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CN111945225B - A control method for high saturation continuous rapid growth of crystals - Google Patents

A control method for high saturation continuous rapid growth of crystals Download PDF

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Publication number
CN111945225B
CN111945225B CN202011026213.3A CN202011026213A CN111945225B CN 111945225 B CN111945225 B CN 111945225B CN 202011026213 A CN202011026213 A CN 202011026213A CN 111945225 B CN111945225 B CN 111945225B
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crystal
tank
growth
culture tank
solution
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CN111945225A (en
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潘丰
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Jiangnan University
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Jiangnan University
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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
    • 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
    • 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
    • C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/35—Non-linear optics
    • G02F1/355—Non-linear optics characterised by the materials used
    • G02F1/3551—Crystals

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nonlinear Science (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Inorganic Chemistry (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)

Abstract

本发明涉及一种晶体高饱和度连续快速生长的控制方法，属于生产过程控制领域。晶体高饱和度连续快速生长系统包括检测装置、执行装置、控制装置和晶体生长装置。载晶架旋转停止时通过晶体尺寸视觉测量装置在线检测生长晶体的尺寸，按规则调节培养罐内生长溶液温度设定值、溶液配制罐内生长溶液温度设定值、生长溶液输送泵的转速设定值。由于溶液配制罐温度大于培养罐生长温度，从而使溶液中溶解的溶质浓度高于生长温度下的平衡溶质浓度，保证进入培养罐的溶液处于过饱和状态。本发明方法提高了大尺寸晶体的生长速度。

The present invention relates to a control method for high-saturation continuous and rapid growth of crystals, and belongs to the field of production process control. The high-saturation continuous and rapid growth system of crystals includes a detection device, an execution device, a control device and a crystal growth device. When the rotation of the crystal carrier stops, the size of the growing crystal is detected online by a crystal size visual measurement device, and the temperature setting value of the growth solution in the culture tank, the temperature setting value of the growth solution in the solution preparation tank, and the speed setting value of the growth solution delivery pump are adjusted according to the rules. Since the temperature of the solution preparation tank is greater than the growth temperature of the culture tank, the concentration of the solute dissolved in the solution is higher than the equilibrium solute concentration at the growth temperature, ensuring that the solution entering the culture tank is in a supersaturated state. The method of the present invention increases the growth rate of large-sized crystals.

Description

Control method for continuous and rapid growth of crystal with high saturation
Technical Field
The invention relates to a novel crystal growth control system, in particular to a control method for continuous and rapid growth of crystal with high saturation, and belongs to the field of production process control.
Background
KDP (potassium dihydrogen phosphate, KH 2PO4) crystals are the earliest nonlinear optical crystal materials with excellent performance, which have larger nonlinear optical coefficients, wider transmission wave bands, excellent optical uniformity and easy realization of phase matching, and have the outstanding advantages of easy growth of high-quality large-size single crystals. The high-power optical fiber has the characteristics of larger electro-optical and nonlinear optical coefficients, high optical damage threshold, low optical absorption, high optical uniformity, good transmission wave band and the like, and is widely applied to the high-technology fields of laser, electro-optical modulation, optical fast switching and the like.
Crystal growth is the control of the phase change process of a substance to obtain crystals with certain size and performance. The solution process is the longest crystal growth process. The method is characterized in that raw materials are dissolved in a solvent, crystals are precipitated in a supersaturated state according to a set mode by changing environmental conditions, single crystals are formed, and the method can be divided into tens of crystal growth technologies along with different properties of materials. The cooling method is a method for realizing crystal growth by reducing the temperature of a solution to obtain supersaturation required for crystal growth. The process is discontinuous when the crystal growth is carried out by adopting a cooling method. As the growth progresses, the total amount of solute decreases, and when the solute reaches a certain small value, the crystal will stop growing. If some method is used to continuously replenish the solute during the crystal growth process, continuous crystal growth can be achieved.
The flow method crystal growth equipment consists of a main culture tank, a overheat filtering tank, a solution preparation tank and a high saturation balance tank, and growth solution with low supersaturation degree flows back to the solution preparation tank to dissolve new raw materials. In the flow method, four links of crystal growth, overheat filtering of growth solution, solution preparation and high saturation balance of the growth solution form a closed loop, so that the crystal is always grown under the same condition. Meanwhile, raw materials can be added at any time to make up for the solute consumed in the solution preparation tank.
The flow method is favorable for growing crystals with large size and uniform quality and performance, but the method is more important to control the flow of solution besides controlling the components and the temperature of each link, so the control method is more complicated.
Disclosure of Invention
In order to rapidly produce high-quality large-size potassium dihydrogen phosphate crystals in batches, the invention provides a control method for continuous rapid growth of crystals with high saturation.
