CN113046820A - KDP crystal one-dimensional reciprocating motion growth method - Google Patents
KDP crystal one-dimensional reciprocating motion growth method Download PDFInfo
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- CN113046820A CN113046820A CN202110284799.1A CN202110284799A CN113046820A CN 113046820 A CN113046820 A CN 113046820A CN 202110284799 A CN202110284799 A CN 202110284799A CN 113046820 A CN113046820 A CN 113046820A
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- reciprocating motion
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- 239000013078 crystal Substances 0.000 title claims abstract description 86
- 230000033001 locomotion Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000012982 microporous membrane Substances 0.000 claims description 3
- 238000013021 overheating Methods 0.000 claims description 3
- 239000012047 saturated solution Substances 0.000 claims description 3
- 230000002441 reversible effect Effects 0.000 abstract description 10
- 238000011426 transformation method Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract description 2
- 238000002109 crystal growth method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000004308 accommodation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 239000007836 KH2PO4 Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
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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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
-
- 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
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The project relates to a KDP crystal one-dimensional reciprocating motion growth method which has two advantages. Firstly, three flow areas which are easy to form the wrappage existing in the traditional crystal transformation method, two-dimensional movement method and three-dimensional movement method are avoided: an incident flow stagnation area, a back flow convection vortex cell area and a downstream area of a side wall boundary layer; and secondly, the one-dimensional symmetry of the KDP crystal is fully utilized, reversible shear flow is realized by reciprocating motion, the reversible shear flow has excellent hydrodynamic conditions for growing high-quality crystals, and the method is a theoretically predicted crystal face morphology constant-stability mode. The method is beneficial to realizing rapid growth of the KDP crystal with high quality, and provides a better solution for the KDP crystal with large size and high quality required by an inertial confinement laser nuclear fusion (ICF) laser device.
Description
Technical Field
The invention belongs to the field of artificial crystal growth, and particularly relates to a KDP crystal one-dimensional reciprocating motion growth method which is suitable for rapid high-quality all-dimensional growth of KDP crystals.
Background
KDP(KH2PO4Monopotassium phosphate) crystal is a water-soluble crystal, has excellent optical characteristics and a higher laser damage threshold, is easy to realize phase matching, can grow a large-size crystal, and is a preferred material for a frequency doubling converter and an electro-optical switch in inertial confinement laser nuclear fusion (ICF). In the KDP crystal growth, the thickness of a boundary layer is reduced by crystal rotation to improve the crystal growth speed, and the method is called a crystal transformation method. The crystal transformation method has a fatal weakness, namely a crystal face has three flowing areas which are easy to form a wrapping object: the system comprises an incident flow stagnation area, a back flow convection vortex cell area and a downstream area of a side wall boundary layer. The existence of the regions easily destabilizes the crystal surface morphology, thereby influencing the quality of the grown crystal. The crystal growth method by two-dimensional or three-dimensional movement is complementary by the advantages and disadvantages of periodicity, so that the crystal growth quality is improved, but the problems cannot be completely solved, and three unfavorable flow areas still exist. Theoretical analysis indicates that reversible shear flow, alternate forward and reverse of shear flow by 180 degrees, can ensure the crystal face morphology to be stable, and is the hydrodynamic condition which is most beneficial to growing high-quality crystals. However, reversible shear flow requires the fluid to be inertially free, achieving 180 degrees of reverse flow, which is practically impossible. Potapenko [ Potapenko, SY. Formation of accommodation flow, journal of accommodation growth,1998,186(3) ]446-]The conclusion that the reversible shear flow stabilizes the face against any disturbance has not been practical, and is certainly an unfortunate one.
Disclosure of Invention
Aiming at the defects of the KDP crystal growth method, the invention provides a quick and high-quality KDP crystal growth method. The method can not only utilize convection to enhance solute transport, but also fully utilize the one-dimensional symmetry characteristic of the crystal, realize reversible shear flow by the one-dimensional reciprocating motion of the crystal, and improve the quality of the grown crystal.
