A low-pressure and low-temperature single-crystal diamond batch annealing method, system and terminal

Abstract

The present invention discloses a low-pressure and low-temperature single-crystal diamond batch annealing method, system and terminal, the method comprising: determining a plurality of diamonds to be annealed, and obtaining the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include a semi-finished blank state and a finished blank state; if the diamond blank states of all diamonds to be annealed are the semi-finished blank state, then all the diamonds to be annealed are subjected to a first annealing treatment to obtain a plurality of first target single-crystal diamonds; if the diamond blank states of all diamonds to be annealed are all the finished blank states, then all the diamonds to be annealed are subjected to a slicing treatment and a second annealing treatment to obtain a plurality of second target single-crystal diamonds. The present invention can realize batch annealing of single-crystal diamonds by adopting a low-pressure and low-temperature method, which not only effectively reduces the internal stress of the single-crystal diamond, but also effectively reduces the annealing cost of the single-crystal diamond.

Description

Technical Field

[0001] The present invention relates to the field of diamond cultivation technology, and in particular to a low-pressure and low-temperature single-crystal diamond batch annealing method, system, terminal and computer-readable storage medium. Background Art

[0002] Diamond has many excellent properties, such as extremely high thermal conductivity, extremely low thermal expansion coefficient, strong corrosion resistance and ultra-high hardness, etc. It is a material with relatively broad application prospects. However, due to the changes in temperature conditions and doping during the growth process of single-crystal diamond, the single-crystal diamond obtained after growth generally has the problem of excessive stress, which will cause the diamond blank to release stress during the intermediate cutting, grinding and polishing and the final cutting and grinding of the bare diamond, thereby causing the blank to crack or break, resulting in a decrease in the overall yield. In order to solve the above problems, the prior art generally chooses annealing treatment to reduce or remove the stress of single-crystal diamond.

[0003] The more common annealing processes in the prior art are mainly divided into two categories, one is high pressure high temperature annealing (HPHT), and the other is low pressure high temperature annealing (LPHT) using MPCVD equipment. However, the above two annealing methods are both expensive and are not suitable for batch annealing of single crystal diamonds, and cannot meet users' needs for batch annealing of single crystal diamonds.

[0004] Therefore, the prior art still needs to be improved and developed. Summary of the invention

[0005] The main purpose of the present invention is to provide a low-pressure and low-temperature single-crystal diamond batch annealing method, system, terminal and computer-readable storage medium, aiming to solve the problem that the single-crystal diamond annealing process cost in the prior art is high and cannot meet the user's demand for batch annealing of single-crystal diamond.

[0006] To achieve the above object, the present invention provides a low-pressure and low-temperature single crystal diamond batch annealing method, the low-pressure and low-temperature single crystal diamond batch annealing method comprising the following steps:

[0007] Determine a plurality of diamonds to be annealed, and obtain the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states;

[0008] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds;

[0009] If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds.

[0010] Optionally, in the low-pressure and low-temperature single crystal diamond batch annealing method, the first annealing treatment includes a first temperature increase treatment and a first temperature decrease treatment;

[0011] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds, specifically comprising:

[0012] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, all the diamonds to be annealed are placed on the target molybdenum sheet with the growth surface facing upward, and the target molybdenum sheet carrying all the diamonds to be annealed is placed in the reaction chamber of the MPCVD device;

[0013] Setting a preset temperature rising environment, and performing a first temperature rising treatment on all the diamonds to be annealed according to the preset temperature rising environment, to obtain a plurality of initial target single crystal diamonds;

[0014] After the first temperature increase treatment is completed, a preset temperature reduction environment is set, and the first temperature reduction treatment is performed on all the initial target single crystal diamonds according to the preset temperature reduction environment to obtain a plurality of first target single crystal diamonds.

[0015] Optionally, the low-pressure and low-temperature single crystal diamond batch annealing method, wherein the setting of a preset heating environment and performing a first heating treatment on all the diamonds to be annealed according to the preset heating environment to obtain a plurality of initial target single crystal diamonds, specifically includes:

[0016] Setting the preset temperature rise environment, wherein the preset temperature rise environment includes a preset hydrogen concentration range, a first preset air pressure range, and a first preset power range;

[0017] Acquiring a first current crystal surface temperature of all the diamonds to be annealed, and raising the first current crystal surface temperature of all the diamonds to be annealed to a first preset crystal surface temperature within a first preset time range according to the preset temperature rising environment, and maintaining all the diamonds to be annealed at the first preset crystal surface temperature;

[0018] When the holding time of the first preset crystal surface temperature reaches a second preset time range, it indicates that the first temperature increase treatment of all the diamonds to be annealed is completed, and a plurality of initial target single crystal diamonds are obtained.

[0019] Optionally, the low-pressure and low-temperature single crystal diamond batch annealing method, wherein after the first temperature increase treatment is completed, a preset temperature reduction environment is set, and a first temperature reduction treatment is performed on all the initial target single crystal diamonds according to the preset temperature reduction environment to obtain a plurality of first target single crystal diamonds, specifically includes:

[0020] When the first temperature increase treatment of all the diamonds to be annealed is completed, the preset temperature reduction environment is set, wherein the preset temperature reduction environment includes the preset hydrogen concentration range, the second preset pressure range and the second preset power range, wherein the second preset pressure range is smaller than the first preset pressure range, and the second preset power range is smaller than the first preset power range;

[0021] According to the preset cooling environment, the first preset crystal surface temperature of all the initial target single crystal diamonds is reduced to a second preset crystal surface temperature within the first preset time range, and when the first cooling treatment of all the initial target single crystal diamonds is completed, a plurality of first target single crystal diamonds are obtained.