The technical scheme adopted by the invention is as follows: the control method of the continuous and rapid growth of the crystal with high saturation is realized through a continuous and rapid growth system of the crystal with high saturation, and the continuous and rapid growth system of the crystal with high saturation comprises a detection device, an execution device, a control device and a crystal growth device; the detection device comprises a culture tank thermal resistor, an overheat filter box three-point type liquid level sensor, a solution preparation tank thermal resistor, a high saturation balance box thermal resistor and a high saturation balance box three-point type liquid level sensor; the execution device comprises a crystal carriage alternating current motor, a culture tank electric heater, a culture tank water circulation pump, a culture tank electromagnetic valve, an overheat filter box electric heater, an overheat filter box water circulation pump, an overheat filter box electromagnetic valve, a solution preparation tank electric heater, a solution preparation tank water circulation pump, a solution preparation tank electromagnetic valve, a high saturation balance box electric heater, a high saturation balance box water circulation pump, a high saturation balance box electromagnetic valve and a growth solution conveying pump; the control device comprises a PLC host module, a touch screen, a thermal resistance input module, 12 solid state relays and two frequency converters; the crystal growth device comprises a culture tank with a jacket, a crystal carrier of the culture tank, a overheat filter box, a solution preparation tank with a jacket, a tray for placing crystal raw materials, a high saturation balance box and a growth solution circulation device;
The control method for continuous and rapid growth of the crystal with high saturation comprises the following steps:
(1) After the growth solution is filled in the culture tank and the crystal nucleus is put on the crystal carrier, the system enters an operation preparation state, and the initial set value is set on the touch screen: the temperature T 1 (0) of the growth solution in the culture tank is expressed as two decimal places; an upper growth solution temperature limit T 1max in the culture tank and a lower growth solution temperature limit T 1min in the culture tank; The specific growth rate E (0) of the crystals in the culture tank is expressed as two decimal units, the upper limit E max of the specific growth rate of the crystals in the culture tank and the lower limit E min of the specific growth rate of the crystals in the culture tank; the specific volume growth rate F (0) of the crystals in the culture tank is expressed as two decimal units, the upper limit F max of the specific volume growth rate of the crystals in the culture tank and the lower limit F min of the specific volume growth rate of the crystals in the culture tank; The total height H 1 (0) of the crystals in the culture tank, the height H 2 (0) and the width D (0) of the lower half cube of the crystals in the culture tank, the unit is mm, one decimal; the maximum growth width D max of the crystals in the culture tank is in mm and one decimal unit; The volume V (0) of the grown crystal in the culture tank is expressed as mm 3 and two decimal units; the temperature T 4 (0) of the growth solution in the solution preparation tank is expressed as two decimal places; an upper growth solution temperature limit T 4max in the solution preparation tank and a lower growth solution temperature limit T 4min in the solution preparation tank; The temperature of hot water in the overheating filter box is T 2(0)＝T1 (0) +8.00, and the unit is two decimal places; the hot water temperature of the high-saturation balance box is T 3(0)＝T1 (0) +0.10, and the unit is two-bit decimal; the rotation speed R (0) of the growth solution conveying pump is in units of revolutions per minute and one decimal; the upper rotating speed limit R max of the growth solution conveying pump and the lower rotating speed limit R min of the growth solution conveying pump;
k=0, k is a natural number representing a discrete time, k e [0,2400];
(2) The system enters an automatic running state, and a timer T starts to count;
(3) The PLC host module controls the crystal carriage alternating current motor to drive the crystal carriage to rotate clockwise for 20 circles at the speed of 30 revolutions per minute through the frequency converter 1, then stops for 20 seconds, rotates anticlockwise for 20 circles at the speed of 30 revolutions per minute, and stops for 20 seconds; the method rotates clockwise, stops, rotates anticlockwise, stops, and circulates to enable the growth solution in the culture tank to fully contact with the crystal nucleus;
The size of the grown crystal is detected on line by a crystal size vision measuring device when rotation is stopped: total height H 1 (k), height H 2 (k) and width D (k) of the lower half cube of the crystal in mm, one decimal;
The PLC host module detects the temperature of the growth solution in the culture tank, the electric heater in the jacket of the culture tank is controlled to firstly heat water in the jacket, and then the heat exchange is carried out on the wall of the tank to control the temperature of the growth solution in the culture tank to be T 1 (k), so that the control precision is +/-0.01 ℃; controlling the temperature of the growth solution in the solution preparation tank to be T 4 (k), the temperature of hot water in the overheating filtering box to be T 2 (k), the temperature of hot water in the high-saturation balancing box to be T 3 (k), and the rotating speed of the growth solution conveying pump to be R (k);
Wherein: t 1 (k) is a set value of the temperature of the growth solution in the culture tank at the moment k, H 1 (k) is a total height detection value of the crystal at the moment k, D (k) is a width detection value of the crystal at the moment k, and H 2 (k) is a height detection value of the lower half cube of the crystal at the moment k; t 4 (k) is a set value of the temperature of the growth solution in the solution preparation tank at the moment k, T 2 (k) is a set value of the hot water temperature of the overheating filter tank at the moment k, T 3 (k) is a set value of the hot water temperature of the high-saturation balance tank at the moment k, and R (k) is a set value of the rotation speed of the growth solution conveying pump at the moment k;
Calculation of the volume of the grown Crystal at time k
(4) Judging whether the timer T is equal to 1 hour or not, and if not, turning to the step (3); if true, go to step (5);
(5) Judging whether the timer k is more than or equal to 24 or not, and if not, turning to the step (16); if true, calculating the specific growth rate of the crystal at the moment k Specific volume growth rate of crystalTurning to step (6);
(6) Judging whether the timer k is smaller than 2400 or D (k) < D max is satisfied, and if not, going to the step (17); if true, go to step (7);
(7) Judging whether E (k) is not less than E max and T 1(k)＜T1max is true, if true When T 1(k)＞T1max is T 1(k)＝T1max, turning to the step (8); if not, the process goes to the step (8);
(8) Judging whether E (k) is not less than E max and T 1(k)＝T1max is true, if true When T 4(k)＜T4min is T 4(k)＝T4min, turning to the step (9); if not, go to step (9);
(9) Judging whether E (k) is less than or equal to E min and T 1(k)＞T1min is true or not, if so When T 1(k)＜T1min is T 1(k)＝T1min, turning to the step (10); if not, the process goes to the step (10);
(10) Judging whether E (k) is less than or equal to E min and T 1(k)＝T1min is true or not, if so When T 4(k)＞T4max is T 4(k)＝T4max, turning to the step (11); if not, go to step (11);
(11) Judging whether E (k) is not less than E max, T 1(k)＝T1max and T 4(k)＝T4min are true or not, if so When R (k+1) < R min then R (k+1) =r min, go to step (13); if not, go to step (13);
(13) Judging whether E (k) is less than or equal to E min, T 1(k)＝T1min and T 4(k)＝T4max are met or not, if so When R (k+1) > R max then R (k+1) =r max, go to step (14); if not, go to step (14);
(14) Judging whether F (k) is equal to or greater than F max, if so When R (k+1) < R min then R (k+1) =r min, go to step (15); if not, go to step (15);
(15) Judging whether F (k) is less than or equal to F min and if so When R (k+1) > R max then R (k+1) =r max, go to step (16); if not, go to step (16);
(16) The timer T is cleared, T 2(k+1)＝T1(k+1)+8.00,T3(k+1)＝T1 (k+1) +0.10, k=k+1, and the timer T starts to count; turning to step (3);
(17) And ending the crystal growth.
