CN109652854A - A kind of single crystal cultivation device and monocrystal cultivation method - Google Patents
A kind of single crystal cultivation device and monocrystal cultivation method Download PDFInfo
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- CN109652854A CN109652854A CN201811653838.5A CN201811653838A CN109652854A CN 109652854 A CN109652854 A CN 109652854A CN 201811653838 A CN201811653838 A CN 201811653838A CN 109652854 A CN109652854 A CN 109652854A
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- 239000013078 crystal Substances 0.000 title claims abstract description 102
- 238000012364 cultivation method Methods 0.000 title claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 67
- 230000012010 growth Effects 0.000 claims description 39
- 230000003750 conditioning effect Effects 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 16
- 239000013077 target material Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 6
- 239000012047 saturated solution Substances 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 3
- 230000005693 optoelectronics Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 abstract description 23
- 150000001875 compounds Chemical group 0.000 description 22
- 239000000243 solution Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 5
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- 238000002474 experimental method Methods 0.000 description 4
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- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000000935 solvent evaporation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002288 cocrystallisation Methods 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- -1 crystallite Substances 0.000 description 1
- 238000012136 culture method Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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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
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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
The invention discloses a kind of single crystal cultivation devices, including accommodating unit and culture unit, wherein culture unit includes the first bottle body, the second bottle body and the second lid.Required amount of through-hole is offered on the portion perimeter wall surface of the first area of second bottle body；Second lid includes closure and takes shape in extension in closure and vertically extending；For extension after the second lid is installed on the second opening of the second bottle body, having makes at least partly open first state of through-hole, and makes the second state that at least partly through-hole is blocked.Second bottle body and the second lid are used cooperatively, and the via count that can be blocked to extension is adjusted, that is, the percent opening of through-hole on the second bottle body is adjusted.When being loaded with the second volatile solvent in the second bottle body, the diffusion rate of solvent is adjusted by adjusting percent opening, improves the monocrystalline quality of culture.The invention discloses a kind of monocrystal cultivation methods, using above-mentioned device, can grow to obtain high quality single crystal.
Description
Technical field
The present invention relates to single crystal cultivation technical fields, and in particular to a kind of single crystal cultivation device and monocrystal cultivation method.
Background technique
Crystal refers to inside substance particle (molecule, atom or ion) in three-dimensional space in being repeated cyclically consolidating for arrangement
Body is the most stable state of thermodynamics existing for substance.Crystalline material is relative to amorphous materials and thin-film material, due to high heap
Product density, good crystal quality and low crystal boundary etc., excellent application prospect is shown in fields such as electricity, optics, magnetics.
The physical property of crystal is often determined that the structure of crystal is decided by the accumulation relationship of material molecule by the structure of crystal.Want
Solution crystal structure needs to carry out X-ray single crystal diffraction to crystal, is parsed by the data of acquisition to crystal structure.It is being coordinated
The fields such as chemistry, Organometallic Chemistry, organic chemistry, inorganic material chemistry, bioinorganic chemistry, especially with crystal engineering and
In the relevant scientific research of supramolecular chemistry, structural analysis is carried out by X-ray single crystal diffraction and has become essential grind
Study carefully means.It is that must turn out good monocrystalline using the premise of X-ray single crystal diffraction parsing crystal structure, therefore monocrystalline
Culture is of great significance for compound structure parsing.
The method of single crystal cultivation is varied, including cooling method, room temperature volatility process, diffusion method, solvent-thermal method and colloidal sol
Gel method etc..Wherein, diffusion method is common synthetic method in experiment and production.Diffusion method is good and right using two kinds of intersolubilities
The biggish solvent A of the dissolubility difference of target compound and solvent B, for example, target compound has higher dissolution in solvent A
Degree, and solvent degree is lower in solvent B, meanwhile, solvent B is easy volatile solvent, and solvent A is not easy volatile solvent.It is closing
In container, the target compound crystallized will be needed to be dissolved in solvent A, solvent B is volatized into solvent A, makes the molten of compound
Solution degree constantly reduces, so that nucleus be precipitated, is grown to monocrystalline.The growth speed and quality of monocrystalline depend on the formation and life of nucleus
Long rate.If the synthesis speed of nucleus is greater than growth rate, it just will form a large amount of crystallites, and it is existing to be easy to appear " crystal reunion "
As.Conversely, too fast growth rate can also make crystal defect occur.Therefore, it is the quality for improving crystal growth, needs strictly to control
The synthesis speed and growth rate of combinations core.
