CN108642558A - Ring ladder pedestal and system for organic crystal spontaneous nucleation growth - Google Patents
Ring ladder pedestal and system for organic crystal spontaneous nucleation growth Download PDFInfo
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- CN108642558A CN108642558A CN201810702636.9A CN201810702636A CN108642558A CN 108642558 A CN108642558 A CN 108642558A CN 201810702636 A CN201810702636 A CN 201810702636A CN 108642558 A CN108642558 A CN 108642558A
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- 239000013078 crystal Substances 0.000 title claims abstract description 125
- 230000012010 growth Effects 0.000 title claims abstract description 72
- 238000010899 nucleation Methods 0.000 title claims abstract description 37
- 230000006911 nucleation Effects 0.000 title claims abstract description 37
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 230000002269 spontaneous effect Effects 0.000 title claims abstract description 31
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000008236 heating water Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000012774 insulation material Substances 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- CSJLBAMHHLJAAS-UHFFFAOYSA-N diethylaminosulfur trifluoride Substances CCN(CC)S(F)(F)F CSJLBAMHHLJAAS-UHFFFAOYSA-N 0.000 claims 1
- 235000013399 edible fruits Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 description 20
- 239000000243 solution Substances 0.000 description 14
- 230000033228 biological regulation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910007709 ZnTe Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910012463 LiTaO3 Inorganic materials 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229950004288 tosilate Drugs 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C30B29/54—Organic compounds
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of ring ladder pedestal and system for organic crystal spontaneous nucleation growth, the ring ladder pedestal has a ring ladder groove, the ring ladder groove is distributed by multistage annular L-type groove in ladder, it, which can cover to be set to, educates bottom in brilliant bottle, is dropped to naturally in cyclic annular L-type groove for the nucleus of spontaneous nucleation；The organic crystal spontaneous nucleation growth system includes water-bath circulator, temperature control equipment and crystal growing apparatus, the water-bath circulator includes water-bath circulation cylinder and circulating pump, to be recycled to aqueous solution in water-bath circulation cylinder, temperature control equipment is used to regulate and control aqueous solution in water-bath circulation cylinder into trip temperature, crystal growing apparatus includes educating brilliant bottle and being set to the ring ladder pedestal for educating bottom in brilliant bottle, this is educated brilliant bottle and is set in water-bath circulation cylinder.The present invention can effectively control nucleus nucleation site, effectively avoid crystal adhesion problems during nucleus growth, can also keep aqueous temperature stability, improve crystal yield rate.
Description
Technical field
The invention belongs to crystal growth equipment technical fields more particularly to a kind of for organic crystal spontaneous nucleation growth
Ring ladder pedestal and system.
Background technology
4- (4- dimethylaminostyryls) picoline tosilate (DAST) crystal is a kind of non-with high second order
Organic Electrooptic crystal material of linear coefficient and low-k, crystal is by negatively charged p-methyl benzenesulfonic acid anion and positively charged
The pyridylium of lotus forms, and pyridine groups make electron acceptor in molecule, and sulfonic acid group does electron donor, and C=C double bonds are by two pi bonds
Conjugation is got up, and is typical D- π-A structures.Under the effect of outer light field, DAST crystal charge can be transferred to separately from one section of molecule
Outer one end, to make DAST molecule non-linear susceptibilities become larger.Studies have shown that electron donor-acceptor (EDA) intensity gets over electric charge transfer in macromolecular
Degree is bigger, and corresponding microcosmic second order susceptibility is also bigger.DAST crystal belongs to monocline in non-centrosymmetrical macroscopical crystal accumulation
Crystallographic system, biaxial crystal, space group Cc, point group M, Z=4, lattice constant
β=92.24 °.The design feature of DAST crystal makes it show good second order nonlinear coefficient (χ(2)=2020 ±
220pm/V@1318nm) and low-k (ε1=5.2 ± 0.4), the crystal electro-optic coefficient at 820nm wavelength is γ11=
400 ± 150pm/V, 1-2 number bigger than the analog value of ZnTe crystal set grade, and frequency-doubled effect is 1000 times of urea.DAST is brilliant
Body is a kind of Organic nonlinear crystal of function admirable, while being also the organic crystal material for generating THz radiation, in 7-
In 20THz frequency ranges, 6 times that energy is ZnTe crystal are generated, LiTaO3185 times of crystal, than high quality GaAs and
InP is 42 times big, is generating terahertz emission and field of detecting based on DAST crystal difference frequencies, is having vast potential for future development.
