CN1234920C - Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category - Google Patents
Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category Download PDFInfo
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- CN1234920C CN1234920C CN 03139027 CN03139027A CN1234920C CN 1234920 C CN1234920 C CN 1234920C CN 03139027 CN03139027 CN 03139027 CN 03139027 A CN03139027 A CN 03139027A CN 1234920 C CN1234920 C CN 1234920C
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Abstract
The present invention relates to a method and a device for growing large-section monocrystal of a potassium dihydrogen phosphate class, which belongs to the technical field of crystal growth. In the method, powder of a solid KDP crystal is used as a raw material; a solution prepared by adopting water or heavy water as a solvent is used as a growing solution; a transparent Z crystal chip identical with a grown crystal is used as a seed crystal. The transparent Z crystal chip is fixed to a crystal carrying frame; the solid KDP crystal as a raw material is added into the bottom of a growing container; a baffle plate is added; after being filtered by an ultrafine microporous filtering film, the well-prepared solution is added into the container; the temperature of two temperature areas of the crystal growing container is controlled respectively; a large-section KDP crystal is grown by a constant temperature method and a temperature falling method. The growing device is characterized in that a baffle plate is arranged in the crystal growing container, and the container is divided into two parts by the baffle plate to form a high temperature area and a low temperature area; small holes are drilled on the baffle plate. The present invention has the advantages of easy realization of growing technology and simple equipment, and high-grade large-section monocrystal of a potassium dihydrogen phosphate class can be obtained.
Description
(1) technical field
The present invention relates to KDP configuration water-soluble crystalline growth, especially large section potassium primary phosphate (KH
2PO
4, be called for short KDP), potassium dideuterium phosphate (K (H
1-xD
x)
2PO
4, be called for short DKDP) or primary ammonium phosphate (NH
4H
2PO
4) wait the growth of single crystal, belong to the crystal technique field.
(2) background technology
The water-soluble crystal of KDP configuration is a quasi-nonlinear optical crystal, high-tech sector such as be widely used in Electro-optical Modulation, frequency inverted, the photoprocess of laser and communicate by letter, particularly heavy caliber KDP and DKDP crystalline material have become unique in the world laser tuning and modulation material that can be used for the laser fusion device at present, improving laser fusion efficient, expanded laser light wave band aspect all has important practical value and scientific meaning, and the growth of its crystalline material has become current international research focus.The main at present employing falling temperature method of KDP configuration crystal, the methods such as method and the quick growth method of some seed crystal that circulate are carried out single crystal growing, and these methods respectively have relative merits.Falling temperature method is referring to people such as Sa Sakai, the growth with large-sized KDP is tested in laser fusion, the crystal growth magazine, 1990,99,820-826 (Sasakai T., Yokotani A., Growth oflarge KDP crystals for laser fusion experiments.J.Crystal Growth, 1990,99, be that equipment is simple from growth from solution crystalline traditional method 820-826), but owing in crystal growing process, can not replenish raw material, grow large-size crystals, the use container is big, and the saturation concentration of solution is wayward evenly, and because growth cycle is long, be prone to sporadic nucleation in the temperature-fall period, destroy normal crystal growth.The method of circulating can constantly be added raw material in process of growth, grow large-sized crystal with less growth apparatus, and growth groove size is less, be easy to control uniform temperature field and concentration field, crystal is grown under constant temperature, permanent supersaturation concentration, can improve the crystalline homogeneity greatly, improve the crystalline quality, referring to Lu Zhikuan, Gao Zhangshou, Li Yiping, Wang Can, the solution circulated method growing large-size KDP crystal that flows, the artificial lens journal, 1996,25 (1), 19-22.Put the seed crystal method for fast growing referring to people such as Lu Si, national portfire large size KDP and KD
*The P crystalline is grown fast, SPIE meeting vol.402 (2000): 152-161 (RuthNawley-Fedder, Navy Roley, Tom Biesiada, et al, Rapid growth of very large KDP and KD
*Pcrystal in support of the national ignition facility, Proceedings of SPIE vol.402 (2000): 152-161), can grow macrocrystal at short notice, the crystal three dimensional growth, the speed of growth improves an order of magnitude than the falling temperature method and the method that circulates.But growth conditions is very harsh fast, and the equipment complexity is of a high price; Solution is in height thermodynamic instability state for a long time, failure very risky; Material purity requires high, and the crystal that crystal mass is just grown near traditional technology in adding continuous filtration, laser annealing.These methods have two common shortcomings, the one, liquor capacity is bigger, need a large amount of solvents to form solution, device takes up room huge, this is for being that influence is little for the KDP crystal of solvent with water, but for expensive heavy water being the rising significantly that the deuterate crystal of solvent such as DKDP etc. then mean cost; The 2nd, in the growth groove in a single day stray crystal appears, because stray crystal scarcely is a single crystal, the speed of growth is many soon than monocrystalline, will fight for raw material with the crystal that will grow, causes crystal to grow.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, the growth method and the device of a kind of large section potassium dihydrogen phosphate single crystal is provided,, reduce cost, improve crystal quality by the volume that dwindles growth solution, the growth of control stray crystal.