At present with diffusion method culture monocrystalline, usually solvent A is contained in small container, solvent B is contained in larger appearance
In device, after larger container is sealed, it is volatized into solvent B in small container.But in above-mentioned single crystal growth process, due to solvent
Diffusion rate it is uncontrollable, lead to not to realize the effective control of rate for being formed and being grown to nucleus, cause to be mixed in crystal
Impurity, crystallite, crystal " reunion ", the generation for generating the bad phenomenons such as amorphous powder.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that overcoming the solvent in the prior art with diffusion method culture monocrystalline
Diffusion rate is uncontrollable, limits the defect of crystal growth quality.
For this purpose, the invention provides the following technical scheme:
In a first aspect, the present invention provides a kind of single crystal cultivation devices, comprising:
Accommodating unit has accommodating inner cavity；
Unit is cultivated, is set in the accommodating inner cavity, including the first bottle body, the second bottle body and the second lid；
First bottle body has first inner chamber, and the connection first inner chamber is opened with the first of the accommodating inner cavity
Mouthful；
Second bottle body has second inner chamber, and the second opening of connection second inner chamber and the accommodating inner cavity；Institute
The periphery wall face for stating the second bottle body has vertically extending first area and second area, and the first area is located at described the
The top in two regions offers required amount of through-hole on the portion perimeter wall surface of the first area；
Second lid includes closure, and takes shape in extension in the closure and vertically extending；It is described
Extension is installed on second opening in second lid, fits, has with the interior sidewall surface of second bottle body
Make at least partly described open first state of through-hole, and the second state for making at least partly described through-hole be blocked.
Preferably, above-mentioned single crystal cultivation device, further includes:
The temperature conditioning unit being set to outside the accommodating unit, the temperature conditioning unit is for adjusting in the accommodating inner cavity
Temperature.
It is further preferred that above-mentioned single crystal cultivation device, the temperature conditioning unit is to be set to accommodating unit outer side surface
On insulating layer.
Preferably, above-mentioned single crystal cultivation device, further includes:
Support unit is arranged in the accommodating inner cavity, offers on the support unit and is suitable for installing described first bottle
At least two mounting holes of body and second bottle body.
It is further preferred that above-mentioned single crystal cultivation device, the support unit is laterally to be embedded in the culture vessel
Interior support plate.
Preferably, above-mentioned single crystal cultivation device, the accommodating unit include:
Culture vessel, the culture vessel there is the accommodating inner cavity and the accommodating inner cavity is in communication with the outside the
Three openings；
Sealing element, being adapted to be mounted to the third opening makes the accommodating inner cavity form seal cavity.
Preferably, above-mentioned single crystal cultivation device, the extension are that have annular wall jaggy in the circumferential, described to lack
First area where the corresponding through-hole of mouth.
It is further preferred that above-mentioned single crystal cultivation device, the vertical height of the extension is greater than or equal to described the
The vertical height in one region.
Preferably, the circumferential lengths of above-mentioned single crystal cultivation device, the first area where the through-hole are shown
The half of first area whole circumferential lengths, the circumferential lengths of the extension are equal to the first area where the through-hole
Circumferential lengths.
Second aspect, the present invention provides a kind of monocrystal cultivation methods based on above-mentioned apparatus, comprising the following steps:
S1, the second solvent is added into the second bottle body, and the liquid level of the second solvent is lower than the height of first area；
Second lid is installed in the second opening of second bottle body by S2, and the extension of the second lid blocks first
The through-hole of partial through holes on region, remainder opens wide, and records the percent opening of through-hole；
The target material of crystallization to be grown is dissolved in the first solvent, obtains the saturated solution of target material, to first by S3
The saturated solution of target material is added in bottle body；
S4 closes accommodating unit, makes to accommodate inner cavity formation closing inner chamber；Stationary culture, until target material is grown to monocrystalline；
S5 judges the monocrystalline quality of growth, if monocrystalline quality reaches aimed quality, culture terminates；
If monocrystalline quality is lower than aimed quality, S2 step is returned, the percent opening of through-hole is adjusted, then proceedes to S3 and S4 step
Suddenly.