Currently, DAST growing methods include mainly：(1) spontaneous nucleation method：Spontaneous nucleation method is slow by solution
Cooling obtains driving force needed for crystal growth to carry out crystal growth, and the high-purity DAST crystal raw materials prepared are put into and educate crystalline substance
In bottle, then controls temperature and slowly decline, crystal can be crystallized slowly in the solution, gradually grow into bulky crystal.This method knot
Structure is simple, easy to operate, can be produced in batches, but nucleus nucleation site cannot control in crystal growing process, is easy
Crystal is sticked together during causing nucleus growth, forms stray crystal, causes crystal yield rate relatively low.(2) tilting plate method：Inclined plate
Method is that the polytetrafluoroethylene (PTFE) inclined plate with V-type groove is added in educating brilliant bottle on the basis of spontaneous nucleation method, and main purpose is
Crystal growth posture is controlled, when occurring nucleus in solution, nucleus can be slipped in inclined plate groove and growth of standing, in certain journey
Can be to avoid nucleus adhesion problems on degree, but V-type groove inclined plate can not educate brilliant bottle perfect matching with circle, lead to available next life
The load crystalline substance effective area of long crystal is smaller, and V-type groove limited amount, and the disposable amount of crystals that grows is few, low production efficiency.
Since V-type groove inclined plate can not be completely covered brilliant bottom of bottle portion of educating, in real crystal growth course, not all nucleus can be slided
It falls in groove, there are part nucleus to be slipped to brilliant bottom of bottle portion of educating, and nuclei growth stick to each other forms stray crystal.(3) seed-grain method：
It is the seed rod that polytetrafluoroethylene (PTFE) is added in educating brilliant bottle and makes that seed-grain method, which prepares DAST crystal, and top adhesion quality is preferable
Seed crystal allows DAST crystalloid solutions along seed crystal face oriented growth, solves crystal adhesion problems, the larger crystal of growth size.But
It is that seed-grain method growth DAST crystal is stringenter to temperature control, more demanding to environmental stability, and crystal growing process
Middle seed crystal is easy to fall off.Three of the above method can prepare DAST crystal, but cut both ways, and cannot carry out high quality, greatly
The batch crystal growth of size.It is all side heat that the water bath heating device of three of the above method is most of simultaneously, is easy to cause
Water temperature heating is uneven, and there are temperature difference, aqueous solution is static solution in crystal growth cylinder, places be easy to cause water for a long time
Pollution, has some impact on environment of crystal growth stability.
Invention content
In view of this, the main purpose of the present invention is to provide a kind of annular steps for organic crystal spontaneous nucleation growth
Terraced pedestal and system, to solve at least one of above-mentioned the technical issues of referring at least partly.
To achieve the above object, technical scheme is as follows：
As one aspect of the present invention, a kind of ring ladder pedestal for organic crystal spontaneous nucleation growth is provided,
It can cover and be set to one and educate bottom in brilliant bottle, the ring ladder pedestal has a ring ladder groove, the ring ladder
Groove, which is distributed by n grades of cyclic annular L-type grooves in ladder, to be formed, wherein n >=2, per level-one described in cyclic annular L-type groove bottom surface with educate crystalline substance
Bottom of bottle portion is parallel to each other, side and educates brilliant bottom of bottle portion at an angle of 90.
Wherein, the bottom width of cyclic annular L-type groove described in every level-one and profile height are 5mm.
Wherein, the ring ladder pedestal is made by polytetrafluoroethylene material.
As another aspect of the invention, a kind of organic crystal spontaneous nucleation growth system, including water-bath cycle are provided
Device, temperature control equipment and crystal growing apparatus, wherein：
The water-bath circulator includes the water-bath circulation cylinder and circulating pump being connected, and is followed to water-bath by the circulating pump
Aqueous solution in ring cylinder is recycled；
The temperature control equipment includes heating rod, temperature sensor, temperature controller and temperature feedback processor,
In：
The heating rod and temperature sensor are respectively arranged in water-bath circulation cylinder；
The temperature feedback processor is connected to temperature sensor, is acquired for the data to the temperature sensor
And processing；
The temperature controller is connected to temperature feedback processor, for the handling result pair according to temperature feedback processor
The heating rod is controlled；
The crystal growing apparatus includes educating brilliant bottle and ring ladder pedestal as described above, and the ring ladder pedestal covers
Lid is set to and educates bottom in brilliant bottle, described to educate brilliant bottle and be positioned in the water-bath circulation cylinder.