The present invention adopt in the crystal growth constant temperature method and in conjunction with falling temperature method growth Large KDP crystalloid.
Raw material of the present invention is the crystal-like powder raw material of solid K DP, and growth solution is to be the solution of solvent configuration with water or heavy water, and concentration is in the temperature of saturation of solution, and it be worth at 30-70 ℃, the transparent Z pellet that the seed crystal employing is identical with growing crystal.
Above-mentioned solid K DP crystalloid is: potassium primary phosphate (KH
2PO
4), potassium dideuterium phosphate (K (H
1-xD
x)
2PO
4) or primary ammonium phosphate (NH
4H
2PO
4).
The growth method concrete steps of large section potassium dihydrogen phosphate single crystal are as follows:
1. 1～1.5 times that presses required growing crystal weight with solid K DP crystalloid raw material adding growth container bottom, add baffle plate, to behind ultra-fine filtering with microporous membrane, add container at the solution for preparing under 35-80 ℃, vitellarium, top solution temperature will be set at the solution saturation point 2-5 ℃ of balance 24-48 hour seed crystal to be put that makes progress.
2. seed crystal adopts transparent Z pellet, in the boring of (001) of seed crystal direction, is fixed on the carrier crystal stand, and the carrier crystal stand of having fixed seed crystal is placed baking oven, is warmed up to the temperature reequilibrate identical with vitellarium solution 12～24 hours.
Seed size according to the crystalline size of required growth routinely technology determine, bore 2-4 aperture, pass aperture with nylon yarn or Stainless Steel Wire seed crystal be fixed on the carrier crystal stand.
3. the Balanced carrier crystal stand that is fixed with seed crystal of temperature in the step (2) is put into the solution of step (1), carried out the rotation of " forward-stop-reverse ".Allow the solution of vitellarium cool to the following crystal of saturation point naturally and begin growth, and then homo(io)thermism is made the crystalchecked growth at the following 0.5-2.5 of saturation point ℃ by the degree of supersaturation of setting, adjust the dissolve area temperature simultaneously to being higher than vitellarium temperature 2-10 ℃, the crystal raw material of container bottom is constantly dissolved, be transported to the vitellarium by the baffle plate hole, to replenish the used up raw material of crystal growth.
4. when treating that desired size is arrived in crystal growth, reduce the vitellarium solution temperature rallentando, cooling rate is exceeded not cause crystal damage, adjust the dissolve area temperature simultaneously and be lower than the vitellarium temperature, when solution temperature is reduced to room temperature, solution is extracted out, take out crystal.
