Tail-section single crystal forming method, crystal pulling equipment and computer storage medium

Abstract

The invention belongs to the technical field of single crystal production, and relates to a tail-section single crystal forming method which comprises the following steps: in a seeding process, setting the crucible rotation of a crucible to be 9-10r / min, and setting the crystal rotation to be 10-10.5 r / min; in the last stage of the shouldering process, the crucible rotation of the crucible is set to be 6-8 r / min, and the crystal rotation is set to be 8.5-9 r / min. The method has the beneficial effects that by continuously adjusting crucible rotation and crystal rotation in the existing technological process and argon flow and furnace pressure in the equal-diameter process, the effective working hour utilization rate of single crystal production is increased, the purposes of reducing cost and increasing efficiency are achieved, meanwhile, a thermal field is protected against loss, production safety is guaranteed, the one-time crystallization rate of single crystals is increased by 8%, and the production cost is reduced. And the bract breaking and material pulling weight is reduced by 41.6%.

Description

Technical Field

[0001] The invention belongs to the technical field of single crystal production, and relates to a tail-end single crystal crystallization method, equipment and computer storage medium. Background Art

[0002] At present, the single crystal pulling process is prone to breakage when pulling the last single crystal. Once breakage occurs, the pulling process will be executed. Since the pulled single crystal can only be returned, this will affect the qualification rate and production capacity of the single crystal. At the same time, the pulled single crystal is very easy to break, so multiple pulling is required, which will affect the effective working time utilization rate of the single crystal. At the same time, the pulled single crystal may fall, causing heat field loss and production safety. Therefore, a tail-end single crystal crystallization method, crystal pulling equipment and computer storage medium are needed to solve the above technical problems. Summary of the invention

[0003] In order to solve the above-mentioned technical problems, the present invention provides a tail-end single crystal crystallization method, crystal pulling equipment and computer storage medium, which can save the waste of labor time caused by breaking the bud and pulling the material, and achieve the economic benefits of increasing production and reducing costs.

[0004] The technical solution adopted by the present invention is: a tail-end single crystal crystallization method, characterized in that it includes the following steps:

[0005] In the seeding process, the crucible rotation is set at 9-10 r / min, and the crystal rotation is set at 10-10.5 r / min;

[0006] At the end of the shoulder release process, the crucible rotation is set to 6-8 r / min, and the crystal rotation is set to 8.5-9 r / min.

[0007] Furthermore, in the early stage of the shoulder release process, the crucible rotation speed is set to 8.5-9.5 r / min, and the crystal rotation speed is set to 9.5-10.5 r / min.

[0008] Furthermore, in the early stage of the shoulder release process, the crucible rotation speed is set to 9 r / min, and the crystal rotation speed is set to 10 r / min.

[0009] Furthermore, in the temperature stabilization process before the seeding process, the crucible rotation speed is set to 8-10 r / min, and the crystal rotation speed is set to 9.5-10.5 r / min.

[0010] Furthermore, in the initial stage of the equal diameter process after the shoulder release process, the crucible rotation speed is set to 8-9 r / min, and the crystal rotation speed is set to 10 r / min.

[0011] Furthermore, the crystal rotation speed is gradually reduced by 1 to 3 r / min.

[0012] Furthermore, during the equal diameter process, the argon flow rate is set to 68-70 slpm.

[0013] Furthermore, during the equal diameter process, the furnace pressure is set to 21 to 24 torr.

[0014] A crystal pulling device, characterized in that it includes a processor and a communication interface, wherein the communication interface is coupled to the processor, and the processor is used to run a computer program or instruction to implement the tail-end single crystal crystallization method as described above.

[0015] A computer storage medium, characterized in that instructions are stored in the computer storage medium, and when the instructions are executed, the tail-end single crystal crystallization method as described above is implemented.

[0016] The present invention relates to a tail-end single crystal crystallization method. In the method, by continuously adjusting the crucible rotation and crystal rotation in the existing process flow, as well as the argon gas flow rate and furnace pressure in the equal-diameter process, the effective working time utilization rate of single crystal production is improved, and the purpose of reducing costs and increasing efficiency is achieved. At the same time, the heat field is protected from loss and production safety is guaranteed, so that the single crystal one-time crystallization rate is increased by 8%, and the weight of the broken bud pulled material is reduced by 41.6%:

[0017] (1) Increase the crucible rotation and crystal rotation in the temperature stabilization process to stabilize the temperature and ensure the stability and accuracy of the seeding power;

[0018] (2) Increase the crucible rotation and crystal rotation during the seeding process to ensure that the seeding process eliminates single crystal growth dislocations and temperature stability to reduce the waste of work time caused by seeding breakage and seeding failure;