The beneficial technical effects of the invention are as follows: and when the rotation of the crystal carrying frame is stopped, the size of the grown crystal is detected on line through a crystal size vision measuring device, and a set value of the temperature of the grown solution in the culture tank, a set value of the temperature of the grown solution in the solution preparation tank and a set value of the rotating speed of the grown solution conveying pump are regulated according to rules. The solvent and the solute in the solution preparation tank coexist, and the solute content dissolved in the solution can be close to the equilibrium solute concentration at the dissolution temperature by controlling the temperature for dissolution. The temperature of the solution preparation tank is higher than the growth temperature of the culture tank, so that the concentration of the solute dissolved in the solution is higher than the equilibrium solute concentration at the growth temperature, the solution entering the culture tank is ensured to be in a supersaturated state, and the growth speed of large-size crystals is improved.
Drawings
Fig. 1 is a flow chart of a control method for continuous rapid growth of a crystal with high saturation.
Fig. 2 is a middle cross-sectional view of a grown crystal.
H1 in fig. 2 is the total height of the crystal; the lower half part of the crystal is a cube, the height is H2, the bottom surface is a regular quadrangle, and the side length is D; the upper half of the crystal is a tetrahedral cone.
FIG. 3 is a schematic diagram of a culture tank with visual measurement.
Fig. 4 is a schematic diagram of a control system for continuous rapid growth of crystals with high saturation.
Fig. 5 is a schematic diagram of a crystal high saturation continuous rapid growth apparatus.
In fig. 5: 1 a jacketed culture tank; 2 an electric heater of the culture tank; 3a culture tank water circulation pump; 4 growing crystals in the culture tank; 5, a crystal carrying frame of the culture tank; 6, carrying a crystal frame alternating current motor; 7a cooling water inlet 7 of the culture tank jacket; 8a water outlet of a jacket of the culture tank; 9 a culture tank electromagnetic valve; 10 total cooling water inlet; 11, an overheat filter box; 12 overheating the electric heater of the filter box; 13 superheating a filter box coil; 14 a conveying pipeline for connecting the outlet of the growth solution conveying pump to the inlet of the serpentine pipe of the overheat filter box; 15 a growth solution delivery pump; a 16 overheat filter box growth solution filter; 17 a superheated filtration tank water circulation pump; 18 superheating the water outlet of the filter box; a cooling water inlet 19 of the overheat filter box; 20 overheat filter box electromagnetic valve; 21 a high saturation balance box; 22 high saturation balance box electric heater; 23 high saturation balancing box coil; 24a transport line for transporting the growth solution, which is connected to the outlet of the growth solution filter in the high saturation balance tank and returns to the culture tank; 25 high saturation balance box growth solution filter; 26 high saturation balance box solenoid valve; 27 high saturation balance tank water circulation pump; a water outlet of the 28 high saturation balance box; 29 cooling water inlet of high saturation balance box; 30 solution preparing tank electromagnetic valve; 31 electric heater of solution preparing tank; 32 jacketed solution preparation tanks; 33 a solution preparation tank water circulation pump; 34 a water outlet of a jacket of the solution preparation tank; a cooling water inlet of a jacket of the 35 solution preparation tank; 36 a transfer line connecting the growth solution in the culture tank to the inlet of the growth solution transfer pump; 37 a delivery line connecting the overheated filter box growth solution filter outlet to the solution formulation tank; 38 a transfer line connecting the growth solution in the solution formulation tank to the inlet of the serpentine tube of the high saturation balancing tank; 39 a tray for holding a crystal raw material; t1 culture tank thermal resistance; t2 overheat filter box thermal resistor; t3 high saturation balancing tank thermal resistor; preparing a tank thermal resistor by using the solution T4; l1 overheat filtering box three-point type liquid level sensor; l2 high saturation balance box three-point type liquid level sensor.
Detailed Description
The following describes the embodiments of the present invention with reference to the drawings.
An application of a control method for continuous and rapid growth of crystal with high saturation comprises the following implementation processes:
The detection device comprises a culture tank thermal resistor T1, an overheat filter box thermal resistor T2, an overheat filter box three-point type liquid level sensor L1, a solution preparation tank thermal resistor T4, a high saturation balance box thermal resistor T3 and a high saturation balance box three-point type liquid level sensor L2;
the execution device comprises a crystal carriage alternating current motor 6, a culture tank electric heater 2, a culture tank water circulation pump 3, a culture tank electromagnetic valve 9, an overheat filter tank electric heater 12, an overheat filter tank water circulation pump 17, an overheat filter tank electromagnetic valve 20, a solution preparation tank electric heater 31, a solution preparation tank water circulation pump 33, a solution preparation tank electromagnetic valve 30, a high saturation balance tank electric heater 22, a high saturation balance tank water circulation pump 27, a high saturation balance tank electromagnetic valve 26 and a growth solution conveying pump 15;
The control device comprises a PLC host module, a touch screen, a thermal resistance input module, 12 solid state relays and two frequency converters;
The crystal growing device comprises a culture tank 1 with a jacket, a crystal carrying frame 5 of the culture tank, a overheat filter box 11, a solution preparation tank 32 with a jacket, a tray 39 for placing crystal raw materials, a high saturation balance box 21 and a growing solution circulating device;
The culture tank thermal resistor T1 is arranged at the upper part of the culture tank 1 with the jacket and used for measuring the temperature of a growing solution in the culture tank 1 with the jacket, the overheat filter tank thermal resistor T2 is arranged at the top of the overheat filter tank 11 and used for measuring the water temperature in the overheat filter tank 11, the overheat filter tank three-point type liquid level sensor L1 is arranged at the top of the overheat filter tank 11 and used for measuring the water level in the overheat filter tank 11, the solution preparation tank thermal resistor T4 is arranged at the upper part of the solution preparation tank 32 with the jacket and used for measuring the temperature of the growing solution in the solution preparation tank 32 with the jacket, the high saturation balance tank thermal resistor T3 is arranged at the top of the high saturation balance tank 21 and used for measuring the water temperature in the high saturation balance tank 21, and the high saturation balance tank three-point type liquid level sensor L2 is arranged at the top of the high saturation balance tank 21 and used for measuring the water level in the high saturation balance tank 21;
