CN1330798C - System and method for growth of lithium niobate crystal with rough chemical ratio by melt injection process - Google Patents
System and method for growth of lithium niobate crystal with rough chemical ratio by melt injection process Download PDFInfo
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- CN1330798C CN1330798C CNB200410019454XA CN200410019454A CN1330798C CN 1330798 C CN1330798 C CN 1330798C CN B200410019454X A CNB200410019454X A CN B200410019454XA CN 200410019454 A CN200410019454 A CN 200410019454A CN 1330798 C CN1330798 C CN 1330798C
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Abstract
The present invention relates to a method for the growth of lithium niobate crystals in a stoichiometric ratio more or less, particularly to a system and a technology thereof for growth by a fusant injection method. Because lithium niobate crystals are not in congruent co-melting, crystallized solid components are not consistent with fusant components, and crystals with even components can not be obtained easily. The present invention provides a system which adopts a fusant injection method, and the system comprise a crystal growth furnace, a feeding furnace, a circuit regulator, a medium frequency powder supply, a manual control computer, a matched flexible member, etc. In crystal growth, balance between the growth quantity of crystals and the quantity of raw materials injected by the feeding furnace is judged, the balance of the quantity of melted raw materials injected in a growth crucible and the growth quantity of crystals is kept, and thereby, components of raw materials in the crystal growth crucible are constant. The present invention has the advantages of good feeding continuity, small fluctuation of components of crystals, good optical uniformity, high automaticity, simple device, etc., and is favorable to industrialization production. The present invention can be used for the growth of other crystals similar to non-congruent co-melting.
Description
Technical field
The present invention relates to a kind of growth of nearly stoichiometric lithium niobate crystal, particularly, belong to the crystal technique field with the system and the technology thereof of the growth of melt injection method.
Background technology
Because lithium niobate crystals is not congruent congruent melting, i.e. mole proportioning Nb: the fusion Lithium niobium trioxide melt of Li=1, the solids component and the bath composition that crystallize out are inconsistent, its Nb: Li＞1, thereby the composition of melt is constantly changed, and the crystalline solids component also constantly changes.Therefore be difficult to obtain the uniform lithium niobate crystals of composition.From mole proportioning Nb: Li=51.2: the solids component that crystallizes out 46.8 the fusion Lithium niobium trioxide melt is consistent with bath composition, can obtain the uniform lithium niobate crystals of composition with comparalive ease, but crystalline component departs from stoicheiometry.
In order to obtain the uniformly nearly stoichiometric lithium niobate crystal of composition, the technology that adopts has following several now:
1, flux method.Add potassium oxide as fusing assistant in the Lithium niobium trioxide raw material, the congruent eutectic point that is Lithium niobium trioxide is near stoicheiometry.
2, double crucible technique.When crystal growth, adopt the method for crucible set crucible, the crucible of the inside adds Nb: Li=44: 56 melt can grow the crystal of Nb: Li=1 like this.Simultaneously, along with the crystalline growth, crucible outside adds the solid material particle of Nb: Li=1.Because two crucibles are communicated with, so the composition that can keep melt is at Nb: Li=44 always: 56, obtained composition near stoichiometric lithium niobate crystal uniformly like this.
3, gas-liquid equilibrium method.The lithium niobate crystals of congruent proportioning, put into the atmosphere of rich Li, by diffusion, be that the content of Li in the lithium niobate crystals increases, thereby obtain the uniformly nearly stoichiometric lithium niobate crystal of composition.
4, zone melting method.Fusing and crystallization in microcell make that the diffusion of melt is limited in the Lithium niobium trioxide, obtain the lithium niobate crystals of nearly chemical ratio like this.
The relative merits of these methods are listed as follows:
| Technical scheme | Advantage | Shortcoming |
| Flux method | 1, method is simple.2, do not need Special Equipment. | 1, congruent eutectic point proportioning is difficult for grasping; 2, the speed of growth is slow; 3, crystalline component lack of homogeneity; 4, be difficult to the macrocrystal of growing; 5, defect concentration height; |
| Double crucible technique | 1, the macrocrystal of can growing; 2, crystalline component good uniformity; | 1, equipment complexity; 2, the reinforced control of solid is difficult for; 3, the speed of growth is slow; |
| The gas-liquid equilibrium method | 1, composition uniformity is good; | 1, is difficult to prepare thick crystal; |
| 2, optical homogeneity is good; | 2, the cycle is long; | |
| Zone melting method | 1, method is fairly simple; 2, the macrocrystal of can growing; | 1, the crystalline component fluctuation is big; 2, defect concentration height; |
Summary of the invention
The object of the invention is to overcome 4 kinds of the deficiencies in the prior art, and a kind of melt method for implanting is provided, and utilizes computer tie loop setter to constitute the control hardware system core, realizes the growth of nearly stoichiometric lithium niobate crystal.