The technical solution of the invention is as follows:
a KDP crystal one-dimensional reciprocating motion growth method is characterized by comprising the following steps:
1) preparing a growth solution: preparing a saturated solution at the temperature of 45-75 ℃ according to a solubility formula;
2) filtering and overheating the solution: filtering the solution with microporous membrane to obtain pure clear solution; the pure clear liquid is overheated for more than 24 hours at the constant temperature of 15-20 ℃ above the saturation temperature to prepare a growth solution;
3) seed crystal fixing: sticking the cut seed crystal to the top end of a crystal pulling rod, wherein the z direction is vertical to the crystal pulling rod;
4) installing and sealing the growing device: placing a crystal incubator filled with a growth solution in a program temperature control water bath, maintaining the temperature of the water bath slightly higher than the saturation temperature, placing a crystal pulling rod adhered with seed crystals above the crystal incubator, connecting the upper end of the crystal pulling rod to a reciprocating mechanism, and sealing the growth container;
5) crystal growth: slowly adding seed crystals into the growth solution after heat balance, cooling to below the saturation temperature after slight dissolution, and starting a controller to start crystal growth; the crystal does one-dimensional reciprocating motion in a horizontal plane, the speed range of the reciprocating motion is 0.02-0.2 m/s, and the distance range is 0.05-0.5 m.
Compared with the prior art, the KDP crystal one-dimensional reciprocating motion growth method has the following advantages:
1) the flow areas which are easy to cause the formation of the wrappage are avoided by a crystal transformation method and inevitable three flow areas of incident flow, side flow and wake flow of a crystal two-dimensional and three-dimensional movement methods. The reversible shear flow is realized by utilizing the buffer drainage and the alternate reciprocating motion of the conical surfaces at two sides with one-dimensional symmetry, and the growth quality of the crystal is expected to be greatly improved.
2) The crystal can grow rapidly in all directions.
Drawings
FIG. 1 is a schematic diagram of the KDP crystal one-dimensional reciprocating motion growing method and apparatus of the present invention;
FIG. 2 is a vector diagram of the velocity near the surface of the crystal after the left and right movement of the crystal is reversed;
Detailed Description
The present invention will be described in further detail below by way of examples with reference to the accompanying drawings, which are not intended to limit the scope of the invention.
A KDP crystal one-dimensional reciprocating motion growth method comprises the following five steps:
1) preparing a growth solution: preparing a saturated solution at the temperature of 45-75 ℃ according to a solubility formula;
2) filtering and overheating the solution: filtering the solution with microporous membrane to obtain pure clear solution; the pure clear liquid is overheated for more than 24 hours at the constant temperature of 15-20 ℃ above the saturation temperature to prepare a growth solution;
3) fixing seed crystal 1: sticking the cut seed crystal 1 on the top end of a crystal pulling rod 4, wherein the z direction is vertical to the crystal pulling rod 4;
4) installing and sealing the growing device: placing a crystal incubator 3 containing a growth solution in a program temperature control water bath, maintaining the temperature of the water bath slightly higher than the saturation temperature, placing a crystal pulling rod 4 adhered with seed crystals 1 above the liquid level in the crystal incubator 3, connecting the upper end of the crystal pulling rod to a reciprocating mechanism 6, and sealing the growth container by using a foldable organic film material 5;
5) crystal growth: slowly dropping seed crystals into the growth solution after heat balance, cooling to below saturation temperature after slight dissolution, starting the one-dimensional reciprocating motion controller 7 to start crystal growth, wherein the controller 7 can adjust and control the motion direction, speed and distance of the crystal pulling rod 4. The crystal 2 is reciprocated in one dimension in the horizontal plane as indicated by the arrows in fig. 1. FIGS. 2a and b are velocity vector diagrams (note: coordinate system is established on the crystal) near the left and right motion crystal planes of the crystal, respectively. When the crystal moves to the left (FIG. 2a), the solution flows through the crystal face from the left to the right; as the crystal moves to the right (fig. 2b), the solution flows across the lattice planes from right to left, and a reversible shear flow forms. The reciprocating speed range is 0.02-0.2 m/s, and the distance range is 0.05-0.5 m.