[0022] Optionally, in the low-pressure and low-temperature single crystal diamond batch annealing method, the second annealing treatment includes a second temperature increase treatment and a second temperature decrease treatment;

[0023] If the diamond blank states of all the diamonds to be annealed are all in the finished blank state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds, specifically comprising:

[0024] If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, all the diamonds to be annealed are sliced ​​to obtain a plurality of sliced ​​diamonds to be annealed, wherein the slicing process refers to cutting off edge polycrystals on all the diamonds to be annealed;

[0025] Placing all the sliced ​​diamonds to be annealed on the target molybdenum sheet with the growth surface facing upward, and placing the target molybdenum sheet carrying all the sliced ​​diamonds to be annealed into the reaction chamber of the MPCVD device;

[0026] Performing a second temperature increase treatment on all the sliced ​​diamonds to be annealed according to the preset temperature increase environment to obtain a plurality of initial sliced ​​diamonds to be annealed;

[0027] After the second temperature rising treatment is completed, a second temperature falling treatment is performed on all the initially sliced ​​diamonds to be annealed according to the preset temperature falling environment to obtain a plurality of second target single crystal diamonds.

[0028] Optionally, the low-pressure and low-temperature single crystal diamond batch annealing method, wherein the second heating treatment is performed on all the sliced ​​diamonds to be annealed according to the preset heating environment to obtain a plurality of initial sliced ​​diamonds to be annealed, specifically comprises:

[0029] Acquiring the second current crystal surface temperature of all the sliced ​​diamonds to be annealed, and raising the second current crystal surface temperature of all the sliced ​​diamonds to be annealed to the first preset crystal surface temperature within the first preset time range according to the preset temperature rising environment, and making all the sliced ​​diamonds to be annealed maintain the first preset crystal surface temperature;

[0030] When the holding time of the first preset crystal surface temperature reaches a third preset time range, it indicates that the second temperature rise treatment of all the sliced ​​diamonds to be annealed is completed, and a plurality of initial sliced ​​diamonds to be annealed are obtained.

[0031] Optionally, the low-pressure and low-temperature single crystal diamond batch annealing method, wherein after the second temperature increase treatment is completed, a second temperature reduction treatment is performed on all the initial sliced ​​diamonds to be annealed according to the preset temperature reduction environment to obtain a plurality of second target single crystal diamonds, specifically comprising:

[0032] After the second temperature increase treatment of all the sliced ​​diamonds to be annealed is completed, the first preset crystal surface temperature of all the initial sliced ​​diamonds to be annealed is reduced to the second preset crystal surface temperature within a fourth preset time range according to the preset temperature reduction environment;

[0033] When the second temperature reduction treatment of all the initially sliced ​​diamonds to be annealed is completed, a plurality of second target single crystal diamonds are obtained.

[0034] In addition, to achieve the above-mentioned purpose, the present invention also provides a low-pressure and low-temperature single crystal diamond batch annealing system, wherein the low-pressure and low-temperature single crystal diamond batch annealing system comprises:

[0035] A diamond blank state acquisition module, used for determining a plurality of diamonds to be annealed, and acquiring the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states;

[0036] A first annealing treatment module, for performing a first annealing treatment on all the diamonds to be annealed if the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, so as to obtain a plurality of first target single crystal diamonds;

[0037] The second annealing treatment module is used for performing slicing treatment and second annealing treatment on all the diamonds to be annealed if the diamond blank states of all the diamonds to be annealed are all in the finished blank state, so as to obtain a plurality of second target single crystal diamonds.

[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 low-pressure and low-temperature single-crystal diamond batch annealing program stored in the memory and executable on the processor, wherein the low-pressure and low-temperature single-crystal diamond batch annealing program, when executed by the processor, implements the steps of the low-pressure and low-temperature single-crystal diamond batch annealing method as described above.

[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 low-pressure and low-temperature single crystal diamond batch annealing program, and when the low-pressure and low-temperature single crystal diamond batch annealing program is executed by a processor, the steps of the low-pressure and low-temperature single crystal diamond batch annealing method as described above are implemented.