Technical scheme of the present invention: this melt injection method nearly stoichiometric lithium niobate crystal system of growing comprises crystal growing furnace, feed stove, 2 controllable silicon controllers, 3 loop controllers, intermediate frequency power supply (31), industrial computer (32) and software kit 7 major parts:
Crystal growing furnace partly includes motor, drives the handle system of following leading screw and the crystal growth of seed rod formation, draw crystal in the melt of seed rod from crucible, it below the crucible thermopair, in its lagging material outside crucible, the crucible periphery is the ruhmkorff coil of heating usefulness, ruhmkorff coil is connected with intermediate frequency power supply, is force transducer below the lagging material.
The feed stove partly includes motor, drives the handle system of following leading screw and pull bar formation feed, promote analogue body in the melt of pull bar from crucible downwards, the crucible periphery is the Si-Mo rod ruhmkorff coil of heating usefulness, is thermopair below the crucible, and they all place the outer lagging material of crucible.
Loop controller is by thermopair and force transducer collecting temperature and deviation of weight signal, and output signal connects intermediate frequency power supply, and industrial computer is connected by serial communication with it, and controls its operation, thus the control crystal growth; Be connected with silicon controlled rectifier unit, thermopair, gather and control the temperature of feed stove; Be connected with silicon controlled rectifier unit, thermopair, gather and control the temperature of conduit.Power supply is powered to silicon controlled rectifier unit, silicon controlled rectifier unit and intermediate frequency power supply.
Built-in motion control card of industrial computer and stepper motor driver are connected with motor with motor respectively, can control crystal pull rate and analogue body lowering speed by industrial computer.Industrial computer adopts auto-control software, and control software is controlled automatically to whole crystal growing process.Be characterized in:
Between crystal growing furnace and the feed stove, connect with conduit, an end of conduit is connected on the feed crucible, and the other end links to each other with crystal growing crucible, and the melt in the feed crucible can flow via a conduit in the crystal growing crucible.
This melt injection method nearly stoichiometric lithium niobate crystal technology of growing comprises the steps:
1) raw material is prepared;
2) charging;
3) intensification melt;
4) select temperature to sow;
5) crystal growth: select auto-control software " crystal growth control ", start crystal growing furnace and lift motor, slowly lift seed rod, seed crystal is pulled out crystal according to the crystallization direction of seed crystal from fused raw material.Simultaneously, Controlling System is according to the signal of force transducer, balance between the amount of judgement crystal growth amount and feed stove injection fused raw material B, and by controlling the lowering speed of analogue body, make amount and the crystalline increment of the fused raw material B that injects growth crucible keep balance, thereby make the composition of raw material in the crystal growing crucible keep constant.
6) mention cooling: crystal stops the decline of analogue body after reaching certain increment, mentions crystal, cooling;
7) come out of the stove: when temperature drops near room temperature, come out of the stove;
Beneficial effect of the present invention: have that reinforced continuity is good, the crystalline component fluctuation is little, the good and level of automation advantages of higher of optical homogeneity, equipment is fairly simple, helps industrialization production.The present invention can be used for carrying out nearly chemical lithium niobate crystals and doped lithium columbate growth, and other similar non-congruent congruent melting crystalline growth.
