Laser irradiation in-situ annealing crystal growing furnace and use method thereof
By laser radiation in situ annealing of the crystal growth furnace, the problems of low crystal quality and multi-step process error superposition in the existing technology are solved, and laser radiation annealing is realized during crystal growth, improving the quality and yield of the crystal .
Patent Information
- Application Number
- CN202411380992.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2024-12-27
AI Technical Summary
In the existing crystal growth technology, due to the low purity of raw materials and poor temperature field stability, the crystal crystal quality and poor performance are low, and the multi-step process reduces the crystal growth efficiency and increases the mass error, and reduces the yield rate.
Laser irradiation in situ annealing crystal growth furnace is used to combine the heating furnace and linear drive assembly with laser assembly to achieve laser irradiation annealing during crystal growth, eliminating inclusion phases, alleviating high-temperature stress, and improving crystal quality.
During the crystal growth process, laser radiation annealing is performed simultaneously, which improves the quality of the crystal, reduces defects and enhances the yield.
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Figure CN119194585A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of crystal growth, and in particular to a laser irradiation in-situ annealing crystal growth furnace and a use method thereof. Background Art
[0002] At present, in the process of growing single crystals, thin films, high-quality polycrystals, and polycrystal purified crystals using crystal growth furnaces, low crystal quality and poor performance often occur due to low raw material purity and poor temperature field stability. At the same time, these grown crystals often require further processing to meet usage requirements, such as annealing, irradiation modification, quenching, and raw material purification.
[0003] That is, the existing multi-step process not only reduces the crystal growth efficiency, but also causes the quality errors of each step to accumulate, thereby reducing the yield rate.
[0004] Therefore, it is necessary to provide a laser irradiation in-situ annealing crystal growth furnace and a method of using the same to solve the above problems. Summary of the invention
[0005] The present invention provides a laser irradiation in-situ annealing crystal growth furnace and a use method thereof, so as to solve the problem that the existing multi-step process not only reduces the crystal growth efficiency, but also causes the quality error of each step to be superimposed, thereby reducing the yield.
[0006] A laser irradiation in-situ annealing crystal growth furnace of the present invention adopts the following technical scheme, including: The heating furnace is erected on a supporting base; A linear drive assembly is arranged at one side of the heating furnace, and its output end is inserted into the cavity of the heating furnace and is used to connect to a clamping assembly for clamping a crystal growth container; And a laser assembly is arranged on one side of the heating furnace, and the laser output by the laser assembly is irradiated on the crystal growth container in the heating furnace cavity through the through hole on the heating furnace.
[0007] Preferably, the laser assembly comprises: a shell, in which a slide rail is slidably connected, a laser is arranged on the slide rail, the laser and the through hole on the heating furnace are concentrically arranged, and a pointer is connected to the laser, and the pointer passes through a long slot arranged on the shell.
[0008] Preferably, scales are provided on both sides of the long slot.
[0009] Preferably, the irradiation wavelength range of the laser is 100nm to 11um, and the output power of the laser is less than 1mW.
[0010] Preferably, the setting direction of the heating furnace is consistent with the growth direction of the growing crystal.
[0011] Preferably, when the heating furnace is arranged horizontally, the clamping assembly is slidably arranged in the cavity of the heating furnace.
[0012] Preferably, it is characterized in that when the heating furnace is horizontally arranged, one end of the crystal growth container passes through the heating furnace through a first connecting rod, wherein the clamping assembly clamps the end of the first connecting rod passing through the heating furnace, and the clamping assembly is connected to the output end of the linear drive assembly through a second connecting rod, the driving direction of the linear drive assembly is parallel to the first connecting rod, and the output end of the linear drive assembly is connected to the first connecting rod through the second connecting rod.
[0013] Preferably, the linear drive assembly adopts a linear motor.
[0014] A method for using a laser irradiation in-situ annealing crystal growth furnace, comprising: Placing the growing crystal in a crystal growth container, and controlling the temperature of the heating furnace to melt the desired growing crystal; Control the moving direction and speed of the crystal growth container to control the growth direction and growth speed of the crystal; At the same time, the laser is turned on, the parameters and position of the laser are set, and the laser is irradiated to the growing crystal to anneal the crystal.
[0015] Preferably, the position of the laser is adjusted by turning the pointer to ensure that the irradiation range of the laser covers the entire cross section of the growing crystal.