Wherein, the water-bath circulation cylinder includes water-bath growth cylinder and heating water bath cylinder, wherein is set in the water-bath growth cylinder
Brilliant bottle and temperature sensor are educated described in being equipped with；The heating rod and temperature sensor are provided in the heating water bath cylinder, it is described
Water-bath, which is grown, to be connected between cylinder and heating water bath cylinder by circulating line, and the circulating pump is set on the circulating line.
Wherein, the water-bath circulation cylinder further includes crystal growing furnace, and the water-bath growth cylinder is set to the crystal growth
In stove, is grown in the water-bath and be provided with thermal insulation material between cylinder and crystal growing furnace.
Wherein, the crystal growing furnace is made of stainless steel material.
Wherein, the circulating line is made by glass material, and outside is coated with thermal insulation material.
Wherein, described to educate brilliant bottle side for cylinder, the ring ladder base side is also cylinder.
Wherein, described to educate brilliant bottle and water-bath circulation cylinder is made by glass material.
As it is still another aspect of the present invention to provide a kind of organic crystal spontaneous nucleation growth systems as described above to make
Application in standby organic nonlinear optical crystal, the especially application in preparing DAST crystal.
Based on the above-mentioned technical proposal, the beneficial effects of the present invention are：
(1) on existing organic crystal spontaneous nucleation growth device basic, one is placed with annular step educating brilliant bottom of bottle portion
The ring ladder pedestal of terraced groove, which, which is distributed by n grades of cyclic annular L-type grooves in ladder, forms, and efficiently solves
The problem of educating brilliant bottle Incomplete matching with circle of rectangular-shaped V-type groove inclined plate pedestal, and can effectively control nucleus nucleation
Position effectively avoids crystal adhesion problems during nucleus growth.
(2) compared to V-type groove inclined plate pedestal, the quantity of cyclic annular L-shaped groove can be more, can disposably carry out
Batch organic crystal is grown, and improves crystal production rate.
(3) water-bath circulator is set, aqueous temperature stability is kept, improves crystal yield rate, obtaining high quality has
Machine crystal.
(4) structure of entire organic crystal spontaneous nucleation growth system is simple, easily operated, can be widely applied to organic non-
Linear optical crystal preparation field.
Description of the drawings
Fig. 1 is organic crystal spontaneous nucleation growth system construction drawing of the present invention；
Fig. 2 is ring ladder schematic diagram of base structure of the present invention；
Fig. 3 is DAST crystal spontaneous nucleation growth process schematics of the embodiment of the present invention.
In above-mentioned attached drawing, reference numeral meaning is specific as follows：
1- crystal growing furnaces；2- thermocouples；3- water-baths grow cylinder；
4- educates brilliant bottle；5- ring ladder pedestals；6- circulating pumps；
7- outlet pipes；8- heating water bath cylinders；9- annular-heating sticks；
10- temperature controllers；11 temperature feedback processors.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
The present invention provides a kind of ring ladder pedestals and system for organic crystal spontaneous nucleation growth, can be effective
Nucleus nucleation site is controlled, crystal adhesion problems during nucleus growth is avoided, improves crystal production rate；Further pass through water
The design of circulator is bathed, aqueous temperature is kept to stablize, high quality, large-size crystals can be obtained, improves crystal yield rate.