Description of drawings
Fig. 1: the melt injection method nearly stoichiometric lithium niobate crystal system of growing constitutes synoptic diagram
Fig. 2: feeder system capillary vessel synoptic diagram of the present invention
Fig. 3: the control flow block diagram of crystal growth automatic control system
Among the figure: 1. motor 2. leading screws 3. seed rods 4. crystal 5s. 27. loop controllers, 28. controllable silicon unit, melt 6. insulation material 7. induction coils, 8. thermocouple 9. power sensors, 10. motor 11. leading screws, 12. pull bar 13. analogue bodies, 14. melt 15. insulation materials, 16. Si-Mo rod induction coil 17. insulation materials, 18. thermocouple 19. conduits, 20. calandria 21. insulation materials, 22. thermocouple 23. crucibles, 24. crucible 25. power supplys, 26. controllable silicon unit, 29. loop controllers, 30. loop controllers, 31. intermediate frequency power supplies, 32. industrial computers, 33. capillary vessels
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is elaborated:
As shown in Figure 1: this melt injection method nearly stoichiometric lithium niobate crystal system of growing, system comprises crystal growing furnace, feed stove, 2 controllable silicon controllers, 3 loop controllers, intermediate frequency power supply 31, industrial computer (32) and software kit 7 major parts:
Crystal growing furnace partly includes motor 1, drives the handle system of following leading screw 2 and seed rod 3 formation crystal growths, draw crystal 4 in the melt 5 of seed rod from crucible 23, it below the crucible thermopair 8, in its lagging material 6 outside crucible, the crucible periphery is the ruhmkorff coil 7 of heating usefulness, ruhmkorff coil 7 is connected with intermediate frequency power supply, is force transducer 9 below the lagging material;
The feed stove partly includes motor 10, drives the handle system of following leading screw 11 and pull bar 12 formation feed, promote analogue body 13 in the melt 14 of pull bar from crucible 24 downwards, the crucible periphery is the Si-Mo rod ruhmkorff coil 16 of heating usefulness, be thermopair 18 below the crucible, they all place the outer lagging material 17 of crucible;
Silicon controlled rectifier unit 26, silicon controlled rectifier unit 28 and intermediate frequency power supply 31 are given in power supply 25 power supplies;
Be characterized in: between crystal growing furnace and the feed stove, connect with conduit 19, one end of conduit is connected on the feed crucible 24, the other end links to each other with crystal growing crucible 23, melt in the feed crucible can flow via a conduit in the crystal growing crucible, and there are heating member 20 and lagging material 21 in the outside of conduit;
This melt injection method nearly stoichiometric lithium niobate crystal technology of growing comprises the steps:
1) raw material is prepared: A: Li molar content 58%, B: Li molar content 50%;
2) charging: the crystal growing furnace crucible A raw material of packing into, the feed stove B raw material of packing into;
3) intensification melt: start auto-control software, select " melt control ", make A raw material and B raw material all reach molten state, melt also can manually carry out under the control;
4) select temperature to sow: to select auto-control software " select temperature sow control ", Controlling System will be regulated the growth furnace crucible temperature, a little more than the Tc of raw material A, and regulate the feed furnace temperature, make it to remain on 1300 ℃, regulate conduit temperature, make it to maintain 1300 ℃, then, after confirming through operator again, fall seed rod, open rotating machine, seed crystal is immersed in the melt;
5) crystal growth: select auto-control software " crystal growth control ", the control floppy disk system will start crystal growing furnace and lift motor, slowly lift seed rod, Li molar content 50% crystal will crystallize out from fused raw material A by the crystallization direction according to seed crystal on seed crystal.Simultaneously, Controlling System is according to the signal of force transducer, balance between the amount of judgement crystal growth amount and feed stove injection fused raw material B, and by controlling the lowering speed of analogue body, make amount and the crystalline increment of the fused raw material B that injects growth crucible keep balance, thereby make the composition of raw material in the crystal growing crucible keep constant; Automatic control system calculates crystalline growth velocity, diameter, weight etc. according to the amount that enters the melt 14 of melt 5, and by loop controller 30 with lift motor 10, makes crystal 4 according to the technology growth of setting;
6) mention cooling: crystal stops the decline of analogue body after reaching certain increment, mentions crystal, cooling;
7) come out of the stove: when temperature drops near room temperature, come out of the stove;
