CN101876574A - Metastable zone width measuring method of KDP saturated solution in tonner crystal growth tank - Google Patents
Metastable zone width measuring method of KDP saturated solution in tonner crystal growth tank Download PDFInfo
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- CN101876574A CN101876574A CN2009101115980A CN200910111598A CN101876574A CN 101876574 A CN101876574 A CN 101876574A CN 2009101115980 A CN2009101115980 A CN 2009101115980A CN 200910111598 A CN200910111598 A CN 200910111598A CN 101876574 A CN101876574 A CN 101876574A
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Abstract
The invention relates to a metastable zone width measuring method of KDP saturated solution in a tonner crystal growth tank. In a dosing tank, after saturated KDP growth solution is prepared, the saturation temperature of the saturated solution is measured in a crystal hanging method accurately. After the consistent superheat temperature of the saturated solution is kept for 24 hours, the saturated solution is filtered and introduced into a crystal growth tank which is provided with a rapid growth crystal loading frame, seed crystals are not placed on the crystal loading frame, and the water bath temperature out of the growth tank is the same as the superheat temperature of the saturated solution. The rotation mode of the crystal loading frame is the same as that of rapid growth, and the cooling mode of the saturated solution is the same as that of rapid growth. When the temperature of the growth solution drops to the saturation temperature, the growth tank is observed. When observing that a first spontaneous crystal appears in the growth tank, the reading on a thermometer is recorded, and the difference of the temperature and the saturation temperature is the metastable zone width. By using the method, the metastable zone width of the KDP saturated solution in a large-scale crystal growth tank can be accurately measured.
Description
Technical field
The present invention relates to potassium dihydrogen phosphate single crystal growth saturated solution metastable zone width measuring method in a kind of tonner crystal growth groove.
Background technology
Potassium dihydrogen phosphate (KDP) crystal is important electric light of a class and nonlinear crystalline material, has higher optical damage threshold and less decay characteristic, is widely used for frequency multiplication, the mixing of solid state laser.Because the raising of laser output energy, tackle heavy caliber KDP crystal mutually and propose bigger requirement in size, traditional KDP growing method is in quantity and far can not satisfy the requirement of application in price, thereby promoted developing by leaps and bounds of KDP crystal method for fast growing, carrying out quick growing technology method is effective way and the research direction that obtains heavy caliber KDP crystal.
KDP solution state figure as shown in Figure 1, solid line is the solubility curve of KDP in aqueous solution among the figure, dotted line is the metastable curve of KDP in aqueous solution.Solid line and dotted line are divided into stable region, metastable region and unstable regin with whole temperature-concentration map: in the stable region, crystallization can not take place; In the metastable region, crystallization can spontaneously not take place in solution, and as seed crystal being put into the solution that is in the metastable region, crystal will be grown on seed crystal; In the unstable regin, crystallization can spontaneously take place in solution.Three zones are the most important with the metastable region, fast growth KDP crystal requires that solution state remains in the metastable region in the whole growth process from solution, can guarantee all growths and the spontaneous crystal (being stray crystal) of quick growth do not occur having a strong impact on fast on seed crystal of the solute of separating out.The size of metastable region also very easily is subjected to the influence of external condition, as growth groove size, and rate of temperature fall, growth initial temperature, solution purity etc., growth is significant fast to the KDP crystal for the metastable zone width of therefore accurate measurement growth solution.
Summary of the invention
In the quick growth course of KDP crystal,, strengthen the cooling amount at early growth period for guaranteeing the speed of growth faster.The cooling amount is too big, exceeds the metastable region, and spontaneous crystal appears in growth solution, has a strong impact on the quick growth of crystal; The cooling amount is too little, and the speed of growth of crystal is little, is difficult to realize three directions growth fast simultaneously of KDP crystal.The present invention adopts a kind of metastable zone width measuring method of new KDP saturated solution, can accurately measure the metastable zone width of the KDP saturated solution in the large-scale crystal growth groove, helps determining of the quick early growth period cooling of KDP crystal amount.
Heavy caliber KDP crystal falling temperature method fast growth is at φ a 1400 * 1600mm, and volume is to carry out in 1.7 tons the cylindrical stainless steel crystal growth cylinder.Growth apparatus as shown in Figure 2, wherein 1 for the crystal growth inner casing, 2 is cylinder cap, is 3 crystal growth outer shells, 4 is the engineering plastics overcoat, 5 is the well heater of cleansing bath tub, 6 is the stirrer of cleansing bath tub, 7 is carrier crystal stand, 8 is saturated KDP growth solution, 9 is thermometer.KDP point seed crystal is fixed on 9 li one-tenth awl 15 growths of saturated KDP growth solution of putting into crystal growth inner casing 1 on the carrier crystal stand 8 during growth, and thermometer 9 is measured growth temperatures.In order to guarantee the heavy caliber KDP crystal of growing, saturated solution has enough salt amounts of folding, and the saturation temperature of general solution is 60-75 ℃.
In dosage bunker, add the KDP powder, add the ultrapure water that forms through the rich ultrapure filtration system filters of overstocked reason again, after intensification, high-speed stirred are mixed with saturated KDP growth solution, with hanging the saturation temperature that brilliant method is accurately measured saturated solution.The overheated constant temperature of saturated solution 24 hours filters to import and is equipped with in the crystal growth groove of quick growth carrier crystal stand, does not put seed crystal on the carrier crystal stand, and the outer bath temperature of growth groove is identical with the saturated solution overtemperature.The rotation mode of carrier crystal stand is identical with the rotation mode of growth fast, and the cooling pattern of saturated solution is identical with the cooling pattern of growth fast.When the growth solution temperature is reduced to saturation temperature, begin to observe the growth groove.When first spontaneous crystallization occurring in observing the growth groove, note temperature reading, this temperature and saturation temperature difference are metastable zone width.