As shown in Fig. 2, the present invention is used for the ring ladder pedestal of organic crystal spontaneous nucleation growth, it can cover and be set to
One educates bottom in brilliant bottle 4, and there is a ring ladder groove, the ring ladder groove to be distributed in ladder by n grades of cyclic annular L-type grooves
Formed, wherein n >=2, per level-one described in cyclic annular L-type groove bottom surface and to educate brilliant bottom of bottle portion parallel to each other, side with educate brilliant bottom of bottle
Portion at an angle of 90, so as to be mutually matched with brilliant bottle is educated, and contributes to the vertical growth of seed crystal.Per level-one ring-type L-type groove
Bottom width, profile height can be according to actual requirement designed, designed, such as 4~6mm can be disposed as, specifically for example
It is set as 5mm；The quantity of cyclic annular L-type groove, i.e. n values can be also adjusted according to the size for educating brilliant bottle, oblique compared to V-type groove
The quantity of board bottom seat, cyclic annular L-shaped groove can be more, can disposably carry out batch organic crystal growth, improve crystal
Productivity.
As shown in Figure 1, organic crystal spontaneous nucleation growth system of the present invention specifically includes water-bath circulator, temperature control
Device and crystal growing apparatus, it is possible to prevente effectively from nucleus adhesion problems, improve environment of crystal growth stability.Below to each
Device composition elaborates.
Water-bath circulator includes water-bath growth cylinder 3, heating water bath cylinder 8, circulating pump 6, water inlet pipe and outlet pipe 7, wherein
Water-bath, which is grown, to be connected between cylinder 3 and heating water bath cylinder 8 by water inlet pipe and outlet pipe 7, and circulating pump 6 is provided on water inlet pipe,
Water inlet pipe and outlet pipe collectively form circulating line, dynamic circulation regulation and control are carried out to aqueous solution, preferably, outside circulating line
It is coated with thermal insulation material, such as polytene heat-insulation material.
Temperature control equipment includes annular-heating stick 9, thermocouple 2, temperature controller 10 and temperature feedback processor 11,
Middle annular heating rod 9 is set in heating water bath cylinder 8, and two thermocouples 2 are used as temperature sensor, is respectively arranged at water-bath growth
In cylinder 3 and heating water bath cylinder 8, temperature feedback processor 11 is connected to two thermocouples 2, carries out acquisition and the place of temperature data
Reason, temperature controller 10 is connected to temperature feedback processor 11 and heating rod 9, according to the handling result of temperature feedback processor 11
Heating rod 9 is controlled, dynamic monitors aqueous solution real-time temperature, is cooled down by the heating of temperature feedback dynamic adjustment aqueous solution
Process, for example, if the handling result of temperature feedback processor 11 shows the temperature data of two thermocouples 2 acquisition less than setting
Value is then controlled by temperature controller 10 and improves heating rod heating efficiency, heated up to aqueous solution；Conversely, then being controlled by temperature
The control of device 10 reduces heating rod heating efficiency, cools down to aqueous solution.
Crystal growing apparatus includes crystal growing furnace 1, educates brilliant bottle 4 and ring ladder pedestal 5, wherein water-bath growth cylinder 3 is set
It is placed in crystal growing furnace 1, is grown in water-bath and be provided with thermal insulation material, such as polytene heat-insulation between cylinder 3 and crystal growing furnace 1
Material；Brilliant bottle 4 is educated to be positioned in water-bath growth cylinder 3；The covering of ring ladder pedestal 5, which is set to, educates bottom in brilliant bottle 4, ring ladder
The structure of pedestal 5 is for example aforementioned.As shown in figure 3, by slow cooling, organic crystal solution spontaneous nucleation, nucleus is fallen naturally
Ring ladder pedestal carries brilliant inclined plate effective area by increasing, effectively avoids crystal adhesion problems during nucleus growth, natural
Crystallization, oriented growth are final to obtain high quality organic crystal.
It is cylinder to educate brilliant bottle 4, therefore ring ladder pedestal is also cylinder, with the base profile phase of educating brilliant bottle 4
Match, efficiently solve the problems, such as rectangular-shaped V-type groove inclined plate pedestal educates brilliant bottle Incomplete matching with circle.
Below in conjunction with attached drawing to be preferably real using organic crystal spontaneous nucleation growth system growth high quality DAST crystal
Example is applied, technical scheme of the present invention is further described.