Be characterized in: when crystal growth, start crystal growing furnace and lift motor, when slowly lifting seed rod, power supply machine drives analogue body and moves downward, fused raw material B in the feed stove simulated body and extrudes, and crawls into feed conduit by kapillary, and injects growth crucible by feed conduit; Simultaneously, Controlling System is according to the signal of force transducer, balance between the amount of judgement crystal growth amount and feed stove injection fused raw material B, and by controlling the lowering speed of analogue body, make amount and the crystalline increment of the fused raw material B that injects growth crucible keep balance, thereby make the composition of raw material in the crystal growing crucible keep constant.Automatic control system calculates crystalline growth velocity, diameter, weight etc. according to the amount that enters the melt 14 of melt 5, and by loop controller 30 with lift motor 10, makes crystal 4 according to the technology growth of setting;
Operating process of the present invention:
1) at first raw material A and raw material B are respectively charged into crucible 23 and crucible 24;
2) connect power supply 25, start the automatic control system program;
3) be connected with loop controller 27,29,30 by industrial computer 32, make feed crucible 24, conduit 19 and growth crucible 23 reach suitable temperature respectively, make raw material A, raw material B melt, and make the temperature of conduit 19 a little more than the temperature of crucible 24;
4) through after the abundant fusing, select suitable temperature to sow, and upwards lift by lifting motor 1, leading screw 2 and seed rod 3, making lithium content is that to go out lithium content in crystallization on the seed crystal be lithium niobate crystals 4 about 50mol% for the melt 5 of 58mol%;
5) automatic control system is by force transducer 9, balance between the increment of judgement crystal 4 and melt 14 enters melt 5 by conduit 19 the amount, lift the speed of motor 10 by change, the lowering speed of control analogue body 13, thereby control enters the amount of the melt 14 of melt 5, makes melt 5 lithium contents maintain 58mol%.Simultaneously, automatic control system calculates crystalline growth velocity, diameter, weight etc. according to the amount that enters the melt 14 of melt 5, and by loop controller 30 with lift motor 10, makes crystal 4 according to the technology growth of setting;
6) after crystal 4 grows into suitable weight, mention crystal 4, make it to break away from, mention analogue body 13 simultaneously with melt 5, and cooling, in the time of will arriving near room temperature, crystal 4 just can be come out of the stove;
7) the raw material B in the additional crucible 24 just can repeat said process, carries out the growth second time.
Claims (3)
1. a melt injection method nearly stoichiometric lithium niobate crystal system of growing, system comprises crystal growing furnace, feed stove, 2 controllable silicon controllers, 3 loop controllers, intermediate frequency power supply (31), industrial computer (32) and software kit 7 major parts:
Crystal growing furnace partly includes motor (1), drives the handle system of following leading screw (2) and the crystal growth of seed rod (3) formation, draw crystal (4) in the melt (5) of seed rod from crucible (23), below the crucible thermopair (8), in its lagging material (6) outside crucible, the crucible periphery is the ruhmkorff coil (7) of heating usefulness, ruhmkorff coil (7) is connected with intermediate frequency power supply, is force transducer (9) below the lagging material;
The feed stove partly includes motor (10), drives the handle system of following leading screw (11) and pull bar (12) formation feed, promote analogue body (13) in the melt (14) of pull bar from crucible (24) downwards, the crucible periphery is the Si-Mo rod ruhmkorff coil (16) of heating usefulness, be thermopair (18) below the crucible, they all place the outer lagging material (17) of crucible;
Loop controller (30) is by thermopair (8) and force transducer (9) collecting temperature and deviation of weight signal, and output signal connects intermediate frequency power supply (31), and industrial computer (32) is connected by serial communication with it, and controls its operation, thus the control crystal growth;
Loop controller (27) is connected with silicon controlled rectifier unit (26), thermopair (18), gathers and control the temperature of feed stove, and industrial computer (32) links to each other with loop controller (27) by serial communication, and control loop setter (27);
Loop controller (29) is connected with silicon controlled rectifier unit (28), thermopair (22), gathers and control the temperature of conduit (19), and industrial computer links to each other with loop controller (29) by serial communication, and control loop setter (29);
Silicon controlled rectifier unit (26), silicon controlled rectifier unit (28) and intermediate frequency power supply (31) are given in power supply (25) power supply;
Built-in motion control card of industrial computer (32) and stepper motor driver are connected with motor (2) with motor (1) respectively, can control crystal (4) pull rate and analogue body (13) lowering speed by industrial computer (32);
Industrial computer (32) adopts auto-control software, and control software is controlled automatically to whole crystal growing process;
It is characterized in that:
Between crystal growing furnace and the feed stove, connect with conduit (19), one end of conduit is connected on the feed crucible (24), the other end links to each other with crystal growing crucible (23), melt in the feed crucible can flow via a conduit in the crystal growing crucible, and there are heating member (20) and lagging material (21) in the outside of conduit.