The crystal carrying frame alternating current motor 6 is arranged at the top of the culture tank to drive the crystal carrying frame 5 of the culture tank to rotate positively and negatively, the electric heater 2 of the culture tank is arranged in a jacket of the culture tank and is used for heating water in the jacket of the culture tank, the water circulating pump 3 of the culture tank is arranged at the outer side of the jacket of the culture tank and is used for circulating the jacket water of the culture tank, the water circulating pump is arranged at the bottom of the culture tank 1 with the jacket, and the electromagnetic valve 9 of the culture tank is arranged on a cooling water inlet pipeline of the culture tank and is used for controlling cooling water entering the jacket; the water inlet of the culture tank water circulation pump 3 is connected with the bottom of the culture tank jacket, and the water outlet of the culture tank water circulation pump 3 is connected with the upper part of the culture tank jacket; the water inlet of the culture tank electromagnetic valve 9 is connected with the total cooling water inlet 10, and the water outlet of the culture tank electromagnetic valve 9 is connected with the cooling water inlet 7 of the culture tank jacket at the bottom of the culture tank;
The overheat filter box electric heater 12 is installed in the overheat filter box 11 for heating water in the overheat filter box 11, the overheat filter box water circulation pump 17 is installed at the outer side of the overheat filter box 11 for circulating water in the overheat filter box 11, and the overheat filter box electromagnetic valve 20 is installed on a cooling water inlet pipe for controlling cooling water entering the overheat filter box 11; the water inlet of the overheat filter box water circulation pump 17 is connected with the bottom of the overheat filter box 11, and the water outlet of the overheat filter box water circulation pump 17 is connected with the upper part of the overheat filter box 11; the water inlet of the overheat filter box electromagnetic valve 20 is connected with the total cooling water inlet 10, and the water outlet of the overheat filter box electromagnetic valve 20 is connected with the cooling water inlet 19 of the overheat filter box on the side surface of the lower part of the overheat filter box 11;
The solution preparation tank electric heater 31 is arranged in the solution preparation tank jacket and used for heating water in the solution preparation tank jacket, the solution preparation tank water circulating pump 33 is arranged outside the solution preparation tank jacket and used for circulating water in the solution preparation tank jacket, and the solution preparation tank electromagnetic valve 30 is arranged on a cooling water inlet pipeline and used for controlling cooling water entering the solution preparation tank jacket; the water inlet of the solution preparation tank water circulating pump 33 is connected with the bottom of the solution preparation tank jacket, and the water outlet of the solution preparation tank water circulating pump 33 is connected with the lower part of the solution preparation tank jacket; the water inlet of the solution preparing tank electromagnetic valve 30 is connected with the total cooling water inlet 10, and the water outlet of the solution preparing tank electromagnetic valve 30 is connected with the cooling water inlet 35 of the solution preparing tank jacket at the side surface of the lower part of the solution preparing tank jacket;
The high saturation balance tank electric heater 22 is installed in the high saturation balance tank 21 for heating water in the high saturation balance tank 21, the high saturation balance tank water circulation pump 27 is installed outside the high saturation balance tank 21 for circulating water in the high saturation balance tank 21, and the high saturation balance tank electromagnetic valve 26 is installed on a cooling water inlet pipe for controlling cooling water entering the high saturation balance tank 21; the water inlet of the high-saturation balance tank water circulating pump 27 is connected with the bottom of the high-saturation balance tank 21, and the water outlet of the high-saturation balance tank water circulating pump 27 is connected with the upper part of the high-saturation balance tank 21; the water inlet of the high-saturation balance box electromagnetic valve is connected with the total cooling water inlet 10, and the water outlet of the high-saturation balance box electromagnetic valve 26 is connected with the cooling water inlet 29 of the high-saturation balance box on the side surface of the lower part of the high-saturation balance box;
The growth solution circulation device comprises a conveying pipeline, a superheated filtration tank serpentine pipe 13 installed in the superheated filtration tank 11 for heat exchange, a superheated filtration tank growth solution filter 16 installed in the superheated filtration tank 11 for filtering impurities, a high saturation balance tank serpentine pipe 23 installed in the high saturation balance tank 21 for heat exchange, and a high saturation balance tank growth solution filter 25 installed in the high saturation balance tank 21 for filtering impurities; a conveying pipeline 36 for connecting the growth solution in the culture tank to the inlet of a growth solution conveying pump stretches into the jacketed culture tank 1 from the bottom of the jacketed culture tank 1, a conveying pipeline 14 for connecting the outlet of the growth solution conveying pump to the inlet of a overheated filter box coiled pipe is connected with the inlet of the overheated filter box coiled pipe 13, the outlet of the overheated filter box coiled pipe 13 is connected with the inlet of a overheated filter box growth solution filter 16, a conveying pipeline 37 for connecting the outlet of the overheated filter box growth solution filter to the solution preparation tank stretches into the jacketed solution preparation tank 32 from the lower part of the side surface of the jacketed solution preparation tank 32, a conveying pipeline 38 for connecting the growth solution in the solution preparation tank to the inlet of a high saturation balance box coiled pipe stretches into the high saturation balance box 21 from the upper part of the side surface of the jacketed solution preparation tank 32, the outlet of the high saturation balance box coiled pipe 23 is connected with the inlet of the high saturation balance box growth solution filter 25, and a conveying pipeline 24 for connecting the growth solution outlet of the high saturation balance box returns to the culture tank stretches into the jacketed culture tank 1 from the top of the jacketed culture tank 1;
The PLC host module adjusts the frequency of the frequency converter according to the crystal growth speed so as to change the rotating speed of the growth solution conveying pump, and the growth solution conveying pump pumps the growth solution to circulate among the culture tank, the overheat filter tank, the solution preparation tank and the high saturation balance tank at an adjustable flow rate.