Claims (1)
1. A KDP crystal one-dimensional reciprocating motion growth method is characterized by comprising the following steps:
1) preparing a growth solution: preparing a saturated solution at the temperature of 45-75 ℃ according to a solubility formula;
2) filtering and overheating the solution: filtering the solution with microporous membrane to obtain pure clear solution; the pure clear liquid is overheated for more than 24 hours at the constant temperature of 15-20 ℃ above the saturation temperature to prepare a growth solution;
3) seed crystal fixing: sticking the cut seed crystal to the top end of a crystal pulling rod, wherein the z direction is vertical to the crystal pulling rod;
4) installing and sealing the growing device: placing a crystal incubator filled with a growth solution in a program temperature control water bath, maintaining the temperature of the water bath slightly higher than the saturation temperature, placing a crystal pulling rod adhered with seed crystals above the crystal incubator, connecting the upper end of the crystal pulling rod to a reciprocating mechanism, and sealing the growth container;
5) crystal growth: slowly adding seed crystals into the growth solution after heat balance, cooling to below the saturation temperature after slight dissolution, and starting a controller to start crystal growth; the crystal does one-dimensional reciprocating motion in a horizontal plane, the speed range of the reciprocating motion is 0.02-0.2 m/s, and the distance range is 0.05-0.5 m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110284799.1A CN113046820A (en) | 2021-03-16 | 2021-03-16 | KDP crystal one-dimensional reciprocating motion growth method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110284799.1A CN113046820A (en) | 2021-03-16 | 2021-03-16 | KDP crystal one-dimensional reciprocating motion growth method |
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| CN113046820A true CN113046820A (en) | 2021-06-29 |
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| CN202110284799.1A Pending CN113046820A (en) | 2021-03-16 | 2021-03-16 | KDP crystal one-dimensional reciprocating motion growth method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233285A (en) * | 2022-07-20 | 2022-10-25 | 江西新余新材料科技研究院 | Crystal growth apparatus and method, and TGS-based crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060888A (en) * | 2013-01-08 | 2013-04-24 | 重庆大学 | Method for growing crystals in crystal three-dimension motion solution |
| US20190136403A1 (en) * | 2017-10-21 | 2019-05-09 | Shanghai Institute Of Optics And Fine Mechanics, Chinese Academy Of Sciences | Method for limiting growth of kdp-type crystals with a long seed |
-
2021
- 2021-03-16 CN CN202110284799.1A patent/CN113046820A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060888A (en) * | 2013-01-08 | 2013-04-24 | 重庆大学 | Method for growing crystals in crystal three-dimension motion solution |
| US20190136403A1 (en) * | 2017-10-21 | 2019-05-09 | Shanghai Institute Of Optics And Fine Mechanics, Chinese Academy Of Sciences | Method for limiting growth of kdp-type crystals with a long seed |
Non-Patent Citations (4)
| Title |
|---|
| 于杰;余娜;王杜娟;卢雯婷;: "KDP晶体生长工艺研究", 昆明理工大学学报(理工版), no. 03, pages 20 - 23 * |
| 周川;李明伟;尹华伟;崔启栋;胡志涛;: "不同运动方式KDP单晶生长流动与物质输运数值分析", 材料导报, no. 02, pages 136 - 141 * |
| 王少丽;常新安;臧和贵;陈学安;: "KDP/DKDP晶体生长研究近况", 硅酸盐通报, no. 03, pages 554 - 559 * |
| 王邦国;李明伟;周川;尹华伟;: "三维运动下KDP晶体生长过程中的应力分析", 人工晶体学报, no. 12, pages 3099 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233285A (en) * | 2022-07-20 | 2022-10-25 | 江西新余新材料科技研究院 | Crystal growth apparatus and method, and TGS-based crystal |
| CN115233285B (en) * | 2022-07-20 | 2024-03-15 | 江西新余新材料科技研究院 | Crystal growth device and method and TGS crystal |
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