CN114381809A - Method for removing mixed crystals in crystal growth tank and tank bottom - Google Patents
Method for removing mixed crystals in crystal growth tank and tank bottom Download PDFInfo
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- CN114381809A CN114381809A CN202210151711.3A CN202210151711A CN114381809A CN 114381809 A CN114381809 A CN 114381809A CN 202210151711 A CN202210151711 A CN 202210151711A CN 114381809 A CN114381809 A CN 114381809A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application provides a method for removing impurity crystals in a crystal growth groove and a groove bottom, and belongs to the field of crystal growth. The crystal growth tank comprises a mixed crystal dissolving cover, a movable connecting pipe, a heater, a tank body, a continuous filtering device, a stirring motor and a crystal carrying frame; the continuous filtering device is arranged outside the tank body; the crystal carrier is arranged in the groove body; the mixed crystal dissolving cover is positioned between the crystal carrying frame and the bottom of the tank body; the opening of the cover body of the mixed crystal dissolving cover faces to the bottom of the groove body; the mixed crystal dissolving cover is provided with a solution inlet and a solution outlet; one end of the movable connecting pipe is communicated with the solution inlet, and the other end of the movable connecting pipe is communicated with the continuous filtering device; a heater is arranged at one end of the movable connecting pipe close to the continuous filtering device; the crystal growth solution enters the mixed crystal dissolving cover through the continuous filtering system, and the movable connecting pipe can move the mixed crystal dissolving cover so as to achieve the purpose of directionally dissolving the mixed crystals, thereby solving the mixed crystal problem in the crystal growth process and improving the success rate of crystal growth.
Description
Technical Field
The invention relates to a method for removing impurity crystals in a crystal growth tank and at the bottom of the crystal growth tank, belonging to the technical field of crystal growth.
Background
Potassium dihydrogen phosphate crystal (KDP) and potassium dideuterium phosphate crystal (DKDP) are important optical elements used in inertial confinement nuclear fusion devices, and have the advantages of capability of simultaneously meeting wide transmission wave bands, large electro-optic coefficients and nonlinear optical coefficients, high damage threshold, large caliber, proper birefringence, low refractive index nonuniformity and the like.
The KDP/DKDP crystal growth at the present stage mainly adopts a fast growth method and a traditional slow growth method, in the process of fast crystal growth, due to the fact that supersaturation degree is large, fine impurities in a solution comprise dust in air and the like, spontaneous nucleation of a crystal growth solution is easily caused, mixed crystals are generated, and due to the fact that the growth speed of the mixed crystals is too fast, the crystal growth process is stopped.
Disclosure of Invention
The crystal growth groove provided by the application heats crystal growth solution through the heater, then the solution enters the mixed crystal dissolving cover, the movable connecting pipe can move the mixed crystal dissolving cover to achieve the purpose of directionally dissolving the mixed crystals, so that the mixed crystal problem in the crystal growth process is solved, and the success rate of crystal growth is improved.
According to one aspect of the application, a crystal growth tank is provided, which comprises a mixed crystal dissolving cover, a movable connecting pipe, a heater, a tank body, a continuous filtering device, a stirring motor and a crystal carrying frame;
the continuous filtering device is arranged outside the tank body and used for circularly filtering the crystal growth solution, so that the quality of the crystal is improved;
the crystal carrier is arranged in the groove body and is used for providing a platform for crystal growth;
the mixed crystal dissolving cover is positioned between the crystal carrying frame and the bottom of the tank body; the opening of the cover body of the mixed crystal dissolving cover faces to the bottom of the groove body; the mixed crystal dissolving cover is provided with a solution inlet and a solution outlet;
one end of the movable connecting pipe is communicated with the solution inlet, and the other end of the movable connecting pipe is communicated with the continuous filtering device; the movement of the mixed crystal dissolving cover at the bottom of the crystal growing tank is realized by controlling the movable connecting pipe;
and a heater is arranged at one end of the movable connecting pipe close to the continuous filtering device and used for heating the solution in the movable connecting pipe.
Optionally, the solution outlet is higher than the solution inlet.
Optionally, a sealing element capable of being connected with the bottom of the tank body in a sealing manner is arranged on the periphery of the opening of the cover body of the mixed crystal dissolving cover.
The sealing element is tightly attached to the bottom of the crystal growth tank by controlling the movable connecting pipe, so that the mixed crystals are fixed in the mixed crystal dissolving cover to prevent the mixed crystals from moving.
Optionally, the sealing member is selected from one of a silicone suction cup and a rubber ring.