[0019] (3) Maintain the crucible rotation and crystal rotation in the early stage of the shoulder release process, reduce the crucible rotation and crystal rotation in the late stage of the shoulder release process, ensure the stability of cooling during the growth of the single crystal shoulder release, facilitate crystallization, and ensure the quality stability of the oxygen content;

[0020] (4) Increase the crucible rotation in the early stage of the equal-diameter process to ensure the longitudinal temperature gradient of the single crystal growth, and gradually reduce the crystal rotation to ensure the stability of the single crystal rotation speed in the final stage; at the same time, slowly increase the argon gas flow rate and furnace pressure during the equal-diameter process to purify impurities and suppress liquid surface vibration at the end of crystal pulling, so as to reduce the single crystal breakage and improve crystal formation. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a flow chart of an embodiment provided by the present invention. DETAILED DESCRIPTION

[0022] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. Figure 1 As shown, this process flow mainly includes four processes: temperature stabilization, crystal induction, shoulder release and equal diameter.

[0023] In a first aspect, the present invention provides a tail-end single crystal crystallization method, characterized in that it comprises the following steps:

[0024] In the seeding process, the crucible rotation is set at 9-10 r / min, and the crystal rotation is set at 10-10.5 r / min;

[0025] At the end of the shoulder release process, the crucible rotation is set to 6-8 r / min, and the crystal rotation is set to 8.5-9 r / min.

[0026] Preferably, in the early stage of the shoulder release process, the crucible rotation speed is set to 8.5-9.5 r / min, and the crystal rotation speed is set to 9.5-10.5 r / min.

[0027] Preferably, in the early stage of the shoulder release process, the crucible rotation speed is set to 9 r / min and the crystal rotation speed is set to 10 r / min.

[0028] Preferably, in the temperature stabilization process before the seeding process, the crucible rotation speed is set to 8-10 r / min, and the crystal rotation speed is set to 9.5-10.5 r / min.

[0029] Preferably, in the initial stage of the equal diameter process after the shoulder release process, the crucible rotation speed is set to 8-9 r / min, and the crystal rotation speed is set to 10 r / min.

[0030] Preferably, the crystal rotation rate is gradually reduced by 1 to 3 r / min.

[0031] Preferably, during the equal diameter process, the argon flow rate is set to 68-70 slpm.

[0032] Preferably, during the equal diameter process, the furnace pressure is set to 21 to 24 torr.

[0033] Embodiment 1:

[0034] During the temperature stabilization process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0035] During the seeding process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0036] During the shoulder release process, the crucible rotation was set at 9 r / min and the crystal rotation was set at 10 r / min;

[0037] At the initial stage of the equal-diameter process, the crucible rotation was set to 7 r / min, the crystal rotation was set to 10 r / min, the argon flow rate was set to 60 slpm, and the furnace pressure was set to 9 torr.

[0038] Embodiment 2:

[0039] Compared with Example 1, in Example 2, the crucible rotation in the temperature stabilization process is increased by 1-3r / min to 8-10r / min, and the crystal rotation is increased by 0.5-1.5r / min to 9.5-10.5r / min. Compared with the technical effect of Example 1, the technical solution of Example 2 reduces the weight of the broken husk pulling material by 5.0%.

[0040] During the temperature stabilization process, the crucible rotation is set at 8-10 r / min and the crystal rotation is set at 9.5-10.5 r / min;

[0041] During the seeding process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0042] During the shoulder release process, the crucible rotation was set at 9 r / min and the crystal rotation was set at 10 r / min;

[0043] At the initial stage of the equal-diameter process, the crucible rotation was set to 7 r / min, the crystal rotation was set to 10 r / min, the argon flow rate was set to 60 slpm, and the furnace pressure was set to 9 torr.

[0044] Embodiment three:

[0045] Compared with Example 1, in Example 3, the crucible rotation in the seeding process is increased by 2-3 r / min to 9-10 r / min, and the crystal rotation is increased by 1-1.5 r / min to 10-10.5 r / min. Compared with the technical effect of Example 1, the technical solution of Example 3 reduces the weight of the broken hulled material by 3.0%.

[0046] During the temperature stabilization process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0047] During the seeding process, the crucible rotation is set at 9-10 r / min and the crystal rotation is set at 10-10.5 r / min;

[0048] During the shoulder release process, the crucible rotation was set at 9 r / min and the crystal rotation was set at 10 r / min;

[0049] At the initial stage of the equal-diameter process, the crucible rotation was set to 7 r / min, the crystal rotation was set to 10 r / min, the argon flow rate was set to 60 slpm, and the furnace pressure was set to 9 torr.

