CN106637381A - High-precision temperature control system for crystal growth process - Google Patents
High-precision temperature control system for crystal growth process Download PDFInfo
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- CN106637381A CN106637381A CN201710068585.4A CN201710068585A CN106637381A CN 106637381 A CN106637381 A CN 106637381A CN 201710068585 A CN201710068585 A CN 201710068585A CN 106637381 A CN106637381 A CN 106637381A
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- temperature control
- growth
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- precision
- temperature
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Classifications
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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
- C30B29/14—Phosphates
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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 invention relates to a high-precision temperature control system for crystal growth process. The high-precision temperature control system comprises a growth device, a filtering device and a control device, wherein the control device consists of a PLC (programmable logic controller), a touch screen, input interfaces, output interfaces, a solid-state relay and a high-precision intelligent temperature control gauge; the PLC is connected with liquid level switches and temperature-measuring thermal resistors in the filtering device through the input interfaces, is connected with electric heaters, electromagnetic valves, circulation pumps and a conveying pump in the filtering device through the output interfaces, and is connected with an electromagnetic valve, a circulation pump and a direct current motor in the growth device; a host of the PLC is connected with the high-precision intelligent temperature control gauge through an RS485 interface, the input of the intelligent temperature control gauge is directly connected with a temperature-measuring thermal resistor in the growth device, and the output of the intelligent temperature control gauge is used for controlling an electric heater in a crystal growth tank jacket through the solid-state relay to control the temperature of growth liquid; the control precision reaches +/-0.01 DEG C. The high-precision temperature control system has the advantage that the growth quality of large-size KDP crystals is improved.
Description
Technical field
The present invention relates to novel crystal growth control system, and in particular to a kind of crystal growing process high accuracy temperature control
System, belongs to production process apparatus field.
Background technology
KDP (potassium dihydrogen phosphate, KH2PO4) crystal is that the excellent electric light of the class for growing up 30～forties of 20th century is non-
Linear optical material.Because its have larger electric light and nonlinear optical coefficients, high light injury threshold, low optical absorption,
The features such as high optical homogeneity and good transmission wave band and be widely used in laser, Electro-optical Modulation and light high-speed switch etc.
High-tech sector.
KDP crystal grows in aqueous, and the driving force of crystal growth derives from the degree of supersaturation of solution.Due to
Solubility and its temperature coefficient of the KDP type crystal in water is larger, and solution quasi stable region is also wider, therefore this type is brilliant
The growth of body generally adopts aqueous solution slow cooling method.In order to produce the KDP crystal of large scale high-quality in batches, must in growth course
Temperature control must be carried out, causes KDP solution to complete the slow cooling from 65 DEG C to 20 DEG C, temperature control essence within the time of 60 days or so
Degree must reach ± 0.01 DEG C.
A few days ago crystal growing apparatus is generally controlled using PLC, but the temperature measurement accuracy of routine PLC is ± 0.1 DEG C,
The control accuracy of requirement is not reached.The present invention is combined using PLC with high-precision intelligent temperature control table, is realizing that crystal growth is complete
While automatically controlling, desired control accuracy has been reached.
The content of the invention
In order to produce the KDP crystal of large scale high-quality in batches, the invention provides a kind of crystal growing process high precision temp
Degree control system.
The technical solution adopted in the present invention is：
Crystal growing process High-precision temperature control system includes grower, filter and control device.
(1) grower educating brilliant tank, educating growth solution temperature in brilliant tank installed in the measurement for educating brilliant tank top by jacketed
The thermal resistance of degree, installed in the carrier crystal stand educated in brilliant tank, installed in educate brilliant tank top drive carrier crystal stand positive and negative rotation direct current
Motor, installed in the electric heater educated in brilliant tank chuck, installed in educate brilliant tank chuck outside for circulate jacket water (J.W.) circulating pump,
Installed in educating the delivery port of brilliant tank chuck upper side, the cooling water inlet of chuck lower side and installed in cooling water inlet pipe
The solenoid valve block controlled into chuck cooling water on road into.