[0040] In the present invention, multiple diamonds to be annealed are determined, and the diamond blank states of the multiple diamonds to be annealed are obtained, wherein the diamond blank states include semi-finished blank states and finished blank states; if the diamond blank states of all the diamonds to be annealed are all the semi-finished blank states, then all the diamonds to be annealed are subjected to a first annealing treatment to obtain multiple first target single crystal diamonds; if the diamond blank states of all the diamonds to be annealed are all the finished blank states, then all the diamonds to be annealed are subjected to a slicing treatment and a second annealing treatment to obtain multiple second target single crystal diamonds. The present invention determines the annealing method of the diamonds to be annealed by different diamond blank states, including the first annealing treatment method for the diamonds to be annealed in the semi-finished blank state, and the slicing treatment and the second annealing treatment method for the diamonds to be annealed in the finished blank state, which can achieve the batch annealing effect of single crystal diamonds under low pressure and low temperature conditions, which not only effectively reduces the internal stress of the single crystal diamond, but also effectively reduces the annealing cost of the single crystal diamond. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a flow chart of a preferred embodiment of the low-pressure and low-temperature single crystal diamond batch annealing method of the present invention;

[0042] Figure 2 It is a structural diagram of a preferred embodiment of the low-pressure and low-temperature single-crystal diamond batch annealing system of the present invention;

[0043] Figure 3 It is a structural diagram of a preferred embodiment of the terminal of the present invention. DETAILED DESCRIPTION

[0044] 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.

[0045] Diamond has many excellent properties, such as extremely high thermal conductivity, extremely low thermal expansion coefficient, extremely strong corrosion resistance and ultra-high hardness (Mohs hardness is 10), and is a material with relatively broad application prospects. However, during the manufacturing process, due to various reasons, such as doping, cutting, grinding and polishing, etc., large stress will be caused, which leads to the following two problems of single crystal diamond: 1. Due to the changes in temperature conditions and doping during the growth process of single crystal diamond, the single crystal diamond after growth generally has the problem of excessive stress, which will cause the single crystal diamond blank to release stress during the intermediate cutting, grinding and polishing and the final cutting and polishing of the bare diamond, resulting in cracks or fragmentation of the single crystal diamond blank, which reduces the overall yield; 2. The reason why diamond shows a sparkling side is that in addition to the very high refractive index, high transparency and relatively excellent cutting of the diamond itself, it is also because the low-defect and low-stress diamond has a high dispersion value, which allows light to propagate smoothly inside it. However, the defects and impurities generated in the growth and processing of cultured diamonds will cause large stress inside the diamond, thereby affecting the diamond's dispersion and absorption of light, and then changing the transparency and fire of the diamond. Based on the above two reasons, many single crystal diamond manufacturers generally choose to use annealing treatment to reduce or remove the internal stress of single crystal diamonds in order to obtain diamonds that are less prone to breakage, whiter in color and have better fire.

[0046] At present, the more common annealing processes on the market are mainly divided into two categories. One is high pressure and high temperature annealing (HPHT). This annealing process can change the defect structure inside the diamond, thereby changing its color, but this annealing process requires the use of six-sided top equipment for special processing. Among them, the process of high pressure and high temperature annealing is as follows: the single crystal diamond is placed in an environment of 1500-2000℃ and an air pressure of about 5GPa, which can rearrange the impurities in the single crystal diamond to form different defect centers. Generally, the single crystal diamond treated with high temperature and high pressure has significantly reduced internal stress, and the diamond color can also be increased by 1-2 levels. For example, diamond blanks with color grades of G and H can generally reach the color level of E and F after high pressure and high temperature annealing.

[0047] Another method is low-pressure high-temperature annealing using MPCVD equipment, namely LPHT. This annealing process requires a gas pressure of at least 240 Torr (generally between 240-296 Torr), a temperature of 1700°C or above, and an annealing time of about 10-60 minutes. However, for MPCVD equipment, under high pressure conditions, the plasma coverage area will be reduced, and its temperature uniformity is extremely poor, so this process cannot be annealed in batches, and can only process 1-2 diamond blanks at a time. In addition, during the operation, diamond crystals are very easy to graphitize, and may even be directly ablated into graphite slag, which is not suitable for mass production.

[0048] The costs of the above two annealing methods are relatively high, especially high temperature and high pressure annealing. For the production of MPCVD cultured diamonds, special six-sided top press equipment is required. Generally, annealing needs to be outsourced. The annealing process cannot be independently controlled, and parameters cannot be adjusted according to the characteristics of their own products.

[0049] In order to solve the above problems, the present invention proposes a low-pressure and low-temperature batch annealing method for single-crystal diamonds. The low-pressure and low-temperature long-term annealing method adopted by the present invention has the advantages of low cost, batch annealing of diamond blanks, meeting the needs of batch production, and the crystals are not easy to graphitize and have a low scrap rate. After long-term annealing at low pressure and low temperature, the internal stress of the diamond crystal can be effectively improved, so that the crystal scrap rate caused by stress during diamond crystal processing is reduced from the previous 20% to less than 0.5%, and the color of the diamond is basically stable and maintained at around F, G, and H.

[0050] The low-pressure and low-temperature batch annealing method for single-crystal diamond described in the preferred embodiment of the present invention is as follows: Figure 1 As shown, the low-pressure and low-temperature single crystal diamond batch annealing method comprises the following steps:

[0051] Step S10, determining a plurality of diamonds to be annealed, and obtaining the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states.

[0052] The annealing process in the present invention is targeted at MPCVD cultured diamonds (i.e., diamonds to be annealed in the present invention). Different annealing processes are selected for cultured diamonds at different stages (i.e., diamonds in a semi-finished rough state and diamonds in a finished rough state in the present invention).