Optionally, the bottom of the side wall of the tank body is provided with an observation port, so that the crystallization condition in the tank body can be observed at any time.
Optionally, a stainless steel corrugated pipe is arranged at an interface of the movable connecting pipe penetrating through the side wall of the tank body and used for supporting the movable connecting pipe; the stainless steel corrugated pipe is arranged outside the tank body and sealed with the side wall of the tank body by adopting a silica gel gasket to prevent the solution from seeping.
Optionally, the mixed crystal dissolving cover is made of transparent materials, and the dissolving condition of the internal crystals can be observed at any time.
Optionally, the movable connecting pipe is selected from a glass pipe or a coated stainless steel pipe and has the self-supporting property.
Optionally, the continuous filtering device comprises a circulating pump and a filter element, the circulating pump provides power for circulation of the crystal growth solution, and the filter element is used for filtering impurities in the crystal growth solution, so that the crystal quality and the crystal growth success rate are improved.
Optionally, the crystal carrying frame is connected with a stirring motor, and the stirring motor is used for driving the crystal carrying frame to rotate so as to ensure the uniformity of the crystal growth solution.
According to one aspect of the application, a method for removing mixed crystals at the bottom of a growth tank is provided, wherein the crystal growth tank is adopted;
the crystal carrying frame rotationally stirs crystal growth solution in the tank body, when mixed crystals appear at the bottom of the tank body, the mixed crystal dissolving cover is moved by controlling the movable connecting pipe to capture the mixed crystals, and the crystal growth solution enters the mixed crystal dissolving cover through the solution inlet after passing through the continuous filtering device and the heater and then enters the crystal growth solution cavity through the solution outlet.
Optionally, when the mixed crystals are captured, the opening of the cover body of the mixed crystal dissolving cover is hermetically connected with the bottom of the groove body.
Optionally, when the mixed crystals occur, the position of the mixed crystals can be determined through an observation port on the side wall of the tank body.
Optionally, the heater heats the crystal growth solution above a saturation point.
Optionally, the heater heats the crystal growth solution to 10-20 ℃ above the saturation point.
Optionally, the rotation circulation mode of the stirring motor is positive rotation-stop-reverse rotation, positive rotation is carried out for 30s, stop rotation is carried out for 5s, reverse rotation is carried out for 30s, repetition is carried out, the rotation speed is 0-60 r/min, and the working time is 24h without stop.
The beneficial effects that this application can produce include:
the method for removing the mixed crystals in the crystal growth tank is suitable for the whole crystal growth stage. When mixed crystals appear in the crystal growth process, the crystal growth solution is heated to a temperature above the saturation point, and then is conveyed to the mixed crystal dissolving cover through the movable connecting pipe and the circulating pump, and the solution enters from bottom to top, so that the mixed crystals can be fully dissolved. The silica gel sucker arranged on the mixed crystal protective cover can prevent the mixed crystals from moving. Because the volume of the mixed crystal dissolving cover is small, the high-temperature solution enters the crystal growth tank and can be ignored relative to the growth solution with the temperature below the saturation point, so that the local heating of the solution can be ensured, the mixed crystal is dissolved on the premise of not damaging the stability of the solution, and the success rate of crystal growth is improved.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus according to embodiment 1 of the present application;
wherein, 1-silica gel sucker; 2-a solution outlet; 3-mixed crystal dissolving cover; 4-a mobile connecting pipe; 5-a heater; 6-groove body; 7-crystal growth solution chamber; 8-a continuous filtration unit; 9-a stirring motor; 10-a crystal carrying frame; 11-KDP crystals; 12-solution inlet.
Detailed Description
The present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples.
For a better illustration of the invention, and to facilitate an understanding of the operational flow of the invention, typical but non-limiting examples of the invention follow.
Example 1
A crystal growth tank, as shown in fig. 1, comprising a mixed crystal dissolving cover 3, a movable connecting pipe 4, a heater 5, a tank 6, a continuous filtering device 8, a stirring motor 9 and a crystal carrying frame 10;
the continuous filtering device 8 is arranged outside the tank body and comprises a circulating pump and a filter element;
a stirring motor 5 is arranged at the center of the top of the tank body 6, and a connecting rod of the stirring motor 5 penetrates through the top of the tank body 6 to enter a crystal growth solution cavity 7 and then is connected with a crystal carrying frame 10;
the crystal carrying frame is arranged in the tank body, a mixed crystal dissolving cover 3 is arranged between the crystal carrying frame 10 and the bottom of the tank body 6, the opening of the cover body of the mixed crystal dissolving cover faces the bottom of the tank body, the diameter of the opening of the cover body is 50mm, the mixed crystal dissolving cover 3 is provided with a solution inlet 12 and a solution outlet 2, and the solution outlet 2 is 30mm higher than the solution inlet 12; one end of the movable connecting pipe 4 is communicated with the solution inlet 12, and the other end of the movable connecting pipe 4 is communicated with the continuous filtering device 8;
the movable connecting pipe 4 is provided with a heater 5 at one side close to the continuous filtering device 8.