[0016] The beneficial effects of the present invention are: The crystal growth furnace of the present invention can perform laser irradiation annealing simultaneously during the crystal growth process, that is, the atoms of the crystal have different chemical activities under the high temperature field just after solidification and crystallization than under normal temperature. At this time, adding laser irradiation during the growth process can eliminate the inclusion phase, relieve high temperature stress, reduce crystal defects, and thus improve the quality of the obtained crystal. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0018] Figure 1 It is a schematic diagram of the overall structure of a laser irradiation in-situ annealing crystal growth furnace embodiment 1 of the present invention; Figure 2 It is a schematic diagram of the overall structure of a laser irradiation in-situ annealing crystal growth furnace embodiment 2 of the present invention; Figure 3It is a schematic diagram of the overall structure of a laser irradiation in-situ annealing crystal growth furnace embodiment 3 of the present invention; Figure 4 This is a crystal that has not been subjected to laser in-situ annealing; Figure 5 This is a crystal after laser in-situ annealing; Figure 6 This is the precipitation of impurities at the tail of the crystal after laser in-situ annealing.
[0019] In the figure: 1. Heating furnace; 2. Laser; 3. Linear motor; 4. Control cabinet; 5. Slide rail; 6. Shell; 7. Long slot; 8. Pointer; 9. Support base; 10. Clamping assembly; 11. Crystal growth container. DETAILED DESCRIPTION
[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0021] Example 1 The present invention discloses a laser irradiation in-situ annealing crystal growth furnace, comprising: a heating furnace 1, a linear drive assembly, a control cabinet 4 and a laser assembly, wherein Figure 1 As shown, the heating furnace 1 of this embodiment 1 is arranged horizontally. Figure 1 The horizontal furnace shown in the figure; the heating furnace 1 is mounted on the supporting base 9; the linear drive component is arranged on one side of the heating furnace 1, and the output end of the linear drive component is inserted into the cavity of the heating furnace 1 to connect to the clamping component 10 for clamping the crystal growth container 11, wherein the linear drive component adopts a linear motor 3; the laser component is arranged on one side of the heating furnace 1, and the laser output by the laser component is irradiated on the crystal growth container 11 in the cavity of the heating furnace 1 through the through hole on the heating furnace 1, wherein the heating temperature of the heating furnace 1, the switch and parameters of the laser component, and the switch of the linear drive component are all controlled by the control cabinet 4 Control, in this embodiment 1, the laser assembly includes: a shell 6 installed on the outer wall of the furnace at the through hole of the heating furnace 1, a slide rail 5 is slidably connected in the shell 6, a laser 2 is arranged on the slide rail 5, the laser 2 and the through hole on the heating furnace 1 are concentrically arranged, a pointer 8 is connected to the laser 2, the pointer 8 passes through the long slot 7 set on the shell 6, and scales are set on the shell 6 on both sides of the long slot 7; the control line at the tail of the laser 2 extends from the line outlet to connect to the control cabinet 4; by pushing the pointer 8 at the tail of the laser 2 and observing the scale at the long slot 7 at the same time, the position of the laser 2 deep into the through hole can be adjusted.
[0022] Specifically, the laser 2 is aimed at the solid phase side of the solid-liquid interface of the growing crystal.
[0023] Specifically, the irradiation wavelength range of laser 2 is 100nm to 11um, the output power of laser 2 is less than 1mW, and the irradiation diameter of laser 2 is 1mm-30mm. In this embodiment, the irradiation wavelength of laser 2 is 10um, the output power of laser 2 is 0.5mW, and the irradiation diameter of laser 2 is 15mm.
[0024] Specifically, the setting direction of the heating furnace 1 is consistent with the growth direction of the growing crystal.
[0025] Example 2 In this embodiment 2, compared with the embodiment 1, the difference is that the heating furnace 1 is vertically arranged to form Figure 2 In the plumb vertical furnace shown in the embodiment 2, one end of the crystal growth container 11 passes through the top of the heating furnace 1 through the first connecting rod and is clamped on the clamping assembly 10, that is, the clamping assembly 10 clamps the end of the first connecting rod passing through the heating furnace 1, and the clamping assembly 10 is connected to the output end of the linear drive assembly through the second connecting rod, the driving direction of the linear drive assembly is vertically upward, and the driving direction of the linear drive assembly is parallel to the first connecting rod, and the output end of the linear drive assembly is connected to the first connecting rod through the second connecting rod. Specifically, the linear drive assembly adopts a linear motor 3.
[0026] Example 3 In this embodiment 3, compared with embodiment 2, the difference is that in this embodiment 3, one end of the crystal growth container 11 passes through the bottom of the heating furnace 1 through the first connecting rod and is clamped on the clamping assembly 10, that is, the clamping assembly 10 clamps the end of the first connecting rod passing through the heating furnace 1, and the clamping assembly 10 is connected to the output end of the linear drive assembly through the second connecting rod, the driving direction of the linear drive assembly is vertically downward, the driving direction of the linear drive assembly is parallel to the first connecting rod, and the output end of the linear drive assembly is connected to the first connecting rod through the second connecting rod. Specifically, the linear drive assembly adopts a linear motor 3.