[0053] Among them, there is a difference in thickness between the diamond in the semi-finished blank state and the diamond in the finished blank state, but the crystal appearance of the diamond in the semi-finished blank state or the finished blank state will not change before and after annealing, but the color before and after annealing will be different (the color of the crystal before annealing is light yellow, and the color of the crystal after annealing is transparent, and the internal stress of the diamond is reduced after annealing).

[0054] In addition, the diamond in the semi-finished rough state needs to continue to grow after annealing until it grows into a diamond in the finished rough state.

[0055] Step S20: If the diamond blanks of all the diamonds to be annealed are in the semi-finished blank state, a first annealing treatment is performed on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds, wherein the first annealing treatment includes a first temperature increase treatment and a first temperature decrease treatment.

[0056] The present invention sets different annealing processes according to different diamond blank states. For diamonds to be annealed in a semi-finished blank state, annealing treatment is required when the edge polycrystalline is not processed (i.e., the first annealing treatment in the present invention). In fact, the annealing process includes the steps of heating up first and then cooling down. By creating a low-pressure and low-temperature environment, the stress inside the single crystal diamond is reduced, thereby achieving the annealing effect.

[0057] Specifically, if the diamond blank state of all the diamonds to be annealed is the semi-finished blank state, all the diamonds to be annealed are placed on the target molybdenum sheet with the growth surface facing upward, and the target molybdenum sheet carrying all the diamonds to be annealed is placed in the reaction chamber of the MPCVD equipment.

[0058] During the annealing process of the plurality of diamonds to be annealed in the state of semi-finished roughcasts, they need to be placed on a molybdenum sheet and then put into the reaction chamber of the MPCVD equipment in batches, so as to realize batch annealing treatment.

[0059] The preset temperature rising environment is set, wherein the preset temperature rising environment includes a preset hydrogen concentration range, a first preset gas pressure range, and a first preset power range; the first current crystal surface temperature of all the diamonds to be annealed is obtained, and the first current crystal surface temperature of all the diamonds to be annealed is increased to a first preset crystal surface temperature within a first preset time range according to the preset temperature rising environment, and all the diamonds to be annealed are kept at the first preset crystal surface temperature; when the holding time of the first preset crystal surface temperature reaches a second preset time range, it indicates that the first temperature rising treatment of all the diamonds to be annealed is completed, and a plurality of initial target single crystal diamonds are obtained.

[0060] For the annealing process of single crystal diamond, it is first necessary to heat it up. By building a preset heating environment, the crystal surface temperature of the diamond to be annealed reaches a preset temperature value and lasts for a period of time, which can make the subsequent cooling annealing process more effective.

[0061] When the first temperature increase treatment of all the diamonds to be annealed is completed, the preset temperature reduction environment is set, wherein the preset temperature reduction environment includes the preset hydrogen concentration range, the second preset pressure range and the second preset power range, wherein the second preset pressure range is smaller than the first preset pressure range, and the second preset power range is smaller than the first preset power range; according to the preset temperature reduction environment, the first preset crystal surface temperature of all the initial target single crystal diamonds is reduced to the second preset crystal surface temperature within the first preset time range, and when the first temperature reduction treatment of all the initial target single crystal diamonds is completed, a plurality of first target single crystal diamonds are obtained.

[0062] The air pressure value and power value in the preset cooling environment set in the present invention are both lower than the air pressure value and power value in the preset heating environment, thereby creating a low-pressure condition; at the same time, by reducing the surface temperature of the diamond to be annealed from a first preset crystal surface temperature to a second preset crystal surface temperature, thereby creating a low-temperature condition, and in this low-pressure and low-temperature environment, the internal stress of the diamond can be effectively improved.

[0063] It is understandable that the thickness of diamond in the semi-finished blank state has not yet reached the standard blank thickness (generally the standard blank thickness is the shortest side * 0.6mm). After the crystal growth of the semi-finished blank is completed (that is, the diamond is in the semi-finished blank state), the diamond in the semi-finished blank state is annealed when the edge is not processed (the reason why annealing is required when the edge is not processed is that cracks will appear when cutting the unannealed diamond. If it is cut directly, the crystal will crack, so it needs to be annealed first to reduce its internal stress before edge trimming).

[0064] The specific annealing process of diamond in the semi-finished rough state is as follows: 1. The crystal heat dissipation surface (i.e., the back side of the diamond to be annealed) of the semi-finished rough state diamond to be annealed is facing downward (i.e., the growth surface is facing upward), and the batch is placed on a molybdenum sheet (i.e., the target molybdenum sheet in the present invention), and placed in the cavity of the MPCVD equipment; 2. The temperature is increased (preferably set to about 30 minutes, i.e., the first preset time range in the present invention), and the atmosphere condition in the cavity of the MPCVD equipment (i.e., the preset heating environment in the present invention) is hydrogen: 200-500sccm (i.e., the preset hydrogen concentration range in the present invention, and ignition is performed by hydrogen). In order to make the temperature more uniform, the gas pressure is preferably set at 130-175Torr (i.e., the first preset gas pressure range in the present invention), and the power is set at 3700-5 3. The temperature of the diamond crystal surface to be annealed is raised to 1100-1300° C. (the first preset crystal surface temperature in the present invention) by applying a power of 300W (i.e., the first preset power range in the present invention) to raise the crystal surface temperature of the diamond to be annealed to 1100-1300° C. (i.e., the first preset crystal surface temperature in the present invention); 3. Stay at this temperature for about 120-180 minutes (i.e., the second preset time range in the present invention), and then cool down (wherein, the cooling environment needs to set the atmosphere environment (i.e., the preset cooling environment in the present invention) to: the air pressure is preferably set to about 25Torr (i.e., the second preset air pressure range in the present invention), and the power is set to about 600W (i.e., the second preset power range in the present invention), until the crystal surface temperature of the diamond to be annealed drops to room temperature, which is the second preset crystal surface temperature in the present invention), wherein the cooling time is generally set to not less than 30 minutes.