(2) filter is made up of hot water bath peace Hengshui bath；Hot water bath is by hot water storgae, on hot water storgae
The bikini liquid level sensor of water level, connection carry out self-fertile in the thermal resistance of coolant-temperature gage, measurement hot water storgae in the measurement hot water storgae of side
The pipeline of the conveying growth solution of brilliant tank, the electric heater of water in heat hot water groove in hot water storgae, for hot water
Water in groove carries out the conveying coiled pipe of growth solution of heat exchange, growth solution delivery pump, growth solution filter, is arranged on
Circulating pump, the delivery port of hot water storgae upper side, the hot water storgae lower side of the water that hot water storgae outside is used in cycling hot tank
Cooling water inlet and the solenoid valve block controlled into hot water storgae cooling water on cooling water inlet pipe road into；Balance water-bath
Groove is balanced the thermal resistance of coolant-temperature gage in tank, measurement and is balanced in tank by tank, the measurement above balance tank is balanced
The bikini liquid level sensor of water level, installed in balance tank in heating equilibrium water groove in water electric heater, for
Water in balance tank carries out the conveying coiled pipe of growth solution of heat exchange, growth solution filter, connection and returns to and educate crystalline substance
The pipeline of the conveying growth solution of tank, circulating pump, balance installed in balance tank outside for the water in cyclic balance tank
The delivery port of tank upper side, the cooling water inlet for balancing tank lower side and the control on cooling water inlet pipe road
Make solenoid valve block into balance tank cooling water into.
(3) control device is by PLC, touch-screen, input interface, output interface, solid-state relay and high-precision intelligent temperature
Control table is constituted, and PLC is made up of the DVP20ES200T types main frame and DVP04PT-E2 type thermal resistance input modules of Delta, and PLC leads to
Cross serial port of host computer to be connected with Delta DOP-W127B type liquid crystal touch screens；PLC is by two three in input interface and filter
Point type liquid-level switch and two thermometric thermal resistances are connected, PLC by two electric heaters in output interface and filter, two
Individual magnetic valve, two circulating pumps and delivery pump are connected, PLC by a magnetic valve in output interface and grower,
One circulating pump, a direct current generator are connected；PLC main frames are connected by RS485 interfaces with high-precision intelligent temperature control table, high
The control table of precision intelligent temperature is the AIJ-5.0A-N-GA-N-N-SA type tables of Yu electricity companies；The input of intelligent temperature control table is straight
Connect and be connected with thermometric thermal resistance in grower, obtain growth liquid temp, the output of intelligent temperature control table passes through solid-state relay
Device control educates the electric heater in brilliant tank chuck so as to control to grow liquid temp.
Educate in brilliant tank and fill growth solution, the nucleus that need to cultivate growth is placed on carrier crystal stand, and by PLC direct current is controlled
Machine drives carrier crystal stand staggeredly slowly to rotate at regular intervals clockwise, counterclockwise, growth solution is fully connect with nucleus
Touch.The temperature measurement accuracy of high-precision intelligent temperature control table is ± 0.001 DEG C, and the electrical heating in brilliant tank chuck is educated by control
Water in device elder generation heating jacket, then make the temperature control precision for educating growth solution in brilliant tank reach ± 0.01 by tank skin heat exchange
DEG C, holding educate in brilliant tank the temperature constant of growth solution and slowly decline in a growth cycle (60 days or so) (from
65 DEG C are slowly decreased to 25 DEG C).During slow cooling, it is important that controlling rate of temperature fall, enable crystal uniform, quick
Ground growth；PLC obtains in real time the measurement temperature of intelligent temperature control table by RS485 interfaces, and PLC is calculated according to rate of temperature fall and worked as
Growth solution temperature needed for front there is not definite value, intelligent temperature control table is sent in real time by RS485 interfaces, by intelligent temperature control
Tabulation carries out educating brilliant tank temperature control.PLC control circulating pumps make the temperature uniformity in chuck everywhere.When needing fast cooling
When, PLC controls the switch of the magnetic valve on cooling water inlet pipe road to adjust the amount into chuck cooling water.
