Device for preparing and transferring crystal solution

Abstract

The invention discloses a device for preparing and transferring a crystal solution, the device is composed of a heating device, a rotating device and a transferring device, the heating device comprises a heating coil, deionized water and a control system; the rotating device comprises a fixed table, a rotating bottle, a rotating motor and a connecting rod; the transfer device comprises a filter element, a silicone tube and a peristaltic pump; a silicone tube extends below the liquid level of the rotary bottle and is connected with an outlet and an inlet of the filter element, a peristaltic pump is used for providing power, and the prepared guanidine tetrafluoroborate solution enters the growth tank through the filter element. Impurities in the solution can be effectively reduced, the probability of secondary nucleation of the solution is reduced, and the success rate of crystal growth is effectively improved. According to the device, impurities in the solution can be effectively removed, the probability of secondary nucleation of crystals is reduced, and the success rate of crystal growth is effectively improved.

Description

Technical Field

[0001] The invention belongs to the technical field of crystal growth, and in particular relates to a device for preparing a crystal solution and transferring it. Background Art

[0002] Guanidine tetrafluoroborate (GFB) is a full-band phase-matched nonlinear optical crystal with a UV cutoff edge of 193 nm. Based on the phase-matching device, the GFB crystal has achieved 193.2-266 nm UV / deep UV tunable laser output and has direct frequency doubling output capability in the entire transmission range. Guanidine tetrafluoroborate (GFB) crystal has excellent linear and nonlinear optical properties, a short UV cutoff edge of -193 nm, and a large effective frequency doubling coefficient. d eff = 1.42 pm / V, short phase matching wavelength -194 nm and high laser damage threshold >BBO@ 266 / 532 nm, 8 ns, 10 Hz, etc. It is a promising nonlinear optical crystal material for 266 nm lasers and is also a nonlinear optical crystal that is expected to replace KDP crystals for laser confinement fusion devices. Therefore, the research on crystal growth and processing technology of guanidine tetrafluoroborate (GFB) needs to make continuous progress.

[0003] The current method for growing guanidine tetrafluoroborate (GFB) crystals is to grow rapidly through aqueous solution. Impurities are easily introduced during the preparation and transfer of guanidine tetrafluoroborate (GFB) solution, and these impurities directly affect the quality of guanidine tetrafluoroborate (GFB) crystal growth. The presence of impurities in the solution will trigger secondary nucleation, making it easy for guanidine tetrafluoroborate (GFB) crystals to grow additional crystals, impurity crystals and other crystal defects at new crystal nuclei during growth, and even lead to crystal growth failure. Therefore, how to effectively remove impurities during solution preparation and transfer is a problem that needs to be solved. Summary of the invention

[0004] The object of the present invention is to provide a device for preparing a crystal solution and transferring the impurities in the above-mentioned solution. The device is composed of a heating device, a rotating device, and a transferring device. The heating device includes a heating coil, deionized water, and a control system; the rotating device fixing table, a rotating bottle, a rotating motor, and a connecting rod; the transferring device includes a filter element, a silicone tube, and a peristaltic pump; the silicone tube is extended under the liquid surface of the rotating bottle, the outlet and the inlet of the filter element are connected with the silicone tube, and the peristaltic pump is used to provide power to pass the prepared guanidine tetrafluoroborate solution through the filter element into the growth tank. It can effectively reduce the impurities in the solution, reduce the probability of secondary nucleation of the solution, and effectively improve the success rate of crystal growth. The device can effectively remove impurities in the solution, reduce the probability of secondary nucleation of the crystal, and effectively improve the success rate of crystal growth.