The speed of crystal growth is by factors such as the whipped state decision of the temperature gap of temperature, vitellarium and the dissolve area of vitellarium, dissolve area, and is also relevant with the factors such as purity of the volume of crystalline size, growth container, raw material simultaneously.In the temperature-fall period after growth is finished, because there is the powdery growth raw material in dissolve area, its surface-area sum is much larger than the surface-area of growing crystal, and the dissolve area temperature is lower than the vitellarium, therefore the solute overwhelming majority of separating out in the temperature-fall period is separated out at dissolve area, has only small portion length to crystal.
In above-mentioned process of growth, relevant processing parameter is except that special proposition, all with reference to state of the art.
The present invention has bigger positive temperature coefficient feature according to KDP crystalloid solubleness, rely on the solution in the container to form and keep certain thermograde up and down, add the seeded growth crystal in the top low-temperature end, adding raw material in the bottom temperature end dissolves, be separated by by baffle plate between the high and low temperature end, solution is kept the hypersaturated state of vitellarium by two kinds of effects of diffusion convection current of temperature difference convection current and concentration, utilize the temperature difference of baffle plate and heat regulation vitellarium and dissolve area, the control crystalline speed of growth.
Technical scheme of the present invention is equally applicable to the growth of other single crystal of KDP type.
The growing apparatus of large section of the present invention potassium dihydrogen phosphate single crystal has following structure:
Crystal growing apparatus of the present invention comprises motor, carrier crystal stand, crystal growth vessel, agitator, temperature sensor, controller, well heater etc., in crystal growth vessel, be provided with a baffle plate container is divided into two portions, form high and low two warm areas, aperture is arranged on the baffle plate.
The slit that 0.1～1cm is arranged between baffle edge and the container inner wall.
Baffle shapes is consistent with the growth container inwall, cooperates closely, can conveniently install and draw off simultaneously.Baffle shapes can be flush type, arc surfaced, positive umbellate form or the umbrella shape of falling, and the perforate mode can be single hole or porous.
Controlled separately respectively by this two-part temperature that baffle plate is divided into, form high and low two warm areas, carry out the dissolving of crystal raw material and the growth of single crystal respectively, the material between two warm areas transports by the slit of design between the aperture on the baffle plate and baffle plate and container and finishes.
In two warm areas of above-mentioned crystal growth vessel, a temperature sensor is housed respectively, is connected with container programmable logic controller, infrared lamp well heater outward respectively.
Support is arranged at above-mentioned crystal growth vessel bottom.
Above-mentioned crystal growth vessel is the crystal growth cylinder.
Compare with methods such as putting the quick growth method of seed crystal with existing falling temperature method, the method that circulates, the present invention has such advantage: (1) can grow under relative constant temperature, permanent degree of supersaturation, helps improving crystal mass; Particularly for the deuterate crystal, can not cause the variation of crystal degree of deuterium because of the variation of growth temperature.(2) volume of solution dwindles greatly, can grow macrocrystal with the smaller size smaller growth container; Particularly for the DKDP crystal, can reduce the usage quantity of heavy water significantly, the input that reduces cost has important economic implications.(3) can be chosen in as the case may be under the high as far as possible temperature and grow, accelerate crystalline growth velocity; (4) adopt the two warm area growing crystals of single groove, significantly reduced growth apparatus and taken up space.(5) baffle plate is the place that the heat transportation of solution must pass through, its upper temp is higher than the crystal growth zone, therefore the stray crystal that occurs in the crystal growing process drops on baffle plate top, though can not dissolve, still can reduce its speed of growth, make its can not with the crystal that will grow contention raw material, crystal can continued growth; (6) equipment is simple, and growth technique realizes that easily solution and extraneous contact area are few, reduce contaminated chance, particularly for the DKDP crystal, can reduce the reduction of the degree of deuterium that causes because of ingress of air; (7) crystal is along the growth of (001) direction, and crystal mass is better than along the crystal of three direction three dimensional growths (the quick growth method of some seed crystal), and the length of growth is long more, and the defective of seed crystal itself is extended few more, and crystal mass is good more, and the crystalline utilization ratio is also high more.(8) only along the growth of (001) direction, the ingredient requirement of growing crystal is general, the acceptable wide scope of material for crystal.