[0065] Furthermore, after the semi-finished rough diamond is annealed, the diamond will continue to be cultivated and can subsequently continue to grow into a finished rough diamond.

[0066] Step S30: If the diamond blanks of all the diamonds to be annealed are in the finished blank state, all the diamonds to be annealed are subjected to slicing and second annealing to obtain a plurality of second target single crystal diamonds. The second annealing includes a second heating treatment and a second cooling treatment.

[0067] For the diamond in the finished rough state, it should be sliced ​​before annealing. By cutting off the edge polycrystalline of the diamond in the finished rough state, the annealing effect of the diamond in the finished rough state can be further optimized.

[0068] Specifically, if the diamond blank state of all the diamonds to be annealed is the finished blank state, all the diamonds to be annealed are sliced ​​to obtain a plurality of sliced ​​diamonds to be annealed, wherein the slicing process refers to cutting off the edge polycrystals on all the diamonds to be annealed; placing all the sliced ​​diamonds to be annealed with the growth surface facing upward on the target molybdenum sheet, and placing the target molybdenum sheet carrying all the sliced ​​diamonds to be annealed into the reaction chamber of the MPCVD equipment.

[0069] The second current crystal surface temperature of all the sliced ​​diamonds to be annealed is obtained, and the second current crystal surface temperature of all the sliced ​​diamonds to be annealed is increased to the first preset crystal surface temperature within the first preset time range according to the preset temperature increase environment, and all the sliced ​​diamonds to be annealed are kept at the first preset crystal surface temperature; when the holding time of the first preset crystal surface temperature reaches a third preset time range, it indicates that the second temperature increase treatment of all the sliced ​​diamonds to be annealed is completed, and a plurality of initial sliced ​​diamonds to be annealed are obtained.

[0070] When the second temperature rising treatment of all the sliced ​​diamonds to be annealed is completed, the first preset crystal surface temperature of all the initial sliced ​​diamonds to be annealed is reduced to the second preset crystal surface temperature within a fourth preset time range according to the preset cooling environment; when the second temperature falling treatment of all the initial sliced ​​diamonds to be annealed is completed, a plurality of second target single crystal diamonds are obtained.

[0071] Diamonds that have reached the finished rough state need to be sliced ​​before the annealing process (using a laser cutting machine to cut off the edge polycrystalline of the diamond in the finished rough state without affecting the internal crystals).

[0072] The annealing process of diamond in the finished blank state is as follows: 1. After edge trimming, the diamond in the finished blank state is placed with its growth surface facing upward on the target molybdenum sheet, and then placed in batches into the reaction chamber of the MPCVD equipment; 2. A heating treatment is performed, the heating time is about 30 minutes (i.e., the first preset time range in the present invention), the atmosphere condition (i.e., the preset heating environment in the present invention, the preset heating environment of the diamond in the finished blank state is the same as that of the diamond in the semi-finished blank state) is hydrogen 200-500sccm (i.e., the preset hydrogen concentration range in the present invention), and in order to make the temperature more uniform, the gas pressure is preferably set at 130-175Torr (i.e., the first preset gas pressure in the present invention). The power is set at 3700-5300W (i.e., the first preset power range in the present invention) so that the crystal surface temperature of the diamond in the finished blank state is 1100-1300°C (i.e., the first preset crystal surface temperature in the present invention); 3. Stay at this temperature for about 480-600 minutes (i.e., the third preset time range in the present invention), and then cool down (to room temperature, i.e., the second preset crystal surface temperature in the present invention), and the cooling time shall not be less than 30 minutes (i.e., the fourth preset time range in the present invention), wherein the cooling link needs to construct a preset cooling environment, and the preset cooling environment of the diamond in the finished blank state is the same as that of the diamond in the semi-finished blank state.

[0073] For the inspection of the effect of annealing of semi-finished rough diamonds or finished rough diamonds, one can check it through a polarizing microscope; the second most direct way is to check the number of crystal cracks before and after annealing. When the crystal is directly processed without annealing, the proportion of crystal cracks is about 22.3%; while the proportion of crystal cracks during processing is only about 0.5% when the crystal is annealed first and then processed. This is because the internal stress of the single crystal diamond is greatly reduced after annealing, so it is not easy to break during intermediate processing and rough diamond cutting and grinding, and it can effectively reduce the color difference caused by stress (the color of the diamond will also change after annealing, from light yellow to transparent).

[0074] In summary, the present invention can achieve batch annealing of single crystal diamond under low pressure and low temperature conditions, which not only effectively reduces the internal stress of the single crystal diamond, but also effectively reduces the annealing cost of the single crystal diamond.