[0005] The present invention discloses a device for preparing a crystal solution and transferring the crystal solution. The device comprises a heating device, a rotating device and a transferring device. The transferring device comprises a peristaltic pump (1), a filter element (2) and a silicone tube (3). The filter element (2) comprises a rotating device comprising a fixed platform (4), a rotating bottle (5) made of PC material, a rotating motor (6) and a connecting rod (7). The heating device comprises a control system (8) and a water bath system. The water bath system comprises a heating coil (9), a fixing ring (10), a lifting rod (11) and a valve (12). One end of the connecting rod (7) is connected to the rotating bottle (5), and the other end of the connecting rod (7) is connected to the rotating motor (6) and the valve (12). The rotating bottle (5) is located in a water bath (10). The water bath (10) is placed at the upper end of the water bath system (17) and can move up and down. Deionized water is provided in (10), a lifting rod (11) is provided on the water bath system (17), a heating coil (9) is provided on one side of the water bath system (17), a rotating motor (6) is fixed on a fixed platform (4), the fixed platform (4) is connected to a first bracket (14) and a second bracket (15) by clips to form a whole fixed on a base (13), a pressure gauge (18) is fixed to the top of the second bracket (15) by a fixing buckle (16), a control system (8) is fixed to the upper part of the fixed platform (4), and the control system (8) is connected to the heating coil (9) by a connecting line (20); both ends of the filter element (2) are connected to the silicone tube (3) by a clamp (19), one end of the silicone tube (3) is inserted into the rotating bottle (5), and the other end of the silicone tube (3) is connected to the peristaltic pump (1), and the specific operation is performed according to the following steps: a. Put guanidine tetrafluoroborate raw material into a rotating bottle (5), the rotating bottle (5) is placed in a water bath (10), the water bath (10) is placed on the upper end of a water bath system (17), and the height of the water bath (10) is adjusted by a lifting rod (11) on the water bath system (17) so that the rotating bottle (5) is below the liquid surface of deionized water in the water bath (10), the resistivity of the deionized water is 18 MΩ·cm, the control system (8) is turned on, the heating coil (9) is heated to a temperature of 40-70° C., the rotating motor (6) is turned on, the rotating speed is 1-50 r / min, and the valve (12) is closed to prepare the solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped. The silicone tube (3) at one end of the filter element (2) is fixed with a clamp to prevent leakage during the transfer process. The filtration accuracy of the filter element (2) is 0.1-5 μm. The inner diameter of the silicone tube (3) is 8-12 mm, and its outer diameter is 13-17 mm. The peristaltic pump (1) connected to the other end of the silicone tube (3) clamps the silicone tube (3). The peristaltic pump (1) provides power. The rotation speed of the peristaltic pump (1) is 50-100 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element (2) to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, impurities in the guanidine tetrafluoroborate solution will remain in the filter element (2) during the transfer process.

[0006] The crystal solution preparation and transfer device provided by the present invention is suitable for use before the crystal transfer growth device. In the early stage, the filter element and the silicone tube need to be fixed with a clamp to prevent leakage, and the guanidine tetrafluoroborate (GFB) crystal raw material is added to the rotating bottle, and deionized water is added to the water bath system to start rotation and heating. After the raw material is completely dissolved, the silicone tube is inserted under the liquid surface of the rotating bottle, and the outlet and inlet of the filter element are connected with the silicone tube, and the silicone tube is clamped with a peristaltic pump to transfer the crystal solution. The solution is in an unsaturated state, and secondary nucleation will not occur, and the solution can be quickly filtered.

[0007] The device for preparing and transferring a crystal solution according to the present invention can produce the following beneficial effects: When there are a large number of visible impurities in the crystal solution, the stability of the solution will be reduced and the probability of secondary nucleation will be greatly increased. The present invention can effectively reduce the impurities in the solution and the probability of secondary nucleation in the solution in the early stage of crystal growth preparation, thereby effectively improving the success rate of crystal growth. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Figure 1 It is a schematic diagram of the device of the present invention.

[0009] Figure 1 As shown, 1 is a peristaltic pump, 2 is a filter element, 3 is a silicone tube, 4 is a fixed platform, 5 is a rotating bottle, 6 is a rotating motor, 7 is a connecting rod, 8 is a control system, 9 is a heating coil, 10 is a water bath, 11 is a lifting rod, 12 is a valve, 13 is a base, 14 is a left fixed rod, 15 is a right fixed rod, 16 is a fixing buckle, 17 is a water bath system, 18 is a pressure gauge, 19 is a clamp, and 20 is a connecting line. DETAILED DESCRIPTION

[0010] The present invention will be described in detail below with reference to the accompanying drawings. Example 1