Embodiment 1
The present invention will live through filtering, natural recrystallization and slowly tie again before realizing high quality DAST crystal growths
The high-purity DAST crystal raw materials of brilliant three step methods of purification, with methanol solution according to 3.8：100 proportional arrangement high-purity DAST lifes
Long solution 300ml, DAST growth solutions are put into made of glass material and are educated in brilliant bottle 4, top ground glass lid and true
Empty fat is educated brilliant bottom of bottle portion and places the ring ladder pedestal 5 made as material using polytetrafluoroethylene (PTFE) into sealing.High-purity will be filled
The brilliant bottle 4 of educating of DAST Crystal Growth Solutions is put into so that in water-bath growth cylinder 3 made of glass material, brilliant bottle is educated in inside placement
Water-bath growth cylinder 3 is put into the crystal growing furnace 1 made of stainless steel material, and on the inside of the furnace wall of crystal growing furnace 1 and bottom is embedding
There is polytene heat-insulation material, to reach heat insulation effect, improves the stability of environment of crystal growth.3 top of water-bath growth cylinder passes through
Water inlet pipe is attached with the heating water bath cylinder 8 made of glass material, and circulating pump 6, water-bath are grown again for setting on water inlet pipe
3 bottom of cylinder is attached by outlet pipe 7 and heating water bath cylinder 8, and outlet pipe and water inlet pipe are coated with polytene heat-insulation material,
Make aqueous solution grow in water-bath by control loop pump 6 to recycle between cylinder 3 and heating water bath cylinder 8.Water-bath grows cylinder 3 and water-bath adds
Hot cylinder 8 is vertical simultaneously to place thermocouple 2, to aqueous solution into the immediately monitoring of trip temperature, while being connect with temperature feedback device 11, into
The dynamic acquisition of trip temperature and regulation and control, temperature feedback device 11 are connect with temperature controller 10, and temperature controller 10 is put by control
Set the annular-heating stick 9 in water-bath grows cylinder 8, the dynamic regulation for being heated up and being cooled down to water bath device.
In the present embodiment, crystal growing furnace internal diameter 40cm, high 60cm；Water-bath grows cylinder bore 36cm, high 50cm；Educate brilliant bottle
Internal diameter 12cm, high 30cm；The width and height of the cyclic annular L-type grooves at different levels of ring ladder pedestal are 5mm；In heating water bath cylinder
Diameter 40cm, high 60cm.
After carrying out Overheating Treatment to DAST Crystal Growth Solutions by temperature regulation and control, the temperature of DAST growth solutions is down to
1 DEG C below saturation point temperature, then cooled down with the rate of temperature fall of 0.1 DEG C/d, it is natural until there is the nucleus of spontaneous nucleation
It drops in cyclic annular L-type groove, then adjusts cooling process, crystal slowly crystallizes, and obtains high quality DAST monocrystalline, crystalline size
More than 12 × 12 × 1mm3, 20% can be about improved compared to V-type groove crystal yield rate.
So far, attached drawing is had been combined the present embodiment is described in detail.It should be noted that in attached drawing or specification
In text, the realization method for not being painted or describing is form known to a person of ordinary skill in the art in technical field, not into
Row is described in detail.In addition, the above-mentioned definition to each element and method be not limited in the various concrete structures mentioned in embodiment,
Shape or mode, those of ordinary skill in the art simply can be changed or replaced to it, such as：Integral type can also be utilized
Water-bath circulation cylinder replace the split type water-bath circulation cylinder that is made of water-bath circulation cylinder and heating water bath cylinder, at this time by circulating pump
Inlet and outlet pipes be connected to the water-bath circulation cylinder, you can the aqueous solution in water-bath circulation cylinder is recycled, at the same by heating rod and
Brilliant bottle is educated to be set in the water-bath circulation cylinder.It is appreciated that the water-bath circulation cylinder of split type water-bath circulation cylinder compared with integral type
Temperature control is more stable.
In conclusion ingehious design of the present invention ring ladder pedestal and the water-bath circulatory system, pedestal and to educate brilliant bottle perfect
Matching increases the effective area for carrying brilliant inclined plate, controls product core nucleation site, improves aqueous temperature stability, carries out high quality
The growth of DAST crystal.The grower, simple in structure, easily operated, nucleation site is controllable, can carry out the organic DAST of batch
Crystal growth is widely used in organic nonlinear optical crystal preparation field.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical solution and advantageous effect
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the protection of the present invention
Within the scope of.