[0075] Furthermore, if Figure 2 As shown, based on the above-mentioned low-pressure and low-temperature single crystal diamond batch annealing method, the present invention also provides a low-pressure and low-temperature single crystal diamond batch annealing system, wherein the low-pressure and low-temperature single crystal diamond batch annealing system comprises:

[0076] A diamond blank state acquisition module 51 is used to determine a plurality of diamonds to be annealed, and acquire the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states;

[0077] A first annealing treatment module 52 is used for performing a first annealing treatment on all the diamonds to be annealed if the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state to obtain a plurality of first target single crystal diamonds;

[0078] The second annealing treatment module 53 is used for performing slicing treatment and second annealing treatment on all the diamonds to be annealed if the diamond rough states of all the diamonds to be annealed are all in the finished rough state, so as to obtain a plurality of second target single crystal diamonds.

[0079] Furthermore, if Figure 3 As shown, based on the above-mentioned low-pressure and low-temperature single crystal diamond batch annealing method and system, the present invention also provides a terminal accordingly, and the terminal includes a processor 10, a memory 20 and a display 30. Figure 3 Only some components of the terminal are shown, but it should be understood that it is not required to implement all of the components shown, and more or fewer components may be implemented instead.

[0080] 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 (Secure Digital, 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 in the terminal, such as the program code of the installation terminal. The memory 20 may also be used to temporarily store data that has been output or is to be output. In one embodiment, a low-pressure and low-temperature single crystal diamond batch annealing program 40 is stored on the memory 20, and the low-pressure and low-temperature single crystal diamond batch annealing program 40 can be executed by the processor 10, thereby realizing the low-pressure and low-temperature single crystal diamond batch annealing method in the present application.

[0081] 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 low-pressure and low-temperature single crystal diamond batch annealing method.

[0082] 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.

[0083] In one embodiment, when the processor 10 executes the low-pressure and low-temperature single crystal diamond batch annealing program 40 in the memory 20, the following steps are implemented:

[0084] Determine a plurality of diamonds to be annealed, and obtain the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states;

[0085] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds;

[0086] If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds.

[0087] Wherein, the first annealing treatment includes a first temperature rising treatment and a first temperature falling treatment;

[0088] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds, specifically comprising:

[0089] If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, all the diamonds to be annealed are placed on the target molybdenum sheet with the growth surface facing upward, and the target molybdenum sheet carrying all the diamonds to be annealed is placed in the reaction chamber of the MPCVD device;

[0090] Setting a preset temperature rising environment, and performing a first temperature rising treatment on all the diamonds to be annealed according to the preset temperature rising environment, to obtain a plurality of initial target single crystal diamonds;

[0091] After the first temperature increase treatment is completed, a preset temperature reduction environment is set, and the first temperature reduction treatment is performed on all the initial target single crystal diamonds according to the preset temperature reduction environment to obtain a plurality of first target single crystal diamonds.

[0092] The step of setting a preset temperature rise environment and performing a first temperature rise treatment on all the diamonds to be annealed according to the preset temperature rise environment to obtain a plurality of initial target single crystal diamonds specifically includes:

[0093] Setting the preset temperature rise environment, wherein the preset temperature rise environment includes a preset hydrogen concentration range, a first preset air pressure range, and a first preset power range;

[0094] Acquiring a first current crystal surface temperature of all the diamonds to be annealed, and raising the first current crystal surface temperature of all the diamonds to be annealed to a first preset crystal surface temperature within a first preset time range according to the preset temperature rising environment, and maintaining all the diamonds to be annealed at the first preset crystal surface temperature;

[0095] When the holding time of the first preset crystal surface temperature reaches a second preset time range, it indicates that the first temperature increase treatment of all the diamonds to be annealed is completed, and a plurality of initial target single crystal diamonds are obtained.

[0096] Wherein, after the first temperature rising treatment is completed, a preset temperature falling environment is set, and a first temperature falling treatment is performed on all the initial target single crystal diamonds according to the preset temperature falling environment to obtain a plurality of first target single crystal diamonds, specifically including:

[0097] When the first temperature increase treatment of all the diamonds to be annealed is completed, the preset temperature reduction environment is set, wherein the preset temperature reduction environment includes the preset hydrogen concentration range, the second preset pressure range and the second preset power range, wherein the second preset pressure range is smaller than the first preset pressure range, and the second preset power range is smaller than the first preset power range;

[0098] According to the preset cooling environment, the first preset crystal surface temperature of all the initial target single crystal diamonds is reduced to a second preset crystal surface temperature within the first preset time range, and when the first cooling treatment of all the initial target single crystal diamonds is completed, a plurality of first target single crystal diamonds are obtained.