The PLC host module is a DVP32ES200T type host of the station, the DVP32ES200T type host is provided with a 16-way switching value input interface and a 16-way switching value output interface, the thermal resistance input module is a DVP04PT-E2 type thermal resistance input module of the station, the two frequency converters are VFD-E type frequency converters of the station, and the touch screen is a DOP-W127B type touch screen of the station;
The PLC host module is connected with an RS232 interface of the touch screen through an RS232 interface, the PLC host module is connected with RS485 interfaces of the frequency converter 1 and the frequency converter 2 through an RS485 interface, the output of the frequency converter 1 is connected with the crystal carrier alternating current motor 6, and the output of the frequency converter 2 is connected with the growth solution conveying pump 15; the switching value input interface is connected with the overheat filtering box three-point type liquid level sensor L1 and the high saturation balance box three-point type liquid level sensor L2, and the thermal resistance input module is connected with the culture tank thermal resistance T1, the overheat filtering box thermal resistance T2, the solution preparation tank thermal resistance T4 and the high saturation balance box thermal resistance T3; the first 12 outputs of the 16 paths of switching value output interfaces are respectively connected with the control ends of 12 solid state relays, and the outputs of the 12 solid state relays are respectively connected with the electric heater 2 of the culture tank, the water circulation pump 3 of the culture tank, the electromagnetic valve 9 of the culture tank, the electric heater 12 of the overheat filter tank, the water circulation pump 17 of the overheat filter tank, the electromagnetic valve 20 of the overheat filter tank, the electric heater 31 of the solution preparation tank, the water circulation pump 33 of the solution preparation tank, the electromagnetic valve 30 of the solution preparation tank, the electric heater 22 of the high saturation balance tank, the water circulation pump 27 of the high saturation balance tank and the electromagnetic valve 26 of the high saturation balance tank.
The culture tank is filled with growth solution, a crystal nucleus to be cultured and grown is placed on the crystal carrier, and the PLC host module controls the crystal carrier alternating current motor to drive the crystal carrier to slowly rotate clockwise and anticlockwise at fixed time intervals, so that the growth solution is fully contacted with the crystal nucleus. The PLC host module collects the temperature of the growth solution in the culture tank through thermal resistance of the culture tank, firstly heats water in the jacket through controlling an electric heater in the jacket of the culture tank, and then enables the temperature control precision of the growth solution in the culture tank to reach +/-0.01 ℃ through tank wall heat exchange, and keeps the temperature T 1 of the growth solution in the culture tank constant. The PLC host module controls the water circulating pump of the culture tank to make the temperature of each part in the jacket of the culture tank uniform. When the temperature needs to be reduced, the PLC host module controls the switch of the electromagnetic valve of the culture tank on the cooling water inlet pipeline to adjust the amount of cooling water entering the jacket.
The solution preparation tank is filled with growth solution, water in the jacket of the solution preparation tank is heated by controlling an electric heater in the jacket of the solution preparation tank, and then the temperature T 4 of the growth solution in the solution preparation tank is kept constant through heat exchange of the tank wall. The water circulation pump of the solution preparation tank is controlled to make the temperature of each part in the jacket of the solution preparation tank uniform. When the temperature needs to be reduced, the electromagnetic valve of the solution preparation tank on the cooling water inlet pipeline is controlled to switch so as to adjust the amount of the jacket cooling water of the solution preparation tank.
The solvent and the solute in the solution preparation tank coexist, and the solute content dissolved in the solution can be close to the equilibrium solute concentration at the dissolution temperature by controlling the temperature T 4 of the solution preparation tank to dissolve. Because the temperature T 4 of the solution preparation tank is higher than the growth temperature T 1 of the culture tank, the concentration of the solute dissolved in the solution is higher than the equilibrium concentration of the solute at the growth temperature of the culture tank, and the solution entering the culture tank is ensured to be in a supersaturated state.
The outer sides of the overheat filtering box and the high saturation balancing box are respectively provided with a water circulating pump, and the starting and stopping of the water circulating pumps are controlled by the PLC host module, so that the temperatures of all the parts in the overheat filtering box and the high saturation balancing box are uniform. The temperature of the growth solution in the coiled pipe pipeline is heated from T 1 to T 2(T2＝T1 +8 ℃ by the hot water bath of the overheat filter box with the temperature of T 2 under the heat exchange effect of the coiled pipe, and the growth solution in the coiled pipe pipeline is balanced to the temperature T 1 of the culture tank by the water bath of the high-saturation balancing box with the temperature of T 3(T3＝T1 +0.1 ℃. The PLC host module controls the electric heater and the electromagnetic valve to adjust the temperature of the hot water bath of the overheat filter box and the water bath of the high-saturation balance box. The PLC host module controls the electromagnetic valve to adjust the water level of the overheat filter box and the high saturation balance box according to the signals of the three-point type liquid level sensors in the overheat filter box and the high saturation balance box, so that no water shortage in the box is ensured.
The specific process is as follows:
(1) Filling a growth solution of potassium dihydrogen phosphate into a culture tank, placing crystal nucleus on a crystal carrier, enabling the system to enter an operation preparation state, and setting an initial set value on a touch screen ：T1(0)＝55.00℃,T1max＝57℃,T2min＝53℃;T4(0)＝5.00℃,T4max＝7℃,T4min＝3℃;E(0)＝0.30％,Emax＝0.60％,Emin＝0.20％;F(0)＝0.20％,Fmax＝0.40％,Fmin＝0.10％;H1(0)＝50.0mm,H2(0)＝25.0mm,D(0)＝50.0mm;R(0)＝500,Rmax＝800,Rmin＝300;k＝0,T＝0.
(2) The system enters an automatic running state, and a timer T starts to count.