The filter process of growth solution is：From the growth solution with granule foreign for educating outflow in brilliant tank, first stream is to warm
Water bath heating for dissolving stray crystal, then filter unrelated impurity through filter；Then flow to balance water bath, make to be back to by cooling
Educate the solution temperature in brilliant tank return to it is consistent with the solution temperature educated in brilliant tank, it is to avoid the solution in educating brilliant tank causes to disturb
It is dynamic, so as to complete continuous circulating filtration.
In order to allow temperature uniformity in hot water storgae and equilibrium water groove everywhere, match somebody with somebody respectively in hot water storgae and equilibrium water groove
Standby water-circulating pump, by PLC start and stop are controlled.By the heat exchange action of coiled pipe, temperature is T2Hot bath by coiled pipe pipeline
In growth solution temperature from T1It is heated to T2(T2=T1+ 8 DEG C), temperature is T3(T3=T1+ 0.1 DEG C) balance water-bath will be snakelike
Growth solution in pipe pipeline equilibrates to T1.PLC controls electric heater and magnetic valve is bathed into trip temperature to hot bath and equilibrium water
Adjustment, the temperature measurement accuracy of PLC is ± 0.1 DEG C, can meet use requirement.PLC in hot water storgae and equilibrium water groove three
Point type liquid level sensor signal controls magnetic valve and carries out water level adjustment to hot bath and equilibrium water bath, it is ensured that not water shortage in tank.
The Advantageous Effects of patent of the present invention are：The temperature measurement accuracy of high-precision intelligent temperature control table for ±
0.001 DEG C, control accuracy reaches ± 0.01 DEG C, and holding educates in brilliant tank the temperature constant of growth solution and in a growth cycle
Slowly decline (being slowly decreased to 25 DEG C from 65 DEG C) in (90 days or so), improve the growth quality of large-size crystals.
Description of the drawings
Patent of the present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the structure chart of crystal growing process High-precision temperature control system.
Fig. 2 is crystal continuous growth and filter apparatus configuration figure.
1 is the brilliant tank of educating of jacketed in accompanying drawing 2, and 2 is the electric heater that the water in brilliant tank chuck is educated in heating, and 3 is for following
The circulating pump of the water in ring chuck, 4 is to educate the crystal grown in brilliant tank, and 5 are mounted in the placement educated in brilliant tank gives birth to
The carrier crystal stand of long crystal, 6 are mounted in the direct current generator of the drive carrier crystal stand positive and negative rotation for educating brilliant tank top, and 7 is chuck cooling
Water inlet, 8 is chuck delivery port, and 9 is to control the magnetic valve into chuck cooling water, and 10 is total cooling water inlet；11 is hot water
Groove, 12 is the electric heater of the water in heat hot water groove, and 13 is for carrying out the conveying growth of heat exchange with the water in hot water storgae
The coiled pipe of solution, 14 is the pipeline of the conveying growth solution that connection carrys out self-fertile crystalline substance tank, and 15 is growth solution delivery pump, and 16 is heat
Growth solution filter in tank, 17 is that, for the circulating pump of the water in cycling hot tank, 18 is the delivery port of hot water storgae, 19
It is the cooling water inlet of hot water storgae, 20 is to control the magnetic valve into hot water storgae cooling water；21 is balance tank, and 22 is heating balance
The electric heater of the water in tank, 23 is for carrying out the snakelike of the conveying growth solution of heat exchange with the water balanced in tank
Pipe, 24 is the pipeline that connection returns to the conveying growth solution for educating brilliant tank, and 25 is to balance the growth solution filter in tank, 26
It is to control the magnetic valve into balance tank cooling water, 27 is that, for the circulating pump of the water in cyclic balance tank, 28 is equilibrium water
The delivery port of groove, 29 is the cooling water inlet for balancing tank；T1 is the thermal resistance that growth solution temperature in brilliant tank is educated in measurement, and T2 is
The thermal resistance of coolant-temperature gage in measurement hot water storgae, T3 is the thermal resistance for balancing coolant-temperature gage in tank；L1 is the bikini in hot water storgae
Liquid level sensor, L2 is to balance the bikini liquid level sensor in tank.