[0050] Embodiment 4:

[0051] Compared with Example 1, in Example 4, the crucible rotation at the end of the shoulder release process is reduced by 1-3r / min to 6-8r / min, and the crystal rotation is reduced by 1-1.5r / min to 8.5-9r / min. Compared with the technical effect of Example 1, the technical solution of Example 4 reduces the weight of the broken husk pulling material by 12.0%.

[0052] During the temperature stabilization process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0053] During the seeding process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0054] At the end of the shoulder release process, the crucible rotation is set to 6-8 r / min and the crystal rotation is set to 8.5-9 r / min;

[0055] At the initial stage of the equal-diameter process, the crucible rotation was set to 7 r / min, the crystal rotation was set to 10 r / min, the argon flow rate was set to 60 slpm, and the furnace pressure was set to 9 torr.

[0056] Embodiment five:

[0057] Compared with Example 1, in Example 4, the crucible rotation speed at the initial stage of the equal diameter process is increased by 1-2 r / min to 8-9 r / min, and the interval of 200-500 mm is set according to the equal diameter length. The crystal rotation speed is gradually reduced by 1-3 r / min to 7-9 r / min at the initial stage of the equal diameter process, the argon gas flow rate is increased by 8-10 to 68-70 slpm, and the furnace pressure is increased by 12-15 torr to 21-24 torr. Compared with the technical effect of Example 1, the technical solution of Example 5 reduces the weight of the broken hulled material by 21.6%.

[0058] During the temperature stabilization process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0059] During the seeding process, the crucible rotation was set at 7 r / min and the crystal rotation was set at 9 r / min;

[0060] During the shoulder release process, the crucible rotation was set at 9 r / min and the crystal rotation was set at 10 r / min;

[0061] In the initial stage of the equal-diameter process, the crucible rotation is set to 8-9 r / min, the crystal rotation is set to 7-9 r / min, the argon flow rate is set to 68-70 slpm, and the furnace pressure is set to 12-15.

[0062] Embodiment six:

[0063] Compared with Examples 1 to 5, this embodiment adjusts the crucible rotation and crystal rotation in the four processes of temperature stabilization, seeding, shoulder release and equal diameter, and adjusts the argon flow rate and furnace pressure in the equal diameter process. Compared with the technical effects of Examples 1 to 5, the technical solution of Example 6 reduces the weight of the broken bud pull by 41.6%, and at the same time increases the single crystal crystallization rate by 8% compared with Example 1.

[0064] A tail-end single crystal crystallization method, characterized in that it comprises the following steps:

[0065] In the seeding process, the crucible rotation is set at 9-10 r / min, and the crystal rotation is set at 10-10.5 r / min;

[0066] At the end of the shoulder release process, the crucible rotation is set to 6-8 r / min, and the crystal rotation is set to 8.5-9 r / min.

[0067] In the early stage of the shoulder release process, the crucible rotation is set to 8.5-9.5 r / min, and the crystal rotation is set to 9.5-10.5 r / min.

[0068] In the early stage of the shoulder release process, the crucible rotation is set to 9r / min and the crystal rotation is set to 10r / min.

[0069] In the temperature stabilization process before the seeding process, the crucible rotation is set to 8-10 r / min, and the crystal rotation is set to 9.5-10.5 r / min.

[0070] In the initial stage of the equal diameter process after the shoulder release process, the crucible rotation is set to 8-9 r / min and the crystal rotation is set to 10 r / min.

[0071] Gradually reduce the crystal rotation speed by 1 to 3 r / min.

[0072] During the equal-diameter process, the argon flow rate was set at 68-70 slpm.

[0073] During the equal-diameter process, the furnace pressure is set at 21 to 24 torr.

[0074] A crystal pulling device, characterized in that it includes a processor and a communication interface, wherein the communication interface is coupled to the processor, and the processor is used to run a computer program or instruction to implement the tail-end single crystal crystallization method as described above.

[0075] A computer storage medium, characterized in that instructions are stored in the computer storage medium, and when the instructions are executed, the tail-end single crystal crystallization method as described above is implemented.

[0076] In a second aspect, the present invention provides a crystal pulling device, using the above-mentioned tail-end single crystal crystallization method, which includes a processor and a communication interface, the communication interface is coupled to the processor, and the processor is used to run a computer program or instruction to implement the above-mentioned tail-end single crystal crystallization method. In this embodiment, the above-mentioned processor is a central processing unit or an integrated circuit for controlling the execution of the program of the technical solution, and the communication interface can be a transceiver device capable of communicating with other devices or communication networks, so that the signal can transmit information between the crystal pulling devices.