(3) The PLC host module controls the crystal carriage alternating current motor to drive the crystal carriage to rotate clockwise for 20 circles at the speed of 30 revolutions per minute through the frequency converter 1, then stops for 20 seconds, rotates anticlockwise for 20 circles at the speed of 30 revolutions per minute, and stops for 20 seconds; the method rotates clockwise, stops, rotates anticlockwise, stops, and circulates to enable the growth solution in the culture tank to fully contact with the crystal nucleus;
The size of the grown crystal is detected on line by a crystal size vision measuring device when rotation is stopped: total height H 1 (k), height H 2 (k) and width D (k) of the lower half cube of the crystal in mm, one decimal;
The PLC host module detects the temperature of the growth solution in the culture tank, the electric heater in the jacket of the culture tank is controlled to firstly heat water in the jacket, and then the heat exchange is carried out on the wall of the tank to control the temperature of the growth solution in the culture tank to be T 1 (k), so that the control precision is +/-0.01 ℃; controlling the temperature of the growth solution in the solution preparation tank to be T 4 (k), the temperature of hot water in the overheating filtering box to be T 2 (k), the temperature of hot water in the high-saturation balancing box to be T 3 (k), and the rotating speed of the growth solution conveying pump to be R (k);
The temperature of the growth solution in the culture tank is T 1 (k), the growth solution in the culture tank is pumped by a growth solution delivery pump, and flows through a coiled pipe in a overheat filter box with the temperature of T 2 (k), the mixed crystal particles are dissolved along with the rise of the temperature of the growth solution, and the temperature of the growth solution reaches T 2 (k); the growth solution flows through the filter to remove extraneous impurities, and the quality of the growth solution is purified.
The growth solution flows through a solution preparation tank with the temperature of T 4 (k), the solvent and the solute coexist in the solution preparation tank, and the solute content dissolved in the solution can be close to the equilibrium solute concentration at the dissolution temperature of T 4 (k) by controlling the temperature of the solution preparation tank to dissolve.
The prepared growth solution flows into a coiled pipe in a high-saturation balance box with the temperature of T 3 (k), the temperature of the growth solution is reduced to be nearly consistent with the temperature of T 1 (k) in a culture tank, irrelevant impurities are filtered by a filter, and finally the growth solution returns to the culture tank to complete the circulation.
(4) According to the crystal size detected by the crystal size vision measuring device on line, regulating a growth solution temperature set value T 1 (k) in a culture tank according to a rule, wherein the growth solution temperature set value T 4 (k) in a solution preparation tank, a overheat filter box hot water temperature set value T 2 (k), a high saturation balance box hot water temperature set value T 3 (k) and R (k) are rotation speed set values of a growth solution conveying pump at the moment k; .
(5) And ending the crystal growth when k is larger than or equal to 2400 or D (k) is larger than or equal to D max.
The invention can increase the growth speed of large-size crystals.
The foregoing is a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation and variation of the above embodiment according to the technical substance of the present invention falls within the scope of the technical solution of the present invention.

Claims (1)

1.一种晶体高饱和度连续快速生长的控制方法，其特征在于，1. A method for controlling the continuous and rapid growth of crystals with high saturation, characterized in that: 该方法是通过晶体高饱和度连续快速生长系统实现的，所述的晶体高饱和度连续快速生长系统包括检测装置、执行装置、控制装置和晶体生长装置；检测装置包括培养罐热电阻、过热过滤箱热电阻、过热过滤箱三点式液位传感器、溶液配制罐热电阻、高饱和度平衡箱热电阻、高饱和度平衡箱三点式液位传感器；执行装置包括载晶架交流电机、培养罐电加热器、培养罐水循环泵、培养罐电磁阀、过热过滤箱电加热器、过热过滤箱水循环泵、过热过滤箱电磁阀、溶液配制罐电加热器、溶液配制罐水循环泵、溶液配制罐电磁阀、高饱和度平衡箱电加热器、高饱和度平衡箱水循环泵、高饱和度平衡箱电磁阀和生长溶液输送泵；控制装置包括PLC主机模块、触摸屏、热电阻输入模块、12个固态继电器和二台变频器；晶体生长装置包括带夹套的培养罐、培养罐载晶架、过热过滤箱、带夹套的溶液配制罐、放置晶体原料的托盘、高饱和度平衡箱和生长溶液循环装置；The method is realized by a crystal high saturation continuous rapid growth system, which comprises a detection device, an execution device, a control device and a crystal growth device; the detection device comprises a culture tank thermal resistor, an overheat filter box thermal resistor, an overheat filter box three-point liquid level sensor, a solution preparation tank thermal resistor, a high saturation balance box thermal resistor, and a high saturation balance box three-point liquid level sensor; the execution device comprises a crystal carrier AC motor, a culture tank electric heater, a culture tank water circulation pump, a culture tank solenoid valve, an overheat filter box electric heater, an overheat filter box water circulation pump, a culture tank solenoid valve, a superheat filter box electric heater, a superheat filter box water circulation pump, a crystal growth device, and a crystal growth device; the detection device comprises a culture tank thermal resistor, an overheat filter box thermal resistor, a superheat filter box three-point liquid level sensor, a solution preparation tank thermal