Specific embodiment
The specific embodiment of patent of the present invention is described further below in conjunction with the accompanying drawings.
A kind of application of crystal growing process High-precision temperature control system, including following implementation process：
(1) after carrying out temperature solution input work, system enters automatic running state.If first start, need to touch
The enterprising trip temperature setting of screen is touched, setting includes：Growth solution temperature T1, growth solution rate of temperature fall, heating bath temperature T2(T2=
T1+ 8 DEG C), balance bath temperature T3(T3=T1+0.1℃)。
(2) educate brilliant tank rotation control subsystem carries out positive and negative rotation control to carrier crystal stand, allow crystal aufwuchsplate equably
Touch solution.
(3) system is entered after automatic running state, and it is T to educate the growth solution temperature in brilliant tank1, temperature is flowed through for T2Heat
Coiled pipe in water-bath, stray crystal particle dissolves with the rising of growth solution temperature, and growth solution temperature reaches T2。
(4) the growth solution Jing delivery pumps in hot water bath flow through filter, filter unrelated impurity, purified solution quality.
(5) it is T that the growth solution after filtering flows into temperature3Balance water-bath in coiled pipe, growth solution temperature reduce
To with educate temperature T in brilliant tank1It is close to unanimously, eventually passes back to educate brilliant tank, completes circulation.
(6) PLC obtains in real time the measurement temperature of intelligent temperature control table by RS485 interfaces, and PLC is according to rate of temperature fall meter
Current desired growth solution desired temperature, is sent in real time intelligent temperature control table, by intelligent temperature by RS485 interfaces
Degree control table carries out educating brilliant tank temperature control.Make the temperature control precision for educating growth solution in brilliant tank reach ± 0.01 DEG C, keep
Educate in brilliant tank the temperature constant of growth solution and slowly decline in a growth cycle (90 days or so) (slow from 65 DEG C
It is reduced to 25 DEG C).
Present system can improve the growth quality of large-size crystals.
It is more than presently preferred embodiments of the present invention, any pro forma restriction, every foundation is not made to the present invention
The technical spirit of the present invention belongs to invention skill to any simple modification made for any of the above embodiments, equivalent variations and modification
In the range of art scheme.
Claims (1)
1. a kind of crystal growing process High-precision temperature control system, it is characterised in that system includes grower, filter
And control device；Control device is by PLC, touch-screen, input interface, output interface, solid-state relay and high-precision intelligent temperature
Control table is constituted, and PLC is by the two bikini liquid-level switches and two thermometric thermal resistance phases in input interface and filter
Even, PLC is by two electric heaters in output interface and filter, two magnetic valves, two circulating pumps and a conveying
Pump is connected, and PLC is connected by output interface with a magnetic valve in grower, circulating pump, a direct current generator,
PLC main frames are connected by RS485 interfaces with high-precision intelligent temperature control table；The input of intelligent temperature control table directly with growth
Thermometric thermal resistance is connected in device, obtains growth liquid temp, and the output of intelligent temperature control table is educated by solid-state relay control
Electric heater in brilliant tank chuck so as to control grow liquid temp；PLC obtains in real time intelligent temperature control table by RS485 interfaces
Measurement temperature, PLC calculates current desired growth solution desired temperature according to rate of temperature fall, real-time by RS485 interfaces
Intelligent temperature control table is sent to, is carried out educating brilliant tank temperature control by intelligent temperature control table；High-precision intelligent temperature control table
Temperature measurement accuracy be ± 0.001 DEG C, the water in the electric heater elder generation heating jacket in brilliant tank chuck is educated by control, then lead to
Crossing tank skin heat exchange makes the temperature control precision for educating growth solution in brilliant tank reach ± 0.01 DEG C, and growth solution in brilliant tank is educated in holding
Temperature constant and slowly from 65 DEG C be slowly decreased to 25 DEG C in trimestral growth cycle.