[0027] A method for using a laser irradiation in-situ annealing crystal growth furnace, comprising: Controlling the temperature of the heating furnace 1 to melt the desired growth crystal; Controlling the moving direction and speed of the crystal growth container 11 to control the growth direction and growth speed of the crystal; At the same time, turn on laser 2, set the parameters and position of laser 2, and irradiate the growing crystal with laser light to anneal the crystal.
[0028] Specifically, the position of the laser 2 in the through hole is adjusted by turning the pointer 8, and the position of the laser 2 can be accurately adjusted by observing the scales on both sides of the slot to ensure that the irradiation range of the laser 2 covers the entire cross section of the growing crystal.
[0029] How it works The crystal growth container 11 is fixed by the sample clamping assembly 11 and sent into the chamber of the heating furnace 1 through the linear motor 3. According to the type of crystal to be grown, the temperature of the heating furnace 1 is controlled to melt the crystal (raw material) to be grown, and a temperature field is formed in the heating furnace 1. The linear motor 3 is used to control the movement of the clamping assembly 11 to control the growth direction and growth speed of the crystal. At the beginning of growth, the laser 2 is turned on, the appropriate parameters of the laser 2 are set, and the pointer 8 is turned to adjust the position of the laser 2 to ensure that the irradiation range of the laser 2 covers the entire cross-section of the crystal, and to ensure that the power of the laser 2 is not too high to melt the crystal. The laser 2 is aimed at the solid phase side of the solid-liquid interface of the crystal, which has the effect of eliminating metastable inclusion phases at high temperatures, surface passivation, stress relief, and irradiation modification; the laser 2 is aimed at the liquid phase side of the solid-liquid interface of the crystal, which has the effect of eliminating tiny crystal nuclei in the liquid phase and refining the grains. Except for the clamping assembly 11 and the dial pointer, all adjustment and control operations are controlled by the operator operating the control cabinet 4.
[0030] like Figure 4 This is the crystal growth result of single crystal Cs3Bi2Br9 without laser irradiation. The overall color of the crystal is dark green due to the presence of impurities. High-quality single crystal Cs3Bi2Br9 is bright yellow. When the crystal is melted for secondary growth, a low-power laser 2 is used to continuously irradiate the crystal growth site, such as Figure 4 After laser in-situ annealing, the crystal returns to a pale yellow color, and the following can be seen at the tail of the crystal: Figure 6 The area where impurities accumulate.
[0031] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A laser irradiation in-situ annealing crystal growth furnace, characterized in that: include: The heating furnace is erected on a supporting base; A linear drive assembly is arranged at one side of the heating furnace, and its output end is inserted into the cavity of the heating furnace and is used to connect to a clamping assembly for clamping a crystal growth container; And a laser assembly is arranged on one side of the heating furnace, and the laser output by the laser assembly is irradiated on the crystal growth container in the heating furnace cavity through the through hole on the heating furnace.
2. The laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: The laser assembly comprises: a shell, a slide rail is slidably connected inside the shell, a laser is arranged on the slide rail, the laser and the through hole on the heating furnace are concentrically arranged, a pointer is connected to the laser, and the pointer passes through a long slot arranged on the shell.
3. The laser irradiation in-situ annealing crystal growth furnace according to claim 2, characterized in that: Scales are arranged on both sides of the long slot.
4. The laser irradiation in-situ annealing crystal growth furnace according to claim 2, characterized in that: The irradiation wavelength range of the laser is from 100nm to 11um, and the output power of the laser is less than 1mW.
5. The laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: The setting direction of the heating furnace is consistent with the growth direction of the growing crystal.
6. The laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: When the heating furnace is arranged horizontally, the clamping assembly is slidably arranged in the cavity of the heating furnace.
7. The laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: When the heating furnace is set horizontally, one end of the crystal growth container passes through the heating furnace through the first connecting rod, wherein the clamping assembly clamps the end of the first connecting rod passing through the heating furnace, and the clamping assembly is connected to the output end of the linear drive assembly through the second connecting rod, the driving direction of the linear drive assembly is parallel to the first connecting rod, and the output end of the linear drive assembly is connected to the first connecting rod through the second connecting rod.
8. The laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: The linear drive assembly uses a linear motor.
9. A method for using a laser irradiation in-situ annealing crystal growth furnace, characterized in that: include: Placing the growing crystal in a crystal growth container, and controlling the temperature of the heating furnace to melt the desired growing crystal; Control the moving direction and speed of the crystal growth container to control the growth direction and growth speed of the crystal; At the same time, the laser is turned on, the parameters and position of the laser are set, and the laser is irradiated to the growing crystal to anneal the crystal.
10. The method for using a laser irradiation in-situ annealing crystal growth furnace according to claim 1, characterized in that: The laser position is adjusted by turning the pointer to ensure that the laser irradiation range covers the entire cross-section of the growing crystal.