(4) description of drawings
Fig. 1 is the structural representation of an embodiment of crystal growing apparatus of the present invention.1 is motor among the figure, and 2 is cylinder cap, and 3 is carrier crystal stand, 4 crystal for growth, 5 are the crystal growth cylinder, 6 is baffle plate, 7 is agitator, and 8 is crystal raw material, and 9 are the growth jar support, 10 is temperature sensor, and 11 is programmable logic controller, and 12 is the well heater infrared lamp, 13 is temperature sensor, and 14 is programmable logic controller, and 15 is the well heater infrared lamp, 16 is motor, the aperture on 17 baffle plates.
Arc surfaced baffle plate synoptic diagram in Fig. 2 crystal growing apparatus of the present invention, Fig. 3 are positive umbrella-shaped baffle synoptic diagram in the crystal growing apparatus of the present invention.
(5) embodiment
The growth of embodiment 1. Large KDP crystalline
Solid phosphoric acid potassium dihydrogen (KH
2PO
4, KDP) crystal raw material is 1.5 kilograms, and growth solution is 7.1 liters of potassium dihydrogen phosphate aqueous solutions, and the temperature of saturation of solution is 52 ℃, and seed crystal adopts and the transparent Z pellet of KDP.
Concrete steps are as follows:
1. first solid K DP crystal raw material with 1.5 kilograms adds the growth container bottom, add baffle plate, will 60 ℃ down the potassium dihydrogen phosphates of preparation behind ultra-fine filtering with microporous membrane, add in the container 7.1 liters, vitellarium, top solution temperature is set at 24 hours seed crystals to be put of 54 ℃ of balances.
2. seed crystal adopts transparent Z pellet, and seed size is 5.1 * 5.2 * 0.5cm
3, at 3 apertures of (001) of seed crystal direction boring, pass aperture with nylon yarn seed crystal is fixed on the carrier crystal stand, the carrier crystal stand of having fixed seed crystal is placed baking oven, be warmed up to 54 ℃ of reequilibrate of the temperature identical 12 hours with vitellarium solution.
3. seed crystal that temperature equilibrium is good and carrier crystal stand are put into above-mentioned solution, carry out the rotation of " forward-stop-reverse ".Allow the solution of vitellarium cool to the following crystal of saturation point naturally and begin growth, and then homo(io)thermism is made the crystalchecked growth on 50.5 ℃ by the degree of supersaturation of setting, adjusting the dissolve area temperature simultaneously is 54.3 ℃, crystal raw material is constantly dissolved, be transported to the vitellarium by the baffle plate hole, to replenish the used up raw material of crystal growth.The average speed of growth 3.1mm/ of crystal days.
4. crystal growth is 30 days, reach desired size, reduce the vitellarium solution temperature rallentando, cooling rate is 1 ℃/h, adjust the dissolve area temperature simultaneously and be lower than 5 ℃ of vitellarium temperature, when solution temperature reduces near room temperature, just solution can be extracted out, take out crystal, crystalline size 5.1 * 5.2 * 11.8cm
3
Embodiment 2: the growth of Large KDP crystalline
As described in embodiment 1, different is: the solid K DP crystal raw material that adds the growth container bottom is 80 kilograms, and growth solution is 560 liters of potassium dihydrogen phosphate aqueous solutions, and the temperature of saturation of solution is 52.5 ℃, and seed size is 23 * 23.5 * 1.5cm
3, the vitellarium solution temperature is set at 54.5 ℃ when putting seed crystal, and homo(io)thermism is at 51.2 ℃ during the crystalchecked growth, and the dissolve area temperature is adjusted into 54.9 ℃.The average speed of growth 1.6mm/ of crystal days.Crystal growth 330 days, crystalline size 23.5 * 24 * 63cm
3The cooling rate of solution was 0.2 ℃/h after growth was finished.
