CN103540994A - Directional growth device for cone face of KDP (Potassium Dihydrogen Phosphate) crystal - Google Patents
Directional growth device for cone face of KDP (Potassium Dihydrogen Phosphate) crystal Download PDFInfo
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- CN103540994A CN103540994A CN201310560583.9A CN201310560583A CN103540994A CN 103540994 A CN103540994 A CN 103540994A CN 201310560583 A CN201310560583 A CN 201310560583A CN 103540994 A CN103540994 A CN 103540994A
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Abstract
The invention belongs to the technical field of crystal growth equipment and relates to a directional growth device for a cone face of a KDP (Potassium Dihydrogen Phosphate) crystal. According to the device, a crystal raising aquarium is placed on a base of a fixed bracket, and a liquid seal is mounted at a small hole formed in the middle of the upper end of the crystal raising aquarium; the crystal raising aquarium contains a growth solution; a seed crystal rack vertically penetrates through the liquid seal at the upper end of the crystal raising aquarium, is placed at the middle part of the growth solution and is rigidly connected with an electric motor fixed on the fixed bracket so as to form a rotating structure; a thermocouple is mounted at one side of the top of the crystal raising aquarium and is inserted into the growth solution; a temperature control device is placed outside the crystal raising aquarium and is in electrical information communication with the thermocouple. The device is simple in structure and convenient in operation, the disturbance to the solution is reduced, raw materials for crystal growth are saved, cone forming areas are reduced, the processing difficulty is reduced, the crystal utilization ratio is increased, and the stability of the solution during crystal growth is improved.
Description
Technical field:
The invention belongs to crystal growth equipment technical field, relate to a kind of crystal growth from solution equipment, a kind of KDP crystalloid conical surface oriented growth device particularly, be used for crystal along conical surface oriented growth, thereby improve the utilization ratio of crystal, the processing difficulties that reduces crystal, obtains high-quality KDP class tabular crystal.
Background technology:
KDP crystalloid is a kind of non-linear optic crystal, main top seed crystal and the bottom seed crystal Fast Growth method of adopting grown at present, although these two kinds of growth methods can grow up to large-sized KDP class monocrystalline, but there is following shortcoming: the one, KDP crystalloid in use, need to cut along frequency multiplication direction, during cutting, easily ftracture; The 2nd, adopt the crystal of top seed crystal and the growth of bottom seed crystal Fast Growth method to become cone region large, reduce the utilization ratio of crystal.Therefore, design a set of device that can realize KDP crystalloid conical surface oriented growth, be of great practical significance.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seek a kind of novel KDP crystalloid conical surface oriented growth device of design design, adopt the seed crystal frame of designed, designed to carry out crystal conical surface oriented growth, reduce the disturbance to solution, save crystal growth raw material, be reduced to cone region, reduce difficulty of processing.
To achieve these goals, agent structure of the present invention comprises electric motor, fluid-tight, thermopair, seed crystal frame, educates crystal glass cylinder, temperature control unit, fixed support and growth solution; The crystal glass cylinder of educating of rectangular structure is placed on support bracket fastened base, and fluid-tight is arranged on educates the aperture place that opens system in the middle of crystal glass cylinder upper end; Educate in crystal glass cylinder growth solution is housed; The seed crystal frame of circular configuration is vertically through the fluid-tight of educating crystal glass cylinder upper end, and hanging type is positioned over the middle part of growth solution, is rigidly connected with the electric motor being fixed on fixed support, and seed crystal frame and electric motor form rotational structure; Electric motor provides power for seed crystal frame, synchronizes together rotation with seed crystal frame; The one side installation of educating crystal glass cylinder top is shaped with thermopair, and thermopair inserts in growth solution; Temperature control unit is positioned over the outside of educating crystal glass cylinder, with thermopair electricity information communication, for controlling the temperature of growth solution.
