CN1329563C - Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution - Google Patents
Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution Download PDFInfo
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- CN1329563C CN1329563C CNB2005100451469A CN200510045146A CN1329563C CN 1329563 C CN1329563 C CN 1329563C CN B2005100451469 A CNB2005100451469 A CN B2005100451469A CN 200510045146 A CN200510045146 A CN 200510045146A CN 1329563 C CN1329563 C CN 1329563C
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Abstract
The present invention discloses a new high-temperature processing technology of potassium dideuterium phosphate crystal growth solution. The new technology comprises the following steps: (1) concentration increase comprises: solution is heated above 105 DEG C for boiling, so that the solution reaches saturation, until crystallization can not be separated out; (2) stir comprises: the solution is stirred at high speed, and is cooled to room temperature within 10 hours; (3) dissolution comprises: the temperature of the cooled solution is raised under the condition of being continuously stirred, until the crystallization is completely dissolved; (4) super fine filter comprises: the solution is filtered by using a filter core below 0.2 micrometer. The present invention decreases soluble impurities and insoluble impurities in the solution, greatly improves the stability of the solution, decreases the diffusion of the crystal, and improves the growth speed of the crystal; a grown DKDP crystal has good optical uniformity.
Description
Technical field
The present invention relates to the high-temperature processing technology of DKDP solution, belong to inorganic nonlinear material field.
Background technology
Potassium dideuterium phosphate (DKDP) crystal is not only important electro-optic crystal, be widely used in the laser Q-switching technology, and be important nonlinear material, can realize two, three, four letters frequently to 1.06 microns laser, important application arranged in that laser frequency is technical, in laser fusion, up to the present be best laser frequency material particularly.Solution is the mother liquor of water-soluble crystal growth, and the state of solution almost is to have determined the characteristic and the crystal mass of crystal growth congenitally and cultivated the crystalline success or failure.The crystal scattering of the solution growth of traditional method preparation is serious, lack of homogeneity, quality instability.The DKDP crystal is from valuable heavy water (D
2O) growth from solution adopts to prepare to directly apply to the DKDP crystal growth after solution filters, middle no any processing at present.The handling problem of DKDP crystal growth solution never is well solved for a long time, and few for a long time when this makes scattering particles in the crystal, the crystal mass instability has influenced the application of DKDP crystal at some key areas.The handling problem of DKDP crystal growth solution is the key that improves its quality.
Summary of the invention
The present invention is directed to the deficiency that above-mentioned prior art exists, but a kind of pyroprocessing novel process that reduces the DKDP crystal growth solution of scattering particles in the solution, solution transmitance height stable crystal quality is provided.
The present invention adopts following solution:
The pyroprocessing novel process of this DKDP crystal growth solution may further comprise the steps:
(1), increase concentration, boiling more than the heated solution to 105 ℃, and solution is reached capacity is no longer separated out till the xln;
(2), stir, above-mentioned solution is stirred fast, at 10 hours internal cooling to room temperature; In this process, water-insoluble substance particularly organism class is constantly assembled and is become big along with the reduction of temperature;
(3), dissolving, under continue stirring, with above-mentioned cooled solution heat up crystallization is dissolved fully till;
(4), hyperfine filtration, with the above-mentioned solution of the filter element filtering below 0.2 micron.
The DKDP solution transmitance that obtains through above-mentioned steps is significantly improved, and the scattering particles in the solution obviously tail off, and is and fills the air shape, and particle attenuates.
The present invention has reduced soluble impurity and the insoluble impurities in the solution, the probability of heterogeneous nucleation reduces greatly, the stability of solution has had very big raising, the DKDP crystal that grows, optical good uniformity not only, reduced the crystalline scattering, also solved the monocline phase interferential problem in the DKDP crystal growth, and improved crystalline growth velocity.
Description of drawings
Fig. 1 is the transmittance curve figure that gets the A sample with the spectrophotometric instrumentation.
Fig. 2 is the transmittance curve figure that gets the B sample with the spectrophotometric instrumentation.
Embodiment
Embodiment:
Produce DKDP crystal growth solution (composition of this solution is the same with existing DKDP crystal growth solution) according to the following steps:
(1), increases concentration, boiling more than the heated solution to 105 ℃, and till under this temperature solution being reached capacity, being as the criterion not separate out crystallization;
(2), stir, the motor of above-mentioned solution with 3000 rev/mins of kinds stirred fast, at 10 hours internal cooling to room temperature.In this process, water-insoluble substance particularly organism class is constantly assembled and is become big along with the reduction of temperature;
(3), dissolving, under continue stirring, with above-mentioned cooled solution heat up crystallization is dissolved fully till;
(4), hyperfine filtration, with 316L Stainless Steel Filter, the filter paper below 0.2 micron or the above-mentioned solution of filter element filtering.This solution can be directly used in the growth of DKDP crystalline.