Embodiment 3: the growth of large section DKDP crystalline
As described in embodiment 1, different is: the solid phosphoric acid two deuterium potassium raw materials that add the growth container bottom are 1.1 kilograms, and growth solution is 7.2 liters of potassium dideuterium phosphate heavy aqueous solutions, and the temperature of saturation of solution is 39 ℃, and seed size is 5 * 5 * 0.5cm
3, the vitellarium solution temperature is set at 43 ℃ when putting seed crystal, and homo(io)thermism is at 38 ℃ during the crystalchecked growth, and the dissolve area temperature is adjusted into 41.5 ℃.The average speed of growth 1.0mm/ of crystal days.Crystal growth 105 days, crystalline size 5.2 * 5.3 * 12.6cm
3The cooling rate of solution was 1.2 ℃/h after growth was finished.
Embodiment 4: the growth of large section DKDP crystalline
As described in embodiment 1, different is: solid phosphoric acid two deuterium potassium (70% deuterate) raw material that adds the growth container bottom is 70 kilograms, growth solution is 550 liters of potassium dideuterium phosphate heavy aqueous solutions (78% deuterate), and the temperature of saturation of solution is 49 ℃, and seed size is 20 * 20 * 1.5cm
3, the vitellarium solution temperature is set at 52 ℃ when putting seed crystal, and homo(io)thermism is at 48 ℃ during the crystalchecked growth, and the dissolve area temperature is adjusted into 51.5 ℃.The average speed of growth 1.2mm/ of crystal days.Crystal growth 150 days, crystalline size 20.2 * 20.3 * 29.6cm
3The cooling rate of solution was 0.2 ℃/h after growth was finished.
Embodiment 5: large section primary ammonium phosphate (NH
4H
2PO
4, ADP) crystalline growth
As described in embodiment 1, different is: raw materials used is primary ammonium phosphate (NH
4H
2PO
4), the temperature of saturation of solution is 50.6 ℃, crystal growth 50 days, crystalline size 8 * 8 * 10.6cm
3
Embodiment 6: the crystal-like growing apparatus of Large KDP
Structure as shown in Figure 1, motor 1 provides power for carrier crystal stand 3, and cylinder cap 2 is arranged on the crystal growth cylinder 5, carrier crystal stand 3 is contained in the first halves in the crystal growth cylinder 5.Agitator 7 is positioned at crystal growth cylinder 5 bottoms, provides power by motor 16, and the middle and lower part is provided with a plane baffle plate 6 container is divided into upper and lower two portions in crystal growth cylinder 5.Have aperture 17 to be evenly distributed near one week of plate center on the baffle plate 6, baffle plate 6 diameters cooperate with inside diameter of vessel, and the slit of 0.5cm is arranged between the limit of baffle plate 6 and the container inner wall.Controlled separately respectively by this two-part temperature that baffle plate 6 is divided into, form high and low two warm areas, carry out the dissolving of crystal raw material and the growth of single crystal respectively, the material between two warm areas transports by the slit of design between the aperture on the baffle plate and baffle plate and container and finishes.At two warm areas temperature sensor 10, programmable logic controller 11, infrared lamp well heater 12 and temperature sensor 13, programmable logic controller 14, infrared lamp well heater 15 are housed respectively.Support 9 is arranged at crystal growth cylinder 5 bottoms, is the crystal 4 of growth below carrier crystal stand 3.
The crystal-like growing apparatus of embodiment 7. Large KDP
As described in embodiment 6, different is that baffle plate 6 is arc surfaceds.
Relevant data and the effect of embodiments of the invention 1-4 are as shown in table 1.