[0077] Preferably, the device further comprises a memory for executing the computer instructions of the technical solution, and the execution is controlled by a processor. The processor is used to execute the computer instructions stored in the memory.

[0078] In a third aspect, the present invention provides a computer storage medium, characterized in that the computer storage medium stores instructions, and when the instructions are executed, the above-mentioned tail-end single crystal crystallization method is implemented. The computer readable storage medium stores instructions, and when the instructions are executed, the functions performed by the crystal pulling device in the above-mentioned embodiment are implemented.

[0079] The beneficial effects of the second aspect, the third aspect and various implementations thereof in the present invention are the same as the beneficial effects of the first aspect or any possible implementation of the first aspect, and are not described in detail herein. In the above embodiments, they can be implemented in whole or in part by software, hardware, firmware or any combination thereof. When implemented by software, they can be implemented in whole or in part in the form of a computer program product.

[0080] The present invention relates to a tail-end single crystal crystallization method. In the method, by continuously adjusting the crucible rotation and crystal rotation in the existing process flow, as well as the argon gas flow rate and furnace pressure in the equal-diameter process, the effective working time utilization rate of single crystal production is improved, and the purpose of reducing costs and increasing efficiency is achieved. At the same time, the heat field is protected from loss and production safety is guaranteed, so that the single crystal one-time crystallization rate is increased by 8%, and the weight of the broken bud pulled material is reduced by 41.6%:

[0081] (1) Increase the crucible rotation and crystal rotation in the temperature stabilization process to stabilize the temperature and ensure the stability and accuracy of the seeding power;

[0082] (2) Increase the crucible rotation and crystal rotation during the seeding process to ensure that the seeding process eliminates single crystal growth dislocations and temperature stability to reduce the waste of work time caused by seeding breakage and seeding failure;

[0083] (3) Maintain the crucible rotation and crystal rotation in the early stage of the shoulder release process, reduce the crucible rotation and crystal rotation in the late stage of the shoulder release process, ensure the stability of cooling during the growth of the single crystal shoulder release, facilitate crystallization, and ensure the quality stability of the oxygen content;

[0084] (4) Increase the crucible rotation in the early stage of the equal-diameter process to ensure the longitudinal temperature gradient of the single crystal growth, and gradually reduce the crystal rotation to ensure the stability of the single crystal rotation speed in the final stage; at the same time, slowly increase the argon gas flow rate and furnace pressure during the equal-diameter process to purify impurities and suppress liquid surface vibration at the end of crystal pulling, so as to reduce the single crystal breakage and improve crystal formation.

[0085] The embodiments of the present invention are described in detail above, but the contents described are only preferred embodiments of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made according to the scope of application of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A tail-end single crystal crystallization method, characterized in that: The steps include: In the seeding process, the crucible rotation is set at 9-10 r / min, and the crystal rotation is set at 10-10.5 r / min; At the end of the shoulder release process, the crucible rotation is set to 6-8 r / min, and the crystal rotation is set to 8.5-9 r / min.

2. The tail-end single crystal crystallization method according to claim 1, characterized in that: In the early stage of the shoulder release process, the crucible rotation is set to 8.5-9.5 r / min, and the crystal rotation is set to 9.5-10.5 r / min.

3. The tail-end single crystal crystallization method according to claim 2, characterized in that: In the early stage of the shoulder release process, the crucible rotation is set to 9 r / min and the crystal rotation is set to 10 r / min.

4. The tail-end single crystal forming method according to claim 1, characterized in that: In the temperature stabilization process before the seeding process, the crucible rotation is set to 8-10 r / min, and the crystal rotation is set to 9.5-10.5 r / min.

5. The tail-end single crystal forming method according to claim 4, characterized in that: In the initial stage of the equal diameter process after the shoulder release process, the crucible rotation is set to 8-9 r / min, and the crystal rotation is set to 10 r / min.

6. The tail-end single crystal forming method according to claim 5, characterized in that: The crystal rotation speed is gradually reduced by 1 to 3 r / min.

7. The tail-end single crystal forming method according to claim 6, characterized in that: During the equal diameter process, the argon gas flow rate is set to 68-70 slpm.

8. The tail-end single crystal forming method according to claim 7, characterized in that: During the equal diameter process, the furnace pressure is set at 21 to 24 torr.

9. A crystal pulling device, characterized in that: It comprises a processor and a communication interface, wherein the communication interface is coupled to the processor, and the processor is used to run a computer program or instruction to implement the tail-end single crystal crystallization method according to any one of claims 1-8.

10. A computer storage medium, characterized in that: The computer storage medium stores instructions, and when the instructions are executed, the tail-end single crystal crystallization method according to any one of claims 1 to 8 is implemented.

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