2. according to the said melt injection method of the claim 1 nearly stoichiometric lithium niobate crystal system of growing, it is characterized in that: conduit (19) links to each other with a capillary vessel (33) on crucible (24) wall, melt is because capillarity rising certain altitude in conduit (33), when melt rises to the height of conduit (19) mouth, melt will enter conduit (19), enter crystal growing crucible (23) along conduit (19).
3. a melt injection method nearly stoichiometric lithium niobate crystal technology of growing, it comprises the steps:
1) raw material is prepared: A: Li molar content 58%, B: Li molar content 50%;
2) charging: the crystal growing furnace crucible A raw material of packing into, the feed stove B raw material of packing into;
3) intensification melt: start auto-control software, select " melt control ", make A raw material and B raw material all reach molten state, melt also can manually carry out under the control;
4) select temperature to sow: to select auto-control software " select temperature sow control ", Controlling System will be regulated the growth furnace crucible temperature, a little more than the Tc of raw material A, and regulate the feed furnace temperature, make it to remain on 1300 ℃, regulate conduit temperature, make it to maintain 1300 ℃, then, after confirming through operator again, fall seed rod, open rotating machine, seed crystal is immersed in the melt;
5) crystal growth: select auto-control software " crystal growth control ", the control floppy disk system will start crystal growing furnace and lift motor, slowly lift seed rod, Li molar content 50% crystal will crystallize out from fused raw material A by the crystallization direction according to seed crystal on seed crystal.Simultaneously, Controlling System is according to the signal of force transducer, balance between the amount of judgement crystal growth amount and feed stove injection fused raw material B, and by controlling the lowering speed of analogue body, make amount and the crystalline increment of the fused raw material B that injects growth crucible keep balance, thereby make the composition of raw material in the crystal growing crucible keep constant; Automatic control system calculates crystalline growth velocity, diameter, weight etc. according to the amount that enters the melt (14) of melt (5), and by loop controller (30) with lift motor (10), crystal (4) is grown according to the technology of setting;
6) mention cooling: crystal stops the decline of analogue body after reaching certain increment, mentions crystal, cooling;
7) come out of the stove: when temperature drops near room temperature, come out of the stove;
It is characterized in that: when crystal growth, start crystal growing furnace and lift motor, when slowly lifting seed rod, feed stove driven by motor analogue body moves downward, fused raw material B in the feed stove simulated body and extrudes, crawl into feed conduit by kapillary, and by feed conduit injection growth crucible, simultaneously, Controlling System is according to the signal of force transducer, judges that crystal growth amount and feed stove inject the balance between the amount of fused raw material B, and the lowering speed by the control analogue body, make amount and the crystalline increment of the fused raw material B that injects growth crucible keep balance, thereby make the composition of raw material in the crystal growing crucible keep constant; Automatic control system calculates crystalline growth velocity, diameter, weight etc. according to the amount that enters the melt (14) of melt (5), and by loop controller (30) with lift motor (10), crystal (4) is grown according to the technology of setting.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410019454XA CN1330798C (en) | 2004-05-31 | 2004-05-31 | System and method for growth of lithium niobate crystal with rough chemical ratio by melt injection process |
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| CNB200410019454XA CN1330798C (en) | 2004-05-31 | 2004-05-31 | System and method for growth of lithium niobate crystal with rough chemical ratio by melt injection process |
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| CN1330798C true CN1330798C (en) | 2007-08-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100398701C (en) * | 2006-09-15 | 2008-07-02 | 嘉兴学院 | Method for treating crystal growth raw material |
| WO2019186870A1 (en) * | 2018-03-29 | 2019-10-03 | 株式会社クリスタルシステム | Single crystal manufacturing device and single crystal manufacturing method |
| EP3572560A4 (en) | 2018-03-29 | 2020-01-22 | Crystal Systems Corporation | Single crystal manufacturing device and single crystal manufacturing method |
| CN110067019A (en) * | 2019-06-03 | 2019-07-30 | 中国电子科技集团公司第二十六研究所 | A kind of continuous automatic feeding device of crystal growth and crystal continuous growing system |
| CN112520437B (en) * | 2020-11-23 | 2021-07-06 | 眉山博雅新材料有限公司 | Charging control method and system |
Citations (1)
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| JPS5148077B2 (en) * | 1971-12-28 | 1976-12-18 |
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| JPS5148077B2 (en) * | 1971-12-28 | 1976-12-18 |
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