The seed crystal frame the present invention relates to comprises synthetic glass A plate, synthetic glass B plate and nylon screw; The bottom of synthetic glass A plate and synthetic glass B plate all adopt circular flat plate structure, and wherein, the thickness of synthetic glass A plate bottom is 10mm, and the thickness of synthetic glass B plate is 5mm; The bottom of synthetic glass A plate is fixedly connected with by nylon screw with synthetic glass B plate, the nucleus producing in crystal growing process is dropped in the bottom of glass crystal nourishing jar, seed crystal frame is in rotation process, from kinetics angle, reduce the disturbance to growth solution, increase the stability of growth solution, required growth solution when circular flat plate structure reduces crystal growth simultaneously.
The crystal-like technological process of conical surface oriented growth KDP of the present invention is: first by analytically pure KH
2pO
4raw material and redistilled water are mixed with the growth solution that weight percent concentration is 30-35%, then are 4.0 by the pH value of analytical pure KOH solution growth regulation solution, effectively suppress the growth of crystal cylinder, thereby obtain high-quality conical surface crystal; Then use respectively 0.45 commercially available μ m and 0.22 μ m filter membrane to filter growth solution and carry out Overheating Treatment 24h after the KDP seed crystal along conical surface directional cutting is fixed on to the central authorities of seed crystal frame; Liquid in fluid-tight will be educated crystal glass cylinder and will be hedged off from the outer world, and reduce the friction between seed crystal frame and fluid-tight; KDP seed crystal is put into and is educated crystal glass cylinder under supersolubility temperature, constant temperature growth 1 day in educating crystal glass cylinder after KDP seed crystal slightly soluble, and KDP seed crystal recovers profile, effectively reduces the hereditary defect of KDP seed crystal seed crystal, makes the crystal can normal growth; In KDP seeded growth process, electric motor adopts the rotation rotating manner of forward-stall-reversion to rotate, and rotating speed is 20r/min; Temperature control unit according to KDP solution pH=4.0 time solubility curve temperature program is set, cooling rate is 0.5-1 ℃/day; The lamellar growth under the restriction of seed crystal frame of KDP seed crystal, the speed of growth is 1mm/ days, and crystal takes out after growing into predetermined size, and growth obtains 25 * 25 * 5mm
3the KDP crystal of conical surface oriented growth.
Compared with prior art, it is simple in structure in the present invention, easy to operate, reduces the disturbance to solution, saves crystal growth raw material, is reduced to cone region, reduces difficulty of processing, improves crystal utilization ratio, increases the stability of solution in crystal growing process.
Accompanying drawing explanation:
Fig. 1 is agent structure principle schematic of the present invention.
Fig. 2 is the seed crystal shelf structure principle schematic the present invention relates to.
Embodiment:
Below by embodiment, be also described further by reference to the accompanying drawings.
Embodiment:
The agent structure of the present embodiment comprises electric motor 1, fluid-tight 2, thermopair 3, seed crystal frame 4, educates crystal glass cylinder 5, temperature control unit 6, fixed support 7 and growth solution 8; The crystal glass cylinder 5 of educating of rectangular structure is placed on the base of fixed support 7, and fluid-tight 2 is arranged on educates the aperture place that opens system in the middle of crystal glass cylinder 5 upper ends; Educate growth solution 8 is housed in crystal glass cylinder 5; The seed crystal frame 4 of circular configuration is vertically through the fluid-tight 2 of educating crystal glass cylinder 5 upper ends, and hanging type is positioned over the middle part of growth solution 8, is rigidly connected with the electric motor 1 being fixed on fixed support 7, and seed crystal frame 4 and electric motor 1 form rotational structure; Electric motor 1 provides power for seed crystal frame 4, synchronizes together rotation with seed crystal frame 4; The one side installation of educating crystal glass cylinder 5 tops is shaped with thermopair 3, and thermopair 3 inserts in growth solutions 8; Temperature control unit 6 is positioned over the outside of educating crystal glass cylinder 5, with the electric information communication of thermopair 3, for controlling the temperature of growth solution 8.
The seed crystal frame 4 that the present embodiment relates to comprises synthetic glass A plate 9, synthetic glass B plate 10, nylon screw 11; The bottom of synthetic glass A plate 9 and synthetic glass B plate 10 all adopt circular flat plate structure, and wherein, the thickness of synthetic glass A plate 9 bottoms is 10mm, and the thickness of synthetic glass B plate 10 is 5mm; The bottom of synthetic glass A plate 9 is fixedly connected with by nylon screw 11 with synthetic glass B plate 10, the nucleus producing in crystal growing process is dropped in the bottom of glass crystal nourishing jar 5, seed crystal frame 4 is in rotation process, from kinetics angle, reduce the disturbance to growth solution 8, increase the stability of growth solution 8, required growth solution 8 when circular flat plate structure reduces crystal growth simultaneously.