Claims (10)
1. a kind of ring ladder pedestal for organic crystal spontaneous nucleation growth, it can cover and be set to one and educate bottom in brilliant bottle
Portion, it is in ladder by n grades of cyclic annular L-type grooves that the ring ladder pedestal, which has a ring ladder groove, the ring ladder groove,
Be distributed, wherein n >=2, per the bottom surface of cyclic annular L-type groove described in level-one and to educate brilliant bottom of bottle portion parallel to each other, side with educate crystalline substance
Bottom of bottle portion is at an angle of 90.
2. ring ladder pedestal according to claim 1, which is characterized in that the bottom surface of cyclic annular L-type groove described in per level-one
Width and profile height are 4~6mm.
3. ring ladder pedestal according to claim 1, which is characterized in that the ring ladder pedestal is by polytetrafluoroethylene (PTFE)
Material is made.
4. a kind of organic crystal spontaneous nucleation growth system, including water-bath circulator, temperature control equipment and crystal growth dress
It sets, wherein：
The water-bath circulator includes the water-bath circulation cylinder and circulating pump being connected, by the circulating pump to water-bath circulation cylinder
Interior aqueous solution is recycled；
The temperature control equipment includes heating rod, temperature sensor, temperature controller and temperature feedback processor, wherein：
The heating rod and temperature sensor are respectively arranged in water-bath circulation cylinder；
The temperature feedback processor is connected to temperature sensor, is acquired and locates for the data to the temperature sensor
Reason；
The temperature controller is connected to temperature feedback processor and heating rod, for the processing knot according to temperature feedback processor
Fruit controls the heating rod；
The crystal growing apparatus includes educating brilliant bottle and the ring ladder pedestal as described in claims 1 to 3 any one, described
The covering of ring ladder pedestal is set to and educates bottom in brilliant bottle, described to educate brilliant bottle and be positioned in the water-bath circulation cylinder.
5. organic crystal spontaneous nucleation growth system according to claim 4, which is characterized in that the water-bath circulation cylinder packet
It includes and cylinder and heating water bath cylinder is grown by the water-bath that circulating line is connected, wherein be provided with described educate in the water-bath growth cylinder
Brilliant bottle, the heating rod is provided in the heating water bath cylinder, and the temperature sensor is two and is respectively arranged at the water
In bath growth cylinder and heating water bath cylinder, the circulating pump is set on the circulating line.
6. organic crystal spontaneous nucleation growth system according to claim 5, which is characterized in that the crystal growing apparatus
Further include crystal growing furnace, the water-bath growth cylinder is set in the crystal growing furnace, grows cylinder and crystal in the water-bath
Thermal insulation material is provided between growth furnace.
7. organic crystal spontaneous nucleation growth system according to claim 6, which is characterized in that the crystal growing furnace by
Stainless steel material is made.
8. organic crystal spontaneous nucleation growth system according to claim 5, which is characterized in that the circulating line is by glass
Glass material is made, and outside is coated with thermal insulation material.
9. the organic crystal spontaneous nucleation growth system according to claim 4 to 8 any one, it is characterised in that：
Described to educate brilliant bottle for cylinder, the ring ladder pedestal is cylinder；
It is described to educate brilliant bottle and water-bath circulation cylinder is made by glass material.
10. a kind of organic crystal spontaneous nucleation growth system as described in claim 4 to 8 any one prepare it is organic non-thread
Application in property optical crystal, the especially application in preparing DAST crystal.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810504593 | 2018-05-23 | ||
| CN2018105045933 | 2018-05-23 |
Publications (2)
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| JPH10212192A (en) * | 1997-01-27 | 1998-08-11 | Japan Energy Corp | Method for growing bulk crystal |
| US6200385B1 (en) * | 2000-03-20 | 2001-03-13 | Carl Francis Swinehart | Crucible for growing macrocrystals |
| JP2006027967A (en) * | 2004-07-16 | 2006-02-02 | Ricoh Co Ltd | Apparatus and method for manufacturing substrate with organic crystal |
| CN204918834U (en) * | 2015-09-09 | 2015-12-30 | 重庆文理学院 | Frame is cultivateed with cascaded single crystal in laboratory |
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| CN106757346A (en) * | 2016-12-19 | 2017-05-31 | 山东大学 | A kind of method for protecting aqueous solution growth plane of crystal step |
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