The mixed crystal dissolving cover is made of transparent materials (high borosilicate glass), a circle of silica gel sucker 1 is arranged at an opening at the bottom of the mixed crystal dissolving cover, the silica gel sucker 1 is tightly attached to the bottom of the crystal growth tank body 6 by controlling the movable connecting pipe 4, and mixed crystals are fixed in the mixed crystal dissolving cover 3 to prevent the mixed crystals from moving.
The bottom of the side wall of the tank body 6 is provided with an observation port; the movable connecting tube 4 is a glass tube.
The external part of the interface of the movable connecting pipe 4 penetrating through the side wall of the tank body 6 is provided with a stainless steel corrugated pipe for supporting the movable connecting pipe.
Example 2
A method for removing mixed crystals at the bottom of a groove during KDP crystal preparation adopts the crystal growth groove described in the embodiment 1, a crystal carrying frame 10 rotates and stirs a crystal growth solution in the groove 6, and the stirring rotation circulation mode is positive rotation, stopping rotation and reverse rotation, positive rotation for 30s, stopping rotation for 5s, reverse rotation for 30s, repetition, and the rotation speed is 30 r/min. After the crystal growth solution is circularly filtered by the continuous filtering device 8, the solution is heated to a temperature of more than 15 ℃ of the saturation point by the heater 5 and enters the mixed crystal dissolving cover 3 through the movable connecting pipe 4.
When mixed crystals appear in the growth process, after the mixed crystal position is found, the movable connecting pipe 4 is controlled to enable the mixed crystals to be located in the mixed crystal dissolving cover 3, pressure is applied to enable the silica gel sucker 1 to be tightly attached to the bottom of the crystal growth groove body 6, the mixed crystals are fixed in the mixed crystal dissolving cover 3, and the mixed crystals are prevented from moving. The solution in the mixed crystal dissolving cover 3 dissolves the mixed crystal from bottom to top through the high-temperature solution flow, and the dissolved solution enters the crystal growth solution cavity 7 through the solution outlet 2 for reuse.
The above description is only for the purpose of illustrating the present invention and is not intended to limit the present invention in any way, and the present invention is not limited to the above description, but rather should be construed as being limited to the scope of the present invention.
Claims (10)
1. The crystal growth tank is characterized by comprising a mixed crystal dissolving cover (3), a movable connecting pipe (4), a heater (5), a tank body (6), a continuous filtering device (8), a stirring motor (9) and a crystal carrying frame (10);
the continuous filtering device (8) is arranged outside the tank body (6) and is used for circulating and filtering the crystal growth solution;
the crystal carrying frame (10) is arranged inside the groove body (6) and is used for providing a platform for crystal growth;
the mixed crystal dissolving cover (3) is positioned between the crystal carrying frame (10) and the bottom of the tank body (6); the opening of the cover body of the mixed crystal dissolving cover (3) faces to the bottom of the groove body (6); the mixed crystal dissolving cover (3) is provided with a solution inlet (12) and a solution outlet (2);
one end of the movable connecting pipe (4) is communicated with the solution inlet (12), and the other end is communicated with the continuous filtering device (8); and a heater (5) is arranged at one end of the movable connecting pipe (4) close to the continuous filtering device (8).
2. Crystal growth cell according to claim 1, characterized in that the solution outlet (2) is higher than the solution inlet (12).
3. The crystal growth groove of claim 2, wherein the periphery of the opening of the cover body of the mixed crystal dissolving cover (3) is provided with a sealing element which can be connected with the bottom of the groove body (6) in a sealing way;
preferably, the sealing element is selected from one of a silicon rubber suction cup and a rubber ring.
4. A crystal growth trough according to claim 1, characterized in that the bottom of the side walls of the trough body (6) is provided with a viewing port.
5. The crystal growth trough of claim 1, wherein a stainless steel corrugated pipe is arranged at the interface of the movable connecting pipe (4) and the side wall of the trough body (6), the stainless steel corrugated pipe is positioned outside the trough body (6), and the interface is sealed by a silica gel pad.
