that all or part of the processes in the above embodiments can be implemented by a computer program instructing related hardware (such as a processor, controller, etc.). The program can be stored in a computer-readable storage medium, and when executed, it can include the processes described in the above method embodiments. The computer-readable storage medium can be a memory, magnetic disk, optical disk, etc.
[0141] It should be understood that the application of the present invention is not limited to the examples above. Those skilled in the art can make improvements or modifications based on the above description, and all such improvements and modifications should fall within the protection scope of the appended claims.
Claims
1. A method for producing a polycrystalline diamond film, characterized by, The method for preparing the polycrystalline diamond film comprises the following steps: determining a target MPCVD device, and performing cavity cleaning treatment and ignition treatment on a reaction cavity in the target MPCVD device to obtain a target reaction cavity; determining a target nucleation formula, and performing nucleation growth treatment on a target diamond placed in the target reaction cavity according to the target nucleation formula to obtain an initial diamond; The method further comprises the following steps before the step of determining a target nucleation formula and performing nucleation growth treatment on a target diamond placed in the target reaction cavity according to the target nucleation formula to obtain an initial diamond: determining a preset heat dissipation device in the target MPCVD device, and performing temperature difference setting on the preset heat dissipation device to obtain a target heat dissipation device; The preset heat dissipation device comprises a silicon wafer, a molybdenum sheet, a molybdenum heat dissipation sheet, a substrate table and a molybdenum cone table; The silicon wafer is located at the uppermost part of the preset heat dissipation device and is used for carrying the target diamond; The molybdenum sheet is located below the silicon wafer and is adjacent to the silicon wafer; The molybdenum heat dissipation sheet is located below the molybdenum sheet and is adjacent to the molybdenum sheet; The substrate table is located at the lowermost part of the preset heat dissipation device and is adjacent to the molybdenum heat dissipation sheet; The molybdenum cone table is connected with the silicon wafer and the substrate table, respectively; The temperature difference setting on the preset heat dissipation device to obtain a target heat dissipation device comprises the following steps: setting a heat dissipation ring at the position where the molybdenum cone table contacts with the substrate table, reducing the contact between the molybdenum cone table and the substrate table, reducing the heat dissipation efficiency of the molybdenum cone table, and increasing the edge temperature of the target diamond on the silicon wafer to a first preset value; suspension setting the silicon wafer and the molybdenum sheet, so that the edge temperature of the target diamond on the silicon wafer is increased from the first preset value to a second preset value; obtaining the center temperature of the target diamond on the silicon wafer, and calculating the temperature difference between the second preset value and the center temperature; when the temperature difference reaches a preset temperature difference, the temperature difference setting is completed, and a target heat dissipation device is obtained; By improving the preset heat dissipation device, a target heat dissipation device is obtained, and the center region temperature and the edge region temperature of the silicon wafer and the diamond thereon are controlled within a preset range, so as to reduce the edge region warping degree and ensure the normal growth of the polycrystalline diamond film; determining a target growth formula, and performing growth cultivation treatment on the initial diamond according to the target growth formula to obtain a target polycrystalline diamond film.
2. The method of claim 1, wherein the diamond thin film is polycrystalline. The cavity cleaning treatment comprises vacuumizing treatment and gas replacement treatment; The method further comprises the following steps before the step of determining a target MPCVD device, and performing cavity cleaning treatment and ignition treatment on a reaction cavity in the target MPCVD device to obtain a target reaction cavity: determining a target MPCVD device, and performing vacuumizing treatment on a reaction cavity in the target MPCVD device by a vacuum pump to obtain a vacuumized reaction cavity; filling a first preset concentration range of hydrogen into the vacuumized reaction cavity, and performing gas replacement treatment on the vacuumized reaction cavity by the hydrogen to obtain a replaced reaction cavity; The evacuated reaction cavity is iteratively subjected to the vacuumizing process and the gas replacing process, and when the iteration number reaches a preset iteration number, the cavity cleaning process is completed, and a cleaned cavity is obtained; Microwaves are turned on, and microwave energy in the cleaned cavity is obtained, and the hydrogen in the cleaned cavity is subjected to a breakdown process by the microwave energy, and a plasma ball is obtained, the ignition process is completed, and a target reaction cavity is obtained.
3. The method of claim 1, wherein the diamond thin film is polycrystalline. The target nucleation formula is determined, and the target diamond placed in the target reaction cavity is subjected to a nucleation growth process according to the target nucleation formula, and an initial diamond is obtained, specifically including: A target nucleation formula is determined, and the target nucleation formula is filled into the target reaction cavity, wherein the nucleation formula includes hydrogen gas in a second preset concentration range, methane in a third preset concentration range, and nitrogen gas in a fourth preset concentration range; When the temperature of the target reaction cavity is increased to a preset temperature, the target diamond is subjected to an initial growth process by the preset temperature and the target nucleation formula, and an initial diamond is obtained.
4. The method of claim 1, wherein the diamond film is polycrystalline. The target growth formula includes a first growth formula and a second growth formula; The target growth formula is determined, and the initial diamond is subjected to a growth cultivation process according to the target growth formula, and a target polycrystalline diamond film is obtained, specifically including: An initial growth formula is determined, and the initial growth formula is adjusted by a preset gradient value to obtain the first growth formula and the second growth formula; The first growth formula is methane in a fifth preset concentration range, oxygen in a sixth preset concentration range, and nitrogen in a seventh preset concentration range; The second growth formula is methane in an eighth preset concentration range, oxygen in a ninth preset concentration range, and nitrogen in a tenth preset concentration range; A first growth time is determined, and the first growth formula is added to the target reaction cavity within the first growth time range, and the initial diamond is subjected to a first growth cultivation process by the first growth formula, and an initial polycrystalline diamond film is obtained; A second growth time is determined, and when the growth time of the initial polycrystalline diamond film reaches the second growth time, the initial polycrystalline diamond film is subjected to a second growth cultivation process by the second growth formula, and a target polycrystalline diamond film is obtained.
5. A polycrystalline diamond film production system, characterised in that, The polycrystalline diamond film generation system is used to implement the polycrystalline diamond film generation method of any one of claims 1-4, and the polycrystalline diamond film generation system includes: a cavity environment setting module, configured to determine a target MPCVD device, and perform cavity cleaning and ignition processes on a reaction cavity in the target MPCVD device to obtain a target reaction cavity; A nucleation growth process module is configured to determine a target nucleation formula, and to perform a nucleation growth process on a target diamond placed in the target reaction cavity according to the target nucleation formula, and to obtain an initial diamond; A growth treatment module is configured to determine a target growth recipe and perform a growth treatment on the initial diamond according to the target growth recipe to obtain a target polycrystalline diamond film.
6. A terminal, characterized by comprising: The terminal comprises a memory, a processor, and a polycrystalline diamond film generation program stored in the memory and executable on the processor, and the polycrystalline diamond film generation program, when executed by the processor, implements the steps of the polycrystalline diamond film generation method according to any one of claims 1-4.
7. A computer-readable storage medium, characterized in that, The computer readable storage medium stores a polycrystalline diamond film generation program, and the polycrystalline diamond film generation program, when executed by the processor, implements the steps of the polycrystalline diamond film generation method according to any one of claims 1-4.
Citation Information
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