Preferably, above-mentioned cultural method, further includes: S6 repeats S5 step, until monocrystalline quality reaches aimed quality.
Preferably, above-mentioned cultural method, the S4 step include: closing accommodating unit (1), make to accommodate inner cavity formation envelope
Close inner cavity；Using temperature conditioning unit (3), the temperature in accommodating inner cavity, stationary culture, until target material is grown to monocrystalline are set.
Preferably, above-mentioned cultural method, the S5 step include:
Judge the monocrystalline quality of growth, if monocrystalline quality reaches aimed quality, culture terminates；If monocrystalline quality is lower than target
Quality returns to S2 step, adjusts the temperature in the percent opening and accommodating inner cavity of through-hole (221), then proceedes to S3 and S4 step.
The third aspect, the present invention provides a kind of monocrystalline, the monocrystalline is obtained by above-mentioned single crystal cultivation device culture.
Fourth aspect, the present invention provides the monocrystalline by above-mentioned single crystal cultivation device culture to prepare optical element, lead to
Interrogate the application in element, laser device, optoelectronic component and/or piezoelectric element.
Technical solution of the present invention has the advantages that
1. single crystal cultivation device provided by the invention, including accommodating unit and culture unit, culture unit include first bottle
Body, the second bottle body and the second lid.The single crystal cultivation device of this structure, when being used to cultivate monocrystalline, by the first of the first bottle body
The first solvent for being dissolved with target compound is contained in inner cavity, contains the second solvent in the second inner chamber of the second bottle body, second
The liquid level of solvent is located in second area, to prevent the second solvent from flowing out the second bottle body by through-hole.First solvent is to target
The solubility of compound is high, hardly possible is volatilized, and the second solvent is low to the solubility of target compound, volatile.Due to the second bottle body
Required amount of through-hole is offered on the portion perimeter wall surface in one region, after the second lid is installed in the second opening, second
By the through-hole on bottle body to external diffusion after solvent volatilization, the second sovent diffusion enters in the first bottle body, mixes with the first solvent,
Making the solubility of target compound reduces, and then crystallizes and be precipitated.
Make at least partly described open first state of through-hole since the extension of the second lid has, and makes at least portion
The second state for dividing the through-hole to be blocked, it is the location of upper in the second opening by adjusting the second lid, it can be to extension
The via count that the via count and not extended portion that portion is blocked are blocked is adjusted, that is, to through-hole on the second bottle body
Percent opening is adjusted.By controlling the percent opening of through-hole, effective adjusting to the second solvent rate of volatilization can be realized, in turn
It realizes effective control to nucleation rate and growth rate, improves the growth conditions of monocrystalline, improve the monocrystalline quality of growth.
Particularly with the compound that growth conditions is unknown, the percent opening of through-hole is adjusted using above-mentioned single crystal cultivation device, energy
The optimum solvent diffusion rate for being suitable for cultivating monocrystalline is accessed, crystal reunion, crystallite, crystal defect, amorphous powder etc. are avoided
Formation, obtain the monocrystalline with high quality.
2. single crystal cultivation device provided by the invention further includes the temperature conditioning unit being set to outside accommodating unit, temperature control list
Member realizes effective control to the temperature environment of crystal growth, reduces extraneous temperature for adjusting the temperature in the accommodating inner cavity
Influence of the degree variation to crystal growth.Since temperature influences the volatilization of solvent, by the adjusting to environment temperature, to the second solvent
Evaporation rate controlled；While adjusting the second solvent evaporation rate, cooperation adjusts vias rate on the second bottle body
Adjusting, with control the second solvent to accommodating inner cavity in volatile quantity.Temperature, which is adjusted, adjusts the two synergistic effect with percent opening, real
Now to the abundant control of the second sovent diffusion rate, with the formation and growth rate of Effective Regulation nucleus.In addition, passing through control temperature
Degree can reduce the probability of compound Yu solvent cocrystallization, improve the purity of the monocrystalline of growth.