Beneficial effect of the present invention is: this method can accurately be measured the metastable zone width of the KDP saturated solution in the large-scale crystal growth groove, help determining of the quick early growth period cooling of KDP crystal amount, fast growth KDP crystal solution state in whole growth process remains in the metastable region, can guarantee all growths and the spontaneous crystal of quick growth do not occur having a strong impact on fast on seed crystal of the solute of separating out.
Description of drawings
Fig. 1 is KDP solution state figure; Fig. 2 is heavy caliber KDP crystal growth equipment figure.
Embodiment
Embodiment 1: in being of a size of φ 1400 * 1600mm dosage bunker, the KDP powder of the AR level that Shanghai reagent two factories of adding 900Kg produce adds 1.3 tons of ultrapure waters that form through the rich ultrapure filtration system filters of overstocked reason again, and its conductivity reaches 18.2M Ω cm.Heat up, after high-speed stirred is mixed with saturated KDP growth solution, accurately to measure the saturation temperature of saturated solution be 72.5 ℃ with hanging brilliant method.Be warming up to 80 ℃, overheated constant temperature 24 hours.Solution through the secondary micropore filter element continuous filtration of 0.22 μ and 0.1 μ, imports and is equipped with in the crystal growth groove of quick growth carrier crystal stand in closed system.The growth carrier crystal stand is up and down the plectane of 1 meter of diameter fast, and middle the connection highly is 1 meter four blocks of straight plate.The outer bath temperature of crystal growth groove is 80 ℃, begins cooling with 1 ℃ of/day speed, and the mask pattern rotation mode is according to " just changeing-stall-counter-rotating ", and rotating speed is 70 rev/mins.Observed growth groove and recording thermometer reading every 3 hours.Observe when occurring first glittering granule stray crystal in the growth groove on the carrier crystal stand, noting temperature reading is 67.0 ℃.Under these process conditions, crystal growth groove KDP solution metastable zone width is 5.5 ℃, and the maximum cooling amount of growing fast is no more than 5.5 ℃.
Claims (1)
1. KDP saturated solution in tonner crystal growth tank metastable zone width measuring method, it is characterized in that: in dosage bunker, add the KDP powder, add the ultrapure water that forms through the rich ultrapure filtration system filters of overstocked reason again, after intensification, high-speed stirred are mixed with saturated KDP growth solution, with hanging the saturation temperature that brilliant method is accurately measured saturated solution; The overheated constant temperature of saturated solution 24 hours filters to import and is equipped with in the crystal growth groove of quick growth carrier crystal stand, does not put seed crystal on the carrier crystal stand, and the outer bath temperature of growth groove is identical with the saturated solution overtemperature; The rotation mode of carrier crystal stand is identical with the rotation mode of growth fast, and the cooling pattern of saturated solution is identical with the cooling pattern of growth fast; When the growth solution temperature is reduced to saturation temperature, begin to observe the growth groove; When first spontaneous crystallization occurring in observing the growth groove, note temperature reading, this temperature and saturation temperature difference are metastable zone width.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618924A (en) * | 2012-04-25 | 2012-08-01 | 青岛大学 | Rapid lateral growing method of KDP (Potassium Dihydrogen Phosphate) crystals |
| CN105603525A (en) * | 2016-02-01 | 2016-05-25 | 中国科学院上海光学精密机械研究所 | Crystal carrying frame used for KDP type crystal growth |
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| CN2530961Y (en) * | 2002-03-08 | 2003-01-15 | 中国科学院福建物质结构研究所 | Large vat for crystal culture by solution method |
| CN1727522A (en) * | 2004-07-29 | 2006-02-01 | 中国科学院福建物质结构研究所 | The quick growth method of a kind of heavy caliber potassium dihydrogen phosphate single crystal |
| JP2007044639A (en) * | 2005-08-11 | 2007-02-22 | Iwate Univ | Crystallization method and crystallization apparatus |
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| US5122224A (en) * | 1989-10-30 | 1992-06-16 | The United States Of America As Represented By The United States Department Of Energy | Direct flow crystal growth system |
| CN2530961Y (en) * | 2002-03-08 | 2003-01-15 | 中国科学院福建物质结构研究所 | Large vat for crystal culture by solution method |
| CN1727522A (en) * | 2004-07-29 | 2006-02-01 | 中国科学院福建物质结构研究所 | The quick growth method of a kind of heavy caliber potassium dihydrogen phosphate single crystal |
| JP2007044639A (en) * | 2005-08-11 | 2007-02-22 | Iwate Univ | Crystallization method and crystallization apparatus |
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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 |
| CN102618924B (en) * | 2012-04-25 | 2014-07-30 | 青岛大学 | Rapid lateral growing method of KDP (Potassium Dihydrogen Phosphate) crystals |
| CN105603525A (en) * | 2016-02-01 | 2016-05-25 | 中国科学院上海光学精密机械研究所 | Crystal carrying frame used for KDP type crystal growth |
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Application publication date: 20101103 |