6. The crystal growth cell according to claim 1, wherein the mixed crystal dissolving cover (3) is made of transparent material;
the movable connecting pipe (4) is selected from a glass pipe or a coated stainless steel pipe.
7. Crystal growth cell according to claim 1, characterized in that said continuous filtering means (8) comprise a circulation pump and a filter cartridge;
preferably, the crystal carrying frame (10) is connected with a stirring motor (9).
8. A method for removing mixed crystals at the bottom of a growth tank, which is characterized in that a crystal growth tank as claimed in any one of claims 1 to 7 is adopted;
the crystal carrying frame (10) rotationally stirs crystal growth solution in the tank body (6), when mixed crystals appear at the bottom of the tank body (6), the mixed crystal dissolving cover (3) is moved by controlling the movable connecting pipe (4) to capture the mixed crystals, and the crystal growth solution enters the mixed crystal dissolving cover (3) through the solution inlet (12) and then enters the crystal growth solution cavity (7) through the solution outlet (2) after passing through the continuous filtering device (8) and the heater (5);
preferably, when the mixed crystals are captured, the opening of the mixed crystal dissolving cover (3) is hermetically connected with the bottom of the groove body (6);
preferably, when the mixed crystals occur, the mixed crystal position can be determined through an observation port on the side wall of the groove body (6).
9. The method according to claim 8, wherein the heater (5) heats the crystal growth solution above a saturation point;
preferably, the heater (5) heats the crystal growth solution to a temperature 10-20 ℃ higher than the saturation point.
10. The method according to claim 8, wherein the rotation of the stirring motor (9) is cycled in a forward rotation-stop-reverse rotation manner at a rotation speed of 0-60 r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210151711.3A CN114381809B (en) | 2022-02-18 | 2022-02-18 | Crystal growth groove and groove bottom impurity crystal removing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210151711.3A CN114381809B (en) | 2022-02-18 | 2022-02-18 | Crystal growth groove and groove bottom impurity crystal removing method |
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| Publication Number | Publication Date |
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| CN114381809A true CN114381809A (en) | 2022-04-22 |
| CN114381809B CN114381809B (en) | 2023-06-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210151711.3A Active CN114381809B (en) | 2022-02-18 | 2022-02-18 | Crystal growth groove and groove bottom impurity crystal removing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990645A (en) * | 2022-06-30 | 2022-09-02 | 深圳惠科新材料有限公司 | Copper sulfate crystal recovery device and method |
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| JPH08301684A (en) * | 1995-05-08 | 1996-11-19 | Canon Inc | Crystal growing apparatus and growth of crystal |
| CN103147116A (en) * | 2013-04-03 | 2013-06-12 | 江南大学 | Continuous culture and filtration system for crystals |
| CN209005316U (en) * | 2018-06-22 | 2019-06-21 | 唐山百城铁塔制造有限公司 | A kind of zinc-plated clean type Sewage Disposal |
| CN110055578A (en) * | 2019-04-15 | 2019-07-26 | 中国科学院上海光学精密机械研究所 | In KDP crystalloid growth course on carrier crystal stand stray crystal cancellation element and method |
| CN110093666A (en) * | 2019-04-15 | 2019-08-06 | 中国科学院上海光学精密机械研究所 | The cancellation element and method of KDP crystalloid growth slot slot bottom stray crystal |
-
2022
- 2022-02-18 CN CN202210151711.3A patent/CN114381809B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08301684A (en) * | 1995-05-08 | 1996-11-19 | Canon Inc | Crystal growing apparatus and growth of crystal |
| CN103147116A (en) * | 2013-04-03 | 2013-06-12 | 江南大学 | Continuous culture and filtration system for crystals |
| CN209005316U (en) * | 2018-06-22 | 2019-06-21 | 唐山百城铁塔制造有限公司 | A kind of zinc-plated clean type Sewage Disposal |
| CN110055578A (en) * | 2019-04-15 | 2019-07-26 | 中国科学院上海光学精密机械研究所 | In KDP crystalloid growth course on carrier crystal stand stray crystal cancellation element and method |
| CN110093666A (en) * | 2019-04-15 | 2019-08-06 | 中国科学院上海光学精密机械研究所 | The cancellation element and method of KDP crystalloid growth slot slot bottom stray crystal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990645A (en) * | 2022-06-30 | 2022-09-02 | 深圳惠科新材料有限公司 | Copper sulfate crystal recovery device and method |
| CN114990645B (en) * | 2022-06-30 | 2024-04-16 | 深圳惠科新材料股份有限公司 | Copper sulfate crystal recovery device and method |
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| CN114381809B (en) | 2023-06-27 |
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