resistor, a high saturation balance box thermal resistor, and a high saturation balance box three-point liquid level sensor; the execution device comprises a crystal carrier AC motor, a culture tank electric heater, a culture tank water circulation pump, a culture tank solenoid valve, a superheat filter box electric heater, a superheat filter box water circulation pump ... Ring pump, solenoid valve of superheat filter box, electric heater of solution preparation tank, water circulation pump of solution preparation tank, solenoid valve of solution preparation tank, electric heater of high saturation balance tank, water circulation pump of high saturation balance tank, solenoid valve of high saturation balance tank and growth solution delivery pump; control device includes PLC host module, touch screen, thermal resistor input module, 12 solid-state relays and two inverters; crystal growth device includes culture tank with jacket, crystal rack of culture tank, superheat filter box, solution preparation tank with jacket, tray for placing crystal raw materials, high saturation balance tank and growth solution circulation device; 所述的一种晶体高饱和度连续快速生长的控制方法，具体包括以下步骤：The method for controlling the high saturation continuous rapid growth of a crystal specifically comprises the following steps: (1)培养罐中装入生长溶液，晶核放到载晶架上后，系统进入运行准备状态，在触摸屏上进行初始设定值的设定：培养罐内生长溶液温度T1(0)，单位为℃，二位小数；培养罐内生长溶液温度上限T1max，培养罐内生长溶液温度下限T1min；培养罐内晶体比生长速率E(0)，单位为％，二位小数，培养罐内晶体比生长速率上限Emax，培养罐内晶体比生长速率下限Emin；培养罐内晶体比体积生长速率F(0)，单位为％，二位小数，培养罐内晶体比体积生长速率上限Fmax，培养罐内晶体比体积生长速率下限Fmin；培养罐内晶体总高度H1(0)、培养罐内晶体的下半部立方体的高度H2(0)和宽度D(0)，单位为mm，一位小数；培养罐内晶体的最大生长宽度Dmax，单位为mm，一位小数；培养罐内生长晶体的体积V(0)，单位为mm3，二位小数；溶液配制罐内生长溶液温度T4(0)，单位为℃，二位小数；溶液配制罐内生长溶液温度上限T4max，溶液配制罐内生长溶液温度下限T4min；过热过滤箱热水温度为T2(0)＝T1(0)+8.00，单位为℃，二位小数；高饱和度平衡箱热水温度为T3(0)＝T1(0)+0.10，单位为℃，二位小数；生长溶液输送泵的转速R(0)，单位为转/分钟，一位小数；生长溶液输送泵的转速上限Rmax，生长溶液输送泵的转速下限Rmin；(1) After the growth solution is placed in the culture tank and the crystal nucleus is placed on the crystal carrier, the system enters the operation preparation state and the initial setting values are set on the touch screen: the temperature of the growth solution in the culture tank T1 (0), in °C, two decimal places; the upper limit of the temperature of the growth solution in the culture tank T1max , the lower limit of the temperature of the growth solution in the culture tank T1min ; the specific growth rate of the crystal in the culture tank E(0), in %, two decimal places, the upper limit of the specific growth rate of the crystal in the culture tank Emax , the lower limit of the specific growth rate of the crystal in the culture tank Emin ; the specific volume growth rate of the crystal in the culture tank F(0), in %, two decimal places, the upper limit of the specific volume growth rate of the crystal in the culture tank Fmax , the lower limit of the specific volume growth rate of the crystal in the culture tank Fmin ; the total height H1 (0) of the crystal in the culture tank, the height H2 (0) and the width D(0) of the lower half cube of the crystal in the culture tank, in mm, one decimal place; the maximum growth width Dmax of the crystal in the culture tank , in mm, one decimal place; volume of growing crystals in the culture tank V(0), in mm 3 , two decimal places; temperature of growing solution in solution preparation tank T 4 (0), in °C, two decimal places; upper limit of temperature of growing solution in solution preparation tank T 4max , lower limit of temperature of growing solution in solution preparation tank T 4min ; temperature of hot water in superheated filter tank T 2 (0)＝T 1 (0)+8.00, in °C, two decimal places; temperature of hot water in high saturation balance tank T 3 (0)＝T 1 (0)+0.10, in °C, two decimal places; speed of growth solution delivery pump R(0), in rpm, one decimal place; upper limit of speed of growth solution delivery pump R max , lower limit of speed of growth solution delivery pump R min ; k是自然数，代表离散时刻，k∈[0,2400]；k is a natural number representing a discrete moment, k∈[0,2400]; (2)系统进入自动运行状态，计时器T开始计时；(2) The system enters the automatic operation state and the timer T starts timing; (3)PLC主机模块通过变频器1控制载晶架交流电机带动载晶架以每分钟30转的速度顺时针旋转20圈，然后停止20秒，再以每分钟30转的速度逆时针旋转20圈，停止20秒；以此方法顺时针旋转、停止、逆时针旋转、停止，循环运行，使培养罐中的生长溶液与晶核充分接触；(3) The PLC host module controls the crystal carrier AC motor through the frequency converter 1 to drive the crystal carrier to rotate clockwise for 20 times at a speed of 30 revolutions per minute, then stop for 20 seconds, and then rotate counterclockwise for 20 times at a speed of 30 revolutions per minute, and stop for 20 seconds; in this way, the crystal carrier rotates clockwise, stops, rotates counterclockwise, and stops in a cycle, so that the growth solution in the culture tank is in full contact with the crystal nucleus; 旋转停止时通过晶体尺寸视觉测量装置在线检测生长晶体的尺寸：总高度H1(k)、晶体的下半部立方体的高度H2(k)和宽度D(k)，单位为mm，一位小数；When the rotation stops, the dimensions of the growing crystal are detected online by a crystal dimension visual measuring device: the total height H 1 (k), the height H 2 (k) and the width D (k) of the lower half cube of the crystal, in mm, with one decimal place; PLC主机模块检测培养罐内生长溶液的温度，通过控制培养罐夹套内的电加热器先加热夹套中的水，再通过罐壁热交换使培养罐内生长溶液的温度控制为T1(k)，控制精度为±0.01℃；控制溶液配制罐内生长溶液温度为T4(k)，过热过滤箱热水温度为T2(k)，高饱和度平衡箱热水温度为T3(k)，生长溶液输送泵的转速为R(k)；The PLC host module detects the temperature of the growth solution in the culture tank, controls the electric