[0011] The device for preparing and transferring a crystal solution described in the present invention is composed of a heating device, a rotating device, and a transferring device. The transferring device is composed of a peristaltic pump 1, a filter element 2 and a silicone tube 3. The filter element 2 is composed of a fixed table 4, a rotating bottle 5 made of PC material, a rotating motor 6, and a connecting rod 7; the heating device is composed of a control system 8 and a water bath system; wherein the water bath system includes a heating coil 9, a fixing ring 10, a lifting rod 11 and a valve 12; one end of the connecting rod 7 is connected to the rotating bottle 5, and the other end of the connecting rod 7 is connected to the rotating motor 6 and the valve 12; the rotating bottle 5 is located in a water bath pot 10, and the water bath pot 10 is placed at the upper end of the water bath system 17 and can move up and down , deionized water is provided in the water bath pot 10, a lifting rod 11 is provided on the water bath system 17, a heating coil 9 is provided on one side of the water bath system 17, a rotating motor 6 is fixed on the fixed platform 4, the fixed platform 4 is connected with the first bracket 14 and the second bracket 15 respectively through clips to form an integral fixed on the base 13, the top of the second bracket 15 is fixed with a pressure gauge 18 through a fixing buckle 16, the upper part of the fixed platform 4 is fixed with a control system 8, and the control system 8 is connected with the heating coil 9 through a connecting line 20; both ends of the filter element 2 are connected with the silicone tube 3 through a clamp 19, one end of the silicone tube 3 is inserted into the rotating bottle 5, and the other end of the silicone tube 3 is connected with the peristaltic pump 1, and the specific operation is carried out according to the following steps: a. Put guanidine tetrafluoroborate raw material into rotating bottle 5, rotating bottle 5 is located in water bath 10, water bath 10 is placed on the upper end of water bath system 17, and the lifting rod 11 on water bath system 17 is adjusted to the upper and lower heights of water bath 10, so that rotating bottle 5 is below the liquid surface of deionized water in water bath 10, and the resistivity of deionized water is 18 MΩ·cm, control system 8 is turned on, heating coil 9 is heated to a temperature of 40°C, rotating motor 6 is turned on, the rotating speed is 1r / min, and valve 12 is closed to prepare solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped, and the silicone tube 3 at one end of the filter element 2 is fixed with a clamp 19 to prevent leakage during the transfer process. The filtration accuracy of the filter element 2 is 0.1 μm, the inner diameter of the silicone tube 3 is 8 mm, and the outer diameter is 13 mm. The peristaltic pump 1 connected to the other end of the silicone tube 3 clamps the silicone tube 3, and the peristaltic pump 1 is used to provide power. The rotation speed of the peristaltic pump 1 is 50 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element 2 to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, secondary nucleation will not occur during the transfer process, and impurities in the guanidine tetrafluoroborate solution will remain in the filter element 2. Example 2

[0012] The device is carried out according to Example 1, and the specific operation is carried out according to the following steps: a. Put guanidine tetrafluoroborate raw material into rotating bottle 5, rotating bottle 5 is located in water bath 10, water bath 10 is placed on the upper end of water bath system 17, and the lifting rod 11 on water bath system 17 is adjusted to the upper and lower heights of water bath 10, so that rotating bottle 5 is below the liquid surface of deionized water in water bath 10, and the resistivity of deionized water is 18 MΩ·cm, control system 8 is turned on, heating coil 9 is heated to a temperature of 50°C, rotating motor 6 is turned on, the rotating speed is 10 r / min, and valve 12 is closed to prepare solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped, and the silicone tube 3 at one end of the filter element 2 is fixed with a clamp 19 to prevent leakage during the transfer process. The filtration accuracy of the filter element 2 is 1 μm, the inner diameter of the silicone tube 3 is 10 mm, and the outer diameter is 15 mm. The peristaltic pump 1 connected to the other end of the silicone tube 3 clamps the silicone tube 3, and the peristaltic pump 1 is used to provide power. The rotation speed of the peristaltic pump 1 is 70 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element 2 to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, secondary nucleation will not occur during the transfer process, and impurities in the guanidine tetrafluoroborate solution will remain in the filter element 2. Example 3

[0013] The device is carried out according to Example 1, and the specific operation is carried out according to the following steps: a. Put guanidine tetrafluoroborate raw material into rotating bottle 5, rotating bottle 5 is located in water bath 10, water bath 10 is placed on the upper end of water bath system 17, and the lifting rod 11 on water bath system 17 is adjusted to the upper and lower heights of water bath 10, so that rotating bottle 5 is below the liquid surface of deionized water in water bath 10, and the resistivity of deionized water is 18 MΩ·cm, control system 8 is turned on, heating coil 9 is heated to a temperature of 60°C, rotating motor 6 is turned on, the rotating speed is 30 r / min, and valve 12 is closed to prepare solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped, and the silicone tube 3 at one end of the filter element 2 is fixed with a clamp 19 to prevent leakage during the transfer process. The filtration accuracy of the filter element 2 is 2 μm, the inner diameter of the silicone tube 3 is 12 mm, and the outer diameter is 17 mm. The peristaltic pump 1 connected to the other end of the silicone tube 3 clamps the silicone tube 3, and the peristaltic pump 1 is used to provide power. The rotation speed of the peristaltic pump 1 is 85 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element 2 to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, secondary nucleation will not occur during the transfer process, and impurities in the guanidine tetrafluoroborate solution will remain in the filter element 2. Example 4