Solution before will handling without above-mentioned steps is got 5ml and is diluted one times with test tube, is sampled as A.With the transmitance that the spectrophotometric instrumentation is got the A sample, its transmittance curve is seen Fig. 1.Solution after above-mentioned steps is handled is got 5ml and diluted one times with test tube, be sampled as B.With the transmitance that same spectrophotometric instrumentation is got the B sample, its transmittance curve is seen Fig. 2.The mensuration of the transmitance of sampling sees the following form:
To the mensuration of sampling transmitance, the result is as follows:
| Wavelength (nm) | Sample A transmitance (%) | Sample B transmitance (%) |
| 1600 | 38.2448 | 40.9393 |
| 1550 1500 | 46.5983 61.9017 | 49.8547 66.377 |
| 1450 | 63.1926 | 68.0114 |
| 1400 | 60.9062 | 65.63 |
| 1350 | 69.0829 | 73.5364 |
| 1300 | 69.4385 | 73.9138 |
| 1250 | 80.7151 | 85.9218 |
| 1200 | 82.9264 | 88.8911 |
| 1150 | 84.4468 | 90.6141 |
| 1100 | 84.6184 | 91.2742 |
| 1050 | 83.8539 | 90.9673 |
| 1000 | 82.887 | 90.4963 |
| 950 | 82.7257 | 91.0785 |
| 900 | 82.3076 | 91.3387 |
| 850 | 81.6789 | 91.1753 |
| 800 | 81.028 | 91.2654 |
| 750 | 79.9283 | 91.1623 |
| 700 | 78.7845 | 90.7115 |
| 650 | 77.5871 | 90.5777 |
| 600 | 76.2549 | 90.2871 |
| 550 | 74.5589 | 89.9248 |
| 500 | 72.8287 | 89.4899 |
| 450 | 70.4826 | 89.1106 |
| 400 | 67.6376 | 88.3427 |
| 350 | 63.8791 | 87.1168 |
| 300 | 55.3386 | 81.9553 |
| 250 | 39.2128 | 68.8854 |
| 200 | 10.2559 | 31.2973 |
Transmittance curve according to data and two duplicate samples in the table, susceptible of proof solution transmitance after treatment is significantly improved, water-insoluble obviously reduces in the solution, this and the observed phenomenon basically identical of scattering experiment, scattering particles in the solution before handling are apparent in view, bigger than normal, and light many of the scattering particles in the solution after handling, and particle is thinner few, fills the air shape.Therefore the DKDP crystal can be at more purified growth from solution.
Claims (1)
- The pyroprocessing novel process of 1 one kinds of potassium dideuterium phosphate crystal growth solution may further comprise the steps:(1), increase concentration, boiling more than the heated solution to 105 ℃, and solution is reached capacity is no longer separated out till the crystallization;(2), stir, above-mentioned solution is stirred fast, at 10 hours internal cooling to room temperature;(3), dissolving, under continue stirring, with above-mentioned cooled solution heat up crystallization is dissolved fully till;(4), hyperfine filtration, with the above-mentioned solution of the filter element filtering below 0.2 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100451469A CN1329563C (en) | 2005-11-23 | 2005-11-23 | Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100451469A CN1329563C (en) | 2005-11-23 | 2005-11-23 | Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1793440A CN1793440A (en) | 2006-06-28 |
| CN1329563C true CN1329563C (en) | 2007-08-01 |
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| CNB2005100451469A Expired - Fee Related CN1329563C (en) | 2005-11-23 | 2005-11-23 | Tech. for high temp. treating potassium dideuteride phosphate crystal growing solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103334156B (en) * | 2013-07-12 | 2016-03-23 | 东南大学 | A kind of optical crystal adulterating method |
| CN110609408A (en) * | 2019-10-25 | 2019-12-24 | 徐州众星显示科技有限公司 | Preparation method of liquid crystal screen crystal material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2289806Y (en) * | 1996-03-13 | 1998-09-02 | 中国科学院福建物质结构研究所 | Carrier crystal stand and its seed crystal for potassium dihydrogen phosphate large single crystal growing |
| WO1998059097A1 (en) * | 1997-06-24 | 1998-12-30 | Commissariat A L'energie Atomique | Making monocrystals in the form of plates by growth in a solution |
| CN1519397A (en) * | 2003-09-01 | 2004-08-11 | 山东大学 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
-
2005
- 2005-11-23 CN CNB2005100451469A patent/CN1329563C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2289806Y (en) * | 1996-03-13 | 1998-09-02 | 中国科学院福建物质结构研究所 | Carrier crystal stand and its seed crystal for potassium dihydrogen phosphate large single crystal growing |
| WO1998059097A1 (en) * | 1997-06-24 | 1998-12-30 | Commissariat A L'energie Atomique | Making monocrystals in the form of plates by growth in a solution |
| EP0991796A1 (en) * | 1997-06-24 | 2000-04-12 | Commissariat A L'energie Atomique | Making monocrystals in the form of plates by growth in a solution |
| CN1519397A (en) * | 2003-09-01 | 2004-08-11 | 山东大学 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
Non-Patent Citations (4)
| Title |
|---|
| Crystal growth. KDP (potassium dihydrogen phosphate) andDKDP (potassium dideuterium phosphate) Tomida,Katsuhiko,Jikken Butsurigaku Koza,Vol.Volume 13 1981 * |
| Crystal growth. KDP (potassium dihydrogen phosphate) andDKDP (potassium dideuterium phosphate) Tomida,Katsuhiko,Jikken Butsurigaku Koza,Vol.Volume 13 1981;DKDP晶体快速生长的研究 潘建国，曾金波等，人工晶体学报，第34卷第4期 2005;Polymorphism and metastable growth of DKDP Jiang,Min.Hua,Fang,Chang.Shui,Yu,Xi.Ling,Wang,Min,Zheng,Tao.Hong,J. Cryst. Growth,53(2) 1981 * |
| DKDP晶体快速生长的研究 潘建国，曾金波等，人工晶体学报，第34卷第4期 2005 * |
| Polymorphism and metastable growth of DKDP Jiang,Min.Hua,Fang,Chang.Shui,Yu,Xi.Ling,Wang,Min,Zheng,Tao.Hong,J. Cryst. Growth,53(2) 1981 * |
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