heater in the jacket of the culture tank to heat the water in the jacket first, and then controls the temperature of the growth solution in the culture tank to be T 1 (k) through the heat exchange of the tank wall, with a control accuracy of ±0.01°C; controls the temperature of the growth solution in the solution preparation tank to be T 4 (k), the temperature of the hot water in the superheated filter tank to be T 2 (k), the temperature of the hot water in the high saturation balance tank to be T 3 (k), and the speed of the growth solution delivery pump to be R (k); 其中：T1(k)为k时刻的培养罐内生长溶液温度设定值，H1(k)为k时刻的晶体总高度检测值，D(k)为k时刻的晶体宽度检测值，H2(k)为k时刻的晶体下半部立方体的高度检测值；T4(k)为k时刻的溶液配制罐内生长溶液温度设定值，T2(k)为k时刻的过热过滤箱热水温度设定值，T3(k)为k时刻的高饱和度平衡箱热水温度设定值，R(k)为k时刻的生长溶液输送泵的转速设定值；Wherein: T 1 (k) is the set value of the temperature of the growth solution in the culture tank at time k, H 1 (k) is the detected value of the total height of the crystal at time k, D(k) is the detected value of the width of the crystal at time k, H 2 (k) is the detected value of the height of the lower half of the cube of the crystal at time k; T 4 (k) is the set value of the temperature of the growth solution in the solution preparation tank at time k, T 2 (k) is the set value of the hot water temperature of the superheated filter box at time k, T 3 (k) is the set value of the hot water temperature of the high saturation balance box at time k, and R(k) is the set value of the speed of the growth solution delivery pump at time k; 计算k时刻生长晶体的体积 Calculate the volume of the growing crystal at time k (4)判断计时器T等于1小时是否成立，不成立则转到步骤(3)；成立则转到步骤(5)；(4) Determine whether the timer T is equal to 1 hour. If not, go to step (3); if yes, go to step (5); (5)判断计时器k≥24是否成立，不成立则转到步骤(16)；成立则计算k时刻晶体比生长速率晶体比体积生长速率转到步骤(6)；(5) Determine whether the timer k ≥ 24 is true. If not, go to step (16); if true, calculate the specific growth rate of the crystal at time k. Crystal volume growth rate Go to step (6); (6)判断计时器k＜2400或D(k)＜Dmax是否成立，不成立则转到步骤(17)；成立则转到步骤(7)；(6) Determine whether timer k < 2400 or D(k) < D max. If not, go to step (17); if yes, go to step (7); (7)判断E(k)≥Emax且T1(k)＜T1max是否成立，成立则当T1(k)＞T1max则T1(k)＝T1max，转到步骤(8)；不成立则转到步骤(8)；(7) Determine whether E(k)≥E max and T 1 (k)＜T 1max . If yes, When T 1 (k)＞T 1max , then T 1 (k)＝T 1max , go to step (8); if not, go to step (8); (8)判断E(k)≥Emax且T1(k)＝T1max是否成立，成立则当T4(k)＜T4min则T4(k)＝T4min，转到步骤(9)；不成立则转到步骤(9)；(8) Determine whether E(k) ≥ E max and T 1 (k) = T 1max . If yes, When T 4 (k)＜T 4min , then T 4 (k)＝T 4min , go to step (9); if not, go to step (9); (9)判断E(k)≤Emin且T1(k)＞T1min是否成立，成立则当T1(k)＜T1min则T1(k)＝T1min，转到步骤(10)；不成立则转到步骤(10)；(9) Determine whether E(k) ≤Emin and T1 (k)＞ T1min. If yes, When T 1 (k)＜T 1min , then T 1 (k)＝T 1min , go to step (10); if not, go to step (10); (10)判断E(k)≤Emin且T1(k)＝T1min是否成立，成立则当T4(k)＞T4max则T4(k)＝T4max，转到步骤(11)；不成立则转到步骤(11)；(10) Determine whether E(k) ≤Emin and T1 (k)＝ T1min . If yes, When T 4 (k)＞T 4max , then T 4 (k)＝T 4max , go to step (11); if not, go to step (11); (11)判断E(k)≥Emax，且T1(k)＝T1max，且T4(k)＝T4min是否成立，成立则当R(k+1)＜Rmin则R(k+1)＝Rmin，转到步骤(12)；不成立则转到步骤(12)；(11) Determine whether E(k) ≥ E max , T 1 (k) = T 1max , and T 4 (k) = T 4min are true. If true, then When R(k+1)＜R min , then R(k+1)＝R min and go to step (12); if not, go to step (12); (12)判断E(k)≤Emin，且T1(k)＝T1min，且T4(k)＝T4max是否成立，成立则当R(k+1)＞Rmax则R(k+1)＝Rmax，转到步骤(13)；不成立则转到步骤(13)；(12) Determine whether E(k) ≤Emin , T1 (k)＝ T1min , and T4 (k)＝ T4max. If yes, When R(k+1)＞R max , then R(k+1)＝R max , go to step (13); if not, go to step (13); (13)判断F(k)≥Fmax是否成立，成立则当R(k+1)＜Rmin则R(k+1)＝Rmin，转到步骤(14)；不成立则转到步骤(14)；(13) Determine whether F(k)≥F max holds. If it holds, then When R(k+1)＜R min , then R(k+1)＝R min and go to step (14); if not, go to step (14); (14)判断F(k)≤Fmin是否成立，成立则当R(k+1)＞Rmax则R(k+1)＝Rmax，转到步骤(15)；不成立则转到步骤(15)；(14) Determine whether F(k)≤F min holds. If it holds, then When R(k+1)＞R max , then R(k+1)＝R max , go to step (15); if not, go to step (15); (15)计时器T清零，T2(k+1)＝T1(k+1)+8.00，T3(k+1)＝T1(k+1)+0.10，k＝k+1，计时器T开始计时；转到步骤(3)；(15) Timer T is reset, T 2 (k+1)=T 1 (k+1)+8.00, T 3 (k+1)=T 1 (k+1)+0.10, k=k+1, timer T starts timing; go to step (3); (16)晶体生长结束。(16) Crystal growth ends.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101824649A (en) * 2010-04-30 2010-09-08 中山大学 Growth early-stage control method of automatic photoelectric crystal furnace
CN102071459A (en) * 2009-11-23 2011-05-25 中国科学院福建物质结构研究所 Calculation method of temperature reducing program in quick growth of large-size potassium dihydrogen phosphate (KDP) monocrystals

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0903428A3 (en) * 1997-09-03 2000-07-19 Leybold Systems GmbH Apparatus and method for determining crystal diameters
CN1234920C (en) * 2003-09-01 2006-01-04 山东大学 Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category
CN105088943A (en) * 2014-05-13 2015-11-25 柳州欧维姆机械股份有限公司 Steel wire stayed cable filled or coated with polyurea protection materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102071459A (en) * 2009-11-23 2011-05-25 中国科学院福建物质结构研究所 Calculation method of temperature reducing program in quick growth of large-size potassium dihydrogen phosphate (KDP) monocrystals
CN101824649A (en) * 2010-04-30 2010-09-08 中山大学 Growth early-stage control method of automatic photoelectric crystal furnace

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