The crystal-like technological process of the present embodiment conical surface oriented growth KDP is: first by analytically pure KH
2pO
4raw material and redistilled water are mixed with the growth solution 8 that weight percent concentration is 30-35%, then are 4.0 by the pH value of analytical pure KOH solution growth regulation solution 8, effectively suppress the growth of crystal cylinder, thereby obtain high-quality conical surface crystal; Then use respectively 0.45 commercially available μ m and 0.22 μ m filter membrane to filter growth solution 8 and carry out Overheating Treatment 24h after the KDP seed crystal 12 along conical surface directional cutting is fixed on to the central authorities of seed crystal frame 4; Liquid in fluid-tight 2 will be educated crystal glass cylinder 5 and will be hedged off from the outer world, and reduce the friction between seed crystal frame 4 and fluid-tight 2; KDP seed crystal 12 is put into and is educated crystal glass cylinder 5 under supersolubility temperature, constant temperature growth 1 day in educating crystal glass cylinder 5 after KDP seed crystal 12 slightly solubles, and KDP seed crystal 12 recovers profiles, effectively reduces the hereditary defect of KDP seed crystal 12 seed crystals, makes the crystal can normal growth; In KDP seed crystal 12 process of growth, electric motor 1 adopts the rotation rotating manner of forward-stall-reversion to rotate, and rotating speed is 20r/min; Temperature control unit 6 according to KDP solution pH=4.0 time solubility curve temperature program is set, the cooling rate of temperature control unit 6 is 0.5-1 ℃/day; The lamellar growth under the restriction of seed crystal frame 4 of KDP seed crystal, the speed of growth is 1mm/ days, crystal takes out after growing into predetermined size, draws 25 * 25 * 5mm
3the KDP crystal of conical surface oriented growth.
Claims (3)
1. a KDP crystalloid conical surface oriented growth device, is characterized in that agent structure comprises electric motor, fluid-tight, thermopair, seed crystal frame, educates crystal glass cylinder, temperature control unit, fixed support and growth solution; The crystal glass cylinder of educating of rectangular structure is placed on support bracket fastened base, and fluid-tight is arranged on educates the aperture place that opens system in the middle of crystal glass cylinder upper end; Educate in crystal glass cylinder growth solution is housed; The seed crystal frame of circular configuration is vertically through the fluid-tight of educating crystal glass cylinder upper end, and hanging type is positioned over the middle part of growth solution, is rigidly connected with the electric motor being fixed on fixed support, and seed crystal frame and electric motor form rotational structure; Electric motor provides power for seed crystal frame, synchronizes together rotation with seed crystal frame; The one side installation of educating crystal glass cylinder top is shaped with thermopair, and thermopair inserts in growth solution; Temperature control unit is positioned over the outside of educating crystal glass cylinder, with thermopair electricity information communication, for controlling the temperature of growth solution.
2. KDP crystalloid conical surface oriented growth device according to claim 1, is characterized in that the seed crystal frame relating to comprises synthetic glass A plate, synthetic glass B plate and nylon screw; The bottom of synthetic glass A plate and synthetic glass B plate all adopt circular flat plate structure, and wherein, the thickness of synthetic glass A plate bottom is 10mm, and the thickness of synthetic glass B plate is 5mm; The bottom of synthetic glass A plate is fixedly connected with by nylon screw with synthetic glass B plate, the nucleus producing in crystal growing process is dropped in the bottom of glass crystal nourishing jar, seed crystal frame is in rotation process, the disturbance of minimizing to growth solution, increase the stability of growth solution, required growth solution when circular flat plate structure reduces crystal growth simultaneously.