[0014] The device is carried out according to Example 1, and the specific operation is carried out according to the following steps: a. Put guanidine tetrafluoroborate raw material into rotating bottle 5, rotating bottle 5 is located in water bath 10, water bath 10 is placed on the upper end of water bath system 17, and the lifting rod 11 on water bath system 17 is adjusted to the upper and lower heights of water bath 10, so that rotating bottle 5 is below the liquid surface of deionized water in water bath 10, and the resistivity of deionized water is 18 MΩ·cm, control system 8 is turned on, heating coil 9 is heated to a temperature of 70°C, rotating motor 6 is turned on, the rotating speed is 50 r / min, and valve 12 is closed to prepare solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped, and the silicone tube 3 at one end of the filter element 2 is fixed with a clamp 19 to prevent leakage during the transfer process. The filtration accuracy of the filter element 2 is 5 μm, the inner diameter of the silicone tube 3 is 11 mm, and the outer diameter is 16 mm. The peristaltic pump 1 connected to the other end of the silicone tube 3 clamps the silicone tube 3, and the peristaltic pump 1 is used to provide power. The rotation speed of the peristaltic pump 1 is 100 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element 2 to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, secondary nucleation will not occur during the transfer process, and the impurities in the guanidine tetrafluoroborate solution will remain in the filter element 2.

[0015] The above descriptions are merely embodiments of the present invention and are not intended to limit the scope of the present invention. Any slight changes or modifications made using the contents of the specification and drawings of the present invention are equivalent to equivalent implementation cases, or are directly or indirectly applied in other related technical fields, and all fall within the scope of the present technical solution.

Claims

1. A device for preparing a crystal solution and transferring it, characterized in that: The device is composed of a heating device, a rotating device, and a transfer device. The transfer device is composed of a peristaltic pump (1), a filter element (2) and a silicone tube (3). The filter element (2) is composed of a rotating device, which is composed of a fixed platform (4), a rotating bottle (5) made of PC material, a rotating motor (6), and a connecting rod (7). The heating device is composed of a control system (8) and a water bath system. The water bath system includes a heating coil (9), a fixing ring (10), a lifting rod (11) and a valve (12). One end of the connecting rod (7) is connected to the rotating bottle (5), and the other end of the connecting rod (7) is connected to the rotating motor (6) and the valve (12). The rotating bottle (5) is located in a water bath pot (10). The water bath pot (10) is placed at the upper end of the water bath system (17) and can move up and down. A degassing device is provided in the water bath pot (10). A water bath system (17) is provided with a lifting rod (11), a heating coil (9) is provided on one side of the water bath system (17), a rotating motor (6) is fixed on a fixed platform (4), the fixed platform (4) is connected to a first bracket (14) and a second bracket (15) by clamps to form a whole fixed on a base (13), a pressure gauge (18) is fixed to the top of the second bracket (15) by a fixing buckle (16), a control system (8) is fixed to the upper part of the fixed platform (4), and the control system (8) is connected to the heating coil (9) by a connecting line (20); both ends of the filter element (2) are connected to the silicone tube (3) by a clamp (19), one end of the silicone tube (3) is inserted into the rotating bottle (5), and the other end of the silicone tube (3) is connected to the peristaltic pump (1), and the specific operation is performed according to the following steps: a. Put guanidine tetrafluoroborate raw material into a rotating bottle (5), the rotating bottle (5) is placed in a water bath (10), the water bath (10) is placed on the upper end of a water bath system (17), and the height of the water bath (10) is adjusted by a lifting rod (11) on the water bath system (17) so that the rotating bottle (5) is below the liquid surface of deionized water in the water bath (10), the resistivity of the deionized water is 18 MΩ·cm, the control system (8) is turned on, the heating coil (9) is heated to a temperature of 40-70° C., the rotating motor (6) is turned on, the rotating speed is 1-50 r / min, and the valve (12) is closed to prepare the solution; b. After the guanidine tetrafluoroborate raw material is completely dissolved, the rotation is stopped. The silicone tube (3) at one end of the filter element (2) is fixed with a clamp to prevent leakage during the transfer process. The filtration accuracy of the filter element (2) is 0.1-5 μm. The inner diameter of the silicone tube (3) is 8-12 mm, and its outer diameter is 13-17 mm. The peristaltic pump (1) connected to the other end of the silicone tube (3) clamps the silicone tube (3). The peristaltic pump (1) provides power. The rotation speed of the peristaltic pump (1) is 50-100 r / min. The guanidine tetrafluoroborate solution prepared in step a is pumped into the growth tank through the filter element (2) to transfer the crystal solution. Since the guanidine tetrafluoroborate solution is in an unsaturated state, impurities in the guanidine tetrafluoroborate solution will remain in the filter element (2) during the transfer process.

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