Table 1, the two warm area growth of single groove KDP type crystals embodiment
| Crystal type | Liquor capacity (L) | Dissolve area raw material (Kg) | The vitellarium temperature (℃) | The dissolve area temperature (℃) | The average speed of growth (mm/ days) | Growth time (my god) | Crystalline size (cm) | Crystal mass |
| KDP | 7.1 | 1.5 | 50.5 | 54.3 | 3.1 | 30 | 5.1×5.2 ×11.8 | Complete transparent no scattering particles |
| KDP | 560 | 80 | 51.2 | 54.9 | 1.6 | 330 | 23.5×24 ×63 | Complete transparent no scattering particles |
| DKDP | 7.2 | 1.1 | 38.0 | 41.5 | 1.0 | 105 | 5.2×5.3 ×12.6 | Complete transparent no scattering particles |
| DKDP | 550 | 70 | 48.0 | 51.5 | 1.2 | 150 | 20.2×20.3 ×29.6 | Complete transparent no scattering particles |
Claims (10)
1. one kind is adopted constant temperature method in conjunction with the falling temperature method cross section potassium primary phosphate of growing up next life, the method of potassium dideuterium phosphate or primary ammonium phosphate single crystal, crystal raw material is respectively the solid phosphoric acid potassium dihydrogen, the powder raw material of potassium dideuterium phosphate or primary ammonium phosphate, growth solution is to be the solution of solvent preparation with water or heavy water, seed crystal adopts the transparent Z pellet identical with growing crystal, it is characterized in that, employed growth container is become vitellarium, top and bottom dissolve area by narrow meshed barrier partitions, between described baffle plate and the described container slit is arranged, control respectively vitellarium, described top and described bottom dissolve area temperature so that: described crystal raw material dissolves at the bottom dissolve area, the dissolved crystal raw material is transported to the vitellarium, top by described aperture and described slit, crystal is grown in the vitellarium, top.
2. employing constant temperature method as claimed in claim 1 is characterized in that in conjunction with the grow up next life method of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method concrete steps are as follows:
(1) 1～1.5 times of powder raw material with solid phosphoric acid potassium dihydrogen, potassium dideuterium phosphate or primary ammonium phosphate by required growing crystal weight adds the growth container bottom, add baffle plate, to behind ultra-fine filtering with microporous membrane, add container at the solution for preparing under 35-80 ℃, vitellarium, top solution temperature will be set at the solution saturation point 2-5 ℃ of balance 24-48 hour seed crystal to be put that makes progress;
(2) seed crystal adopts transparent Z pellet, in the boring of (001) of seed crystal direction, is fixed on the carrier crystal stand, and the carrier crystal stand of having fixed seed crystal is placed baking oven, is warmed up to the temperature reequilibrate identical with vitellarium solution 12～24 hours;
(3) the Balanced carrier crystal stand that is fixed with seed crystal of temperature in the step (2) is put into the solution of step (1), carried out the rotation of " forward-stop-oppositely "; Make the solution of vitellarium cool to below the saturation point naturally, crystal begins growth, and then homo(io)thermism is made the crystalchecked growth at the following 0.5-2.5 of saturation point ℃ by the degree of supersaturation of setting, adjust the dissolve area temperature simultaneously to being higher than vitellarium temperature 2-10 ℃, the crystal raw material of container bottom is constantly dissolved, be transported to the vitellarium by the slit between baffle plate aperture and baffle plate and the container, to replenish the used up raw material of crystal growth;
When (4) treating that desired size is arrived in crystal growth, reduce the vitellarium solution temperature rallentando, adjust the dissolve area temperature simultaneously and be lower than the vitellarium temperature, when solution temperature drops to room temperature, get final product.
3. employing constant temperature method as claimed in claim 2 is in conjunction with the grow up next life method of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method, it is characterized in that, bore 2-4 aperture on the described seed crystal, pass aperture with nylon yarn or Stainless Steel Wire seed crystal is fixed on the carrier crystal stand.
4. one kind is adopted constant temperature method in conjunction with the falling temperature method cross section potassium primary phosphate of growing up next life, the device of potassium dideuterium phosphate or primary ammonium phosphate single crystal, comprise motor, carrier crystal stand, crystal growth vessel, agitator, temperature sensor, controller, well heater, it is characterized in that: in crystal growth vessel, add a baffle plate described container is divided into vitellarium, top and bottom dissolve area, having on the described baffle plate between aperture and described baffle plate and the described container has the slit, and dissolve area dissolved crystal raw material is transported to the vitellarium, top by described aperture and slit in the bottom.