3. KDP crystalloid conical surface oriented growth device according to claim 1, is characterized in that the crystal-like technological process of conical surface oriented growth KDP is: first by analytically pure KH
2pO
4raw material is dissolved in and in redistilled water, is mixed with the growth solution that weight percent concentration is 30-35%, then is 4.0 by the pH value of analytical pure KOH solution growth regulation solution, effectively suppresses the growth of crystal cylinder, thereby obtains high-quality conical surface crystal; Then use respectively 0.45 commercially available μ m and 0.22 μ m filter membrane to filter growth solution and carry out Overheating Treatment 24h after the KDP seed crystal along conical surface directional cutting is fixed on to the central authorities of seed crystal frame; Liquid in fluid-tight will be educated crystal glass cylinder and will be hedged off from the outer world, and reduce the friction between seed crystal frame and fluid-tight; KDP seed crystal is put into and is educated crystal glass cylinder under supersolubility temperature, constant temperature growth 1 day in educating crystal glass cylinder after KDP seed crystal slightly soluble, and KDP seed crystal recovers profile, effectively reduces the hereditary defect of KDP seed crystal seed crystal, makes the crystal can normal growth; In KDP seeded growth process, electric motor adopts the rotation rotating manner of forward-stall-reversion to rotate, and rotating speed is 20r/min; Temperature control unit according to KDP solution pH=4.0 time solubility curve temperature program is set, cooling rate is 0.5-1 ℃/day; The lamellar growth under the restriction of seed crystal frame of KDP seed crystal, the speed of growth is 1mm/ days, and crystal takes out after growing into predetermined size, and growth obtains 25 * 25 * 5mm
3the KDP crystal of conical surface oriented growth.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310560583.9A CN103540994A (en) | 2013-11-12 | 2013-11-12 | Directional growth device for cone face of KDP (Potassium Dihydrogen Phosphate) crystal |
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| CN201310560583.9A CN103540994A (en) | 2013-11-12 | 2013-11-12 | Directional growth device for cone face of KDP (Potassium Dihydrogen Phosphate) crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475777A (en) * | 2017-07-14 | 2017-12-15 | 中国科学院上海光学精密机械研究所 | High-accuracy oil bath annealing furnace for KDP crystalloids |
| CN109943881A (en) * | 2019-04-10 | 2019-06-28 | 中国科学院上海光学精密机械研究所 | A kind of carrier crystal stand of the long seed crystal list cone crystal growth of KDP class |
| CN110344114A (en) * | 2019-07-02 | 2019-10-18 | 中国科学院上海光学精密机械研究所 | KDP crystalloid conical surface method for fast growing |
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| CN102618924A (en) * | 2012-04-25 | 2012-08-01 | 青岛大学 | Rapid lateral growing method of KDP (Potassium Dihydrogen Phosphate) crystals |
| CN103361712A (en) * | 2012-04-09 | 2013-10-23 | 中国科学院理化技术研究所 | Crystal carrying bracket for large-section KDP (Potassium Dihydrogen Phosphate) crystal growth and growing method of large-section KDP crystal |
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2013
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Patent Citations (3)
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| CN102144052A (en) * | 2008-08-07 | 2011-08-03 | Soraa有限公司 | Process for large-scale ammonothermal manufacturing of gallium nitride boules |
| CN103361712A (en) * | 2012-04-09 | 2013-10-23 | 中国科学院理化技术研究所 | Crystal carrying bracket for large-section KDP (Potassium Dihydrogen Phosphate) crystal growth and growing method of large-section KDP crystal |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475777A (en) * | 2017-07-14 | 2017-12-15 | 中国科学院上海光学精密机械研究所 | High-accuracy oil bath annealing furnace for KDP crystalloids |
| CN109943881A (en) * | 2019-04-10 | 2019-06-28 | 中国科学院上海光学精密机械研究所 | A kind of carrier crystal stand of the long seed crystal list cone crystal growth of KDP class |
| CN110344114A (en) * | 2019-07-02 | 2019-10-18 | 中国科学院上海光学精密机械研究所 | KDP crystalloid conical surface method for fast growing |
| CN110344114B (en) * | 2019-07-02 | 2021-05-04 | 中国科学院上海光学精密机械研究所 | Quick conical surface growth method for KDP crystal |
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Application publication date: 20140129 |