[0099] Wherein, the second annealing treatment includes a second temperature rising treatment and a second temperature falling treatment;

[0100] If the diamond blank states of all the diamonds to be annealed are all in the finished blank state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds, specifically comprising:

[0101] If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, all the diamonds to be annealed are sliced ​​to obtain a plurality of sliced ​​diamonds to be annealed, wherein the slicing process refers to cutting off edge polycrystals on all the diamonds to be annealed;

[0102] Placing all the sliced ​​diamonds to be annealed on the target molybdenum sheet with the growth surface facing upward, and placing the target molybdenum sheet carrying all the sliced ​​diamonds to be annealed into the reaction chamber of the MPCVD device;

[0103] Performing a second temperature increase treatment on all the sliced ​​diamonds to be annealed according to the preset temperature increase environment to obtain a plurality of initial sliced ​​diamonds to be annealed;

[0104] After the second temperature rising treatment is completed, a second temperature falling treatment is performed on all the initially sliced ​​diamonds to be annealed according to the preset temperature falling environment to obtain a plurality of second target single crystal diamonds.

[0105] The step of performing a second heating treatment on all the sliced ​​diamonds to be annealed according to the preset heating environment to obtain a plurality of initial sliced ​​diamonds to be annealed specifically includes:

[0106] Acquiring the second current crystal surface temperature of all the sliced ​​diamonds to be annealed, and raising the second current crystal surface temperature of all the sliced ​​diamonds to be annealed to the first preset crystal surface temperature within the first preset time range according to the preset temperature rising environment, and making all the sliced ​​diamonds to be annealed maintain the first preset crystal surface temperature;

[0107] When the holding time of the first preset crystal surface temperature reaches a third preset time range, it indicates that the second temperature rise treatment of all the sliced ​​diamonds to be annealed is completed, and a plurality of initial sliced ​​diamonds to be annealed are obtained.

[0108] Wherein, after the second temperature rising treatment is completed, a second temperature lowering treatment is performed on all the initially sliced ​​diamonds to be annealed according to the preset temperature lowering environment to obtain a plurality of second target single crystal diamonds, specifically including:

[0109] After the second temperature increase treatment of all the sliced ​​diamonds to be annealed is completed, the first preset crystal surface temperature of all the initial sliced ​​diamonds to be annealed is reduced to the second preset crystal surface temperature within a fourth preset time range according to the preset temperature reduction environment;

[0110] When the second temperature reduction treatment of all the initially sliced ​​diamonds to be annealed is completed, a plurality of second target single crystal diamonds are obtained.

[0111] The present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a low-pressure and low-temperature single crystal diamond batch annealing program, and when the low-pressure and low-temperature single crystal diamond batch annealing program is executed by a processor, the steps of the low-pressure and low-temperature single crystal diamond batch annealing method as described above are implemented.

[0112] In summary, the present invention provides a low-pressure and low-temperature single-crystal diamond batch annealing method and related equipment, the method comprising: determining a plurality of diamonds to be annealed, and obtaining the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include a semi-finished blank state and a finished blank state; if the diamond blank states of all the diamonds to be annealed are all the semi-finished blank states, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single-crystal diamonds; if the diamond blank states of all the diamonds to be annealed are all the finished blank states, performing a slicing treatment and a second annealing treatment on all the diamonds to be annealed to obtain a plurality of second target single-crystal diamonds. The present invention determines the annealing method of the diamond to be annealed according to different diamond blank states, including adopting the first annealing treatment method for the diamond to be annealed in the semi-finished blank state, and adopting the slicing treatment and the second annealing treatment method for the diamond to be annealed in the finished blank state, which can achieve the batch annealing effect of single crystal diamond under low pressure and low temperature conditions, not only effectively reducing the internal stress of the single crystal diamond, but also effectively reducing the annealing cost of the single crystal diamond.

[0113] 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.

[0114] 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.

[0115] 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 low-pressure and low-temperature single crystal diamond batch annealing method, characterized in that: The low-pressure and low-temperature single crystal diamond batch annealing method comprises: Determine a plurality of diamonds to be annealed, and obtain the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states; If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds; If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds.

2. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 1, characterized in that: The first annealing treatment includes a first temperature rising treatment and a first temperature falling treatment; If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, performing a first annealing treatment on all the diamonds to be annealed to obtain a plurality of first target single crystal diamonds, specifically comprising: If the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, all the diamonds to be annealed are placed on the target molybdenum sheet with the growth surface facing upward, and the target molybdenum sheet carrying all the diamonds to be annealed is placed in the reaction chamber of the MPCVD device; Setting a preset temperature rising environment, and performing a first temperature rising treatment on all the diamonds to be annealed according to the preset temperature rising environment, to obtain a plurality of initial target single crystal diamonds; After the first temperature increase treatment is completed, a preset temperature reduction environment is set, and the first temperature reduction treatment is performed on all the initial target single crystal diamonds according to the preset temperature reduction environment to obtain a plurality of first target single crystal diamonds.

3. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 2, characterized in that: The step of setting a preset temperature rising environment and performing a first temperature rising treatment on all the diamonds to be annealed according to the preset temperature rising environment to obtain a plurality of initial target single crystal diamonds specifically includes: Setting the preset temperature rise environment, wherein the preset temperature rise environment includes a preset hydrogen concentration range, a first preset air pressure range, and a first preset power range; Acquiring a first current crystal surface temperature of all the diamonds to be annealed, and raising the first current crystal surface temperature of all the diamonds to be annealed to a first preset crystal surface temperature within a first preset time range according to the preset temperature rising environment, and maintaining all the diamonds to be annealed at the first preset crystal surface temperature; When the holding time of the first preset crystal surface temperature reaches a second preset time range, it indicates that the first temperature increase treatment of all the diamonds to be annealed is completed, and a plurality of initial target single crystal diamonds are obtained.

4. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 3, characterized in that: After the first temperature rise treatment is completed, a preset temperature drop environment is set, and a first temperature drop treatment is performed on all the initial target single crystal diamonds according to the preset temperature drop environment to obtain a plurality of first target single crystal diamonds, specifically including: When the first temperature increase treatment of all the diamonds to be annealed is completed, the preset temperature reduction environment is set, wherein the preset temperature reduction environment includes the preset hydrogen concentration range, the second preset pressure range and the second preset power range, wherein the second preset pressure range is smaller than the first preset pressure range, and the second preset power range is smaller than the first preset power range; According to the preset cooling environment, the first preset crystal surface temperature of all the initial target single crystal diamonds is reduced to a second preset crystal surface temperature within the first preset time range, and when the first cooling treatment of all the initial target single crystal diamonds is completed, a plurality of first target single crystal diamonds are obtained.

5. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 4, characterized in that: The second annealing treatment includes a second temperature rising treatment and a second temperature falling treatment; If the diamond blank states of all the diamonds to be annealed are all in the finished blank state, then all the diamonds to be annealed are subjected to slicing treatment and second annealing treatment to obtain a plurality of second target single crystal diamonds, specifically comprising: If the diamond rough states of all the diamonds to be annealed are all in the finished rough state, all the diamonds to be annealed are sliced ​​to obtain a plurality of sliced ​​diamonds to be annealed, wherein the slicing process refers to cutting off edge polycrystals on all the diamonds to be annealed; Placing all the sliced ​​diamonds to be annealed on the target molybdenum sheet with the growth surface facing upward, and placing the target molybdenum sheet carrying all the sliced ​​diamonds to be annealed into the reaction chamber of the MPCVD device; Performing a second temperature increase treatment on all the sliced ​​diamonds to be annealed according to the preset temperature increase environment to obtain a plurality of initial sliced ​​diamonds to be annealed; After the second temperature rising treatment is completed, a second temperature falling treatment is performed on all the initially sliced ​​diamonds to be annealed according to the preset temperature falling environment to obtain a plurality of second target single crystal diamonds.

6. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 5, characterized in that: The step of performing a second heating treatment on all the sliced ​​diamonds to be annealed according to the preset heating environment to obtain a plurality of initial sliced ​​diamonds to be annealed specifically includes: Acquiring the second current crystal surface temperature of all the sliced ​​diamonds to be annealed, and raising the second current crystal surface temperature of all the sliced ​​diamonds to be annealed to the first preset crystal surface temperature within the first preset time range according to the preset temperature rising environment, and making all the sliced ​​diamonds to be annealed maintain the first preset crystal surface temperature; When the holding time of the first preset crystal surface temperature reaches a third preset time range, it indicates that the second temperature rise treatment of all the sliced ​​diamonds to be annealed is completed, and a plurality of initial sliced ​​diamonds to be annealed are obtained.

7. The low-pressure and low-temperature single crystal diamond batch annealing method according to claim 5, characterized in that: After the second temperature rise treatment is completed, a second temperature drop treatment is performed on all the initial sliced ​​diamonds to be annealed according to the preset temperature drop environment to obtain a plurality of second target single crystal diamonds, specifically including: After the second temperature increase treatment of all the sliced ​​diamonds to be annealed is completed, the first preset crystal surface temperature of all the initial sliced ​​diamonds to be annealed is reduced to the second preset crystal surface temperature within a fourth preset time range according to the preset temperature reduction environment; When the second temperature reduction treatment of all the initially sliced ​​diamonds to be annealed is completed, a plurality of second target single crystal diamonds are obtained.

8. A low-pressure and low-temperature single crystal diamond batch annealing system, characterized in that: The low-pressure and low-temperature single crystal diamond batch annealing system comprises: A diamond blank state acquisition module, used for determining a plurality of diamonds to be annealed, and acquiring the diamond blank states of the plurality of diamonds to be annealed, wherein the diamond blank states include semi-finished blank states and finished blank states; A first annealing treatment module, for performing a first annealing treatment on all the diamonds to be annealed if the diamond blank states of all the diamonds to be annealed are all in the semi-finished blank state, so as to obtain a plurality of first target single crystal diamonds; The second annealing treatment module is used for performing slicing treatment and second annealing treatment on all the diamonds to be annealed if the diamond blank states of all the diamonds to be annealed are all in the finished blank state, so as to obtain a plurality of second target single crystal diamonds.

9. A terminal, characterized in that: The terminal comprises: a memory, a processor, and a low-pressure and low-temperature single crystal diamond batch annealing program stored in the memory and executable on the processor. When the low-pressure and low-temperature single crystal diamond batch annealing program is executed by the processor, the steps of the low-pressure and low-temperature single crystal diamond batch annealing method according to any one of claims 1 to 7 are implemented.

10. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores a low-pressure and low-temperature single crystal diamond batch annealing program, which, when executed by a processor, implements the steps of the low-pressure and low-temperature single crystal diamond batch annealing method according to any one of claims 1 to 7.

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