5. employing constant temperature method as claimed in claim 4 is characterized in that in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method baffle shapes is flush type, arc surfaced, positive umbellate form or the umbrella shape of falling.
6. employing constant temperature method as claimed in claim 4 is characterized in that in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method the slit of 0.1～1cm is arranged between baffle edge and the container inner wall.
7. employing constant temperature method as claimed in claim 4 is characterized in that in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method baffle plate perforate mode is single hole or porous.
8. employing constant temperature method as claimed in claim 4 is in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method, it is characterized in that, in two warm areas of crystal growth vessel, a temperature sensor is housed respectively, is connected with container programmable logic controller, infrared lamp well heater outward respectively.
9. employing constant temperature method as claimed in claim 4 is characterized in that in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method support is arranged at the crystal growth vessel bottom.
10. employing constant temperature method as claimed in claim 4 is characterized in that in conjunction with the grow up next life device of cross section potassium primary phosphate, potassium dideuterium phosphate or primary ammonium phosphate single crystal of falling temperature method crystal growth vessel is the crystal growth cylinder.
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|---|---|---|---|
| CN 03139027 CN1234920C (en) | 2003-09-01 | 2003-09-01 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
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|---|---|---|---|
| CN 03139027 CN1234920C (en) | 2003-09-01 | 2003-09-01 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329563C (en) * | 2005-11-23 | 2007-08-01 | 山东大学 | Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution |
| CN100526519C (en) * | 2006-12-27 | 2009-08-12 | 钟毅 | Device for cultivating DKDP crystal with high-quality and high deuterium-content using light bath method |
| CN100560810C (en) * | 2007-09-18 | 2009-11-18 | 山东大学 | Integration type programmable crystal growth control system |
| CN101684569B (en) * | 2008-09-23 | 2012-01-04 | 宁波大学 | Method and device for growing potassium dihydrogen phosphate single crystal |
| CA2691554A1 (en) * | 2010-02-01 | 2011-08-01 | Michael Krautter | Crystal growing device |
| CN102425009B (en) * | 2011-11-29 | 2014-03-26 | 青岛大学 | KDP crystal all-dimension growing device |
| CN102534778A (en) * | 2012-03-14 | 2012-07-04 | 青岛大学 | Omnibearing growing method for KDP (Potassium Dihydrogen Phosphate) crystals |
| CN103361712B (en) * | 2012-04-09 | 2016-01-13 | 中国科学院理化技术研究所 | A kind of carrier crystal stand for the growth of Large KDP crystalloid and growth method |
| CN102862965A (en) * | 2012-09-14 | 2013-01-09 | 常熟市圆启晶体材料有限公司 | Method of dissolving monopotassium phosphate powder |
| CN104894637B (en) * | 2015-07-01 | 2017-07-28 | 清远先导材料有限公司 | The grower and growing method of a kind of crystal |
| CN105603503B (en) * | 2016-01-13 | 2018-02-06 | 重庆大学 | Planetary rotation crystal growth apparatus by solution method |
| CN105568359B (en) * | 2016-01-27 | 2017-10-31 | 济南晶艺光电技术有限公司 | The integrated growth furnace of water-soluble liquid crystal |
| CN107604441A (en) * | 2017-09-12 | 2018-01-19 | 中国电子科技集团公司第四十六研究所 | A kind of dual temperature area method crystal growing apparatus and DAST crystal growth techniques |
| CN110804759B (en) * | 2019-10-21 | 2020-12-29 | 中国科学院福建物质结构研究所 | Crystal carrying frame and KDP crystal growing method |
| CN110923812A (en) * | 2019-11-27 | 2020-03-27 | 福建福晶科技股份有限公司 | Low-temperature phase barium metaborate crystal growth method |
| CN113604882B (en) * | 2021-06-28 | 2024-03-29 | 重庆大学 | KDP crystal solution alternate flow growth method |
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