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| CN201710068585.4A CN106637381A (en) | 2017-02-08 | 2017-02-08 | High-precision temperature control system for crystal growth process |
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| CN201710068585.4A CN106637381A (en) | 2017-02-08 | 2017-02-08 | High-precision temperature control system for crystal growth process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181199A (en) * | 2018-03-16 | 2018-06-19 | 南京工业大学 | A kind of measuring device and method of suspension surface vapour pressure |
| CN109656286A (en) * | 2018-12-10 | 2019-04-19 | 湖南航天天麓新材料检测有限责任公司 | Macromolecule crystallization space material experimental provision and method |
| CN110359081A (en) * | 2019-08-08 | 2019-10-22 | 江南大学 | A kind of crystal growing process depth-width ratio control method |
| CN110408984A (en) * | 2019-08-08 | 2019-11-05 | 江南大学 | A kind of crystal high quality fast-growth control method |
| WO2023176146A1 (en) * | 2022-03-15 | 2023-09-21 | 月島機械株式会社 | Crystallization system and crystallization method |
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| CN102719878A (en) * | 2012-06-28 | 2012-10-10 | 江南大学 | Macrocrystal continuous cultivation device |
| CN103147116A (en) * | 2013-04-03 | 2013-06-12 | 江南大学 | Continuous culture and filtration system for crystals |
| CN203284495U (en) * | 2013-04-03 | 2013-11-13 | 江南大学 | Crystal continuous culture and filter system |
| CN104562175A (en) * | 2015-02-09 | 2015-04-29 | 江南大学 | Circulating mass crystal continuous culture apparatus |
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| CN102618916A (en) * | 2012-03-29 | 2012-08-01 | 江南大学 | Automatic control method for culturing and continuous filtration of crystals |
| CN102719878A (en) * | 2012-06-28 | 2012-10-10 | 江南大学 | Macrocrystal continuous cultivation device |
| CN103147116A (en) * | 2013-04-03 | 2013-06-12 | 江南大学 | Continuous culture and filtration system for crystals |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181199A (en) * | 2018-03-16 | 2018-06-19 | 南京工业大学 | A kind of measuring device and method of suspension surface vapour pressure |
| CN109656286A (en) * | 2018-12-10 | 2019-04-19 | 湖南航天天麓新材料检测有限责任公司 | Macromolecule crystallization space material experimental provision and method |
| CN109656286B (en) * | 2018-12-10 | 2021-07-30 | 湖南航天天麓新材料检测有限责任公司 | Macromolecular crystallization space material experimental device and method |
| CN110359081A (en) * | 2019-08-08 | 2019-10-22 | 江南大学 | A kind of crystal growing process depth-width ratio control method |
| CN110408984A (en) * | 2019-08-08 | 2019-11-05 | 江南大学 | A kind of crystal high quality fast-growth control method |
| CN110359081B (en) * | 2019-08-08 | 2021-02-19 | 江南大学 | Method for controlling aspect ratio in crystal growth process |
| CN110408984B (en) * | 2019-08-08 | 2021-02-19 | 江南大学 | High-quality rapid growth control method for crystal |
| WO2023176146A1 (en) * | 2022-03-15 | 2023-09-21 | 月島機械株式会社 | Crystallization system and crystallization method |
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Application publication date: 20170510 |