3. single crystal cultivation device provided by the invention, further includes support unit, it is arranged in the accommodating inner cavity, support is single
At least two mounting holes for being suitable for installing the first bottle body and the second bottle body are offered in member.Multiple peaces can be set on support unit
Hole is filled, to increase the quantity of the first bottle body in single crystal cultivation device, in first bottle of different tumor growth monocrystalline, in a monocrystalline
Multiple groups parallel laboratory test can be carried out in incubation, be conducive to improve conventional efficient, save experimental cost, and effectively control is different
The uniformity of condition of culture between experimental group.In addition, being contained in the first different bottle bodies using above-mentioned single crystal cultivation device
The first solvent dissolved with different target compound, additionally it is possible to realize and be cultivated in same accommodating inner cavity with the life of identical second solvent
Long different monocrystalline.
4. single crystal cultivation device provided by the invention, support unit is laterally to be embedded the support plate in culture vessel.Benefit
With support plate, simplify the structure of single crystal cultivation device, while by opening up mounting hole on the supporting plate, realizing in same culture ring
It is cultivated while under border to multiple groups monocrystalline.
5. single crystal cultivation device provided by the invention, the accommodating unit include: culture vessel, the culture vessel has
The accommodating inner cavity and the third opening that the accommodating inner cavity is in communication with the outside；Sealing element is adapted to be mounted to the third
Opening makes the accommodating inner cavity form seal cavity.Using sealing element, so that the accommodating inner cavity of culture vessel is formed sealing inner cavity, be
Crystal growth provides sealed environment, avoids the interference of external environment, make after the second sovent diffusion can well into the first bottle body,
It is effectively mixed with the first solvent.
6. single crystal cultivation device provided by the invention, the extension is that have annular wall jaggy in the circumferential, described
Notch corresponds to the first area where the through-hole.Since extension is the annular wall in circumferential direction with notch, by changing the
Two lids are opened in the upper locating relative position of the second opening to the via count blocked by annular wall and by notch
Via count is adjusted, and realizes that extension makes at least partly described open first state of through-hole, and makes at least partly described
The second state that through-hole is blocked.It is adjusted, is realized to second by the percent opening to the through-hole on the second bottle body periphery wall
Effective control of second sovent diffusion rate in bottle body.
7. single crystal cultivation device provided by the invention, the vertical height in vertical height >=first area of the extension
Degree makes extension at the position for the first area being located at where through-hole, and ring extension can be completely covered in a vertical direction
Through-hole.
8. the circumferential lengths of single crystal cultivation device provided by the invention, the first area where the through-hole are shown
The half of first area whole circumferential lengths, the circumferential lengths of the extension are equal to the first area where the through-hole
Circumferential lengths.The single crystal cultivation device of this structure, by the way that the position of first area corresponding to extension and notch is arranged,
It can be realized the adjusting to the percent opening of through-hole from 0-100%, and then obtain the wide regulation model of the second sovent diffusion rate
It encloses, in actual operation, is conducive to the best culture adjusting for the crystal growth that screening is obtained suitable for target compound.
9. monocrystal cultivation method provided by the invention can be realized and train to diffusion method using above-mentioned single crystal cultivation device
The Effective Regulation of the sovent diffusion rate of monocrystalline is supported, and then realizes effective control to nucleation rate and growth rate, training
It supports and obtains the monocrystalline with high quality.The corresponding crystal growth quality of percent opening by recording different through-holes, can be fitted
In the optimum opening porosity of growth monocrystalline.Using above-mentioned cultural method, compound that can be unknown to single crystal cultivation condition is carried out
Experiment screening obtains the optimum experimental condition suitable for compound growth monocrystalline.On the basis of adjusting percent opening, further cooperate
The temperature in accommodating inner cavity is adjusted, the optimal second sovent diffusion rate suitable for crystal growth can be obtained.
10. the monocrystalline of single crystal cultivation device culture provided by the invention is preparing optical element, communication element, laser
Application in part, optoelectronic component and/or piezoelectric element.By above-mentioned single crystal cultivation culture apparatus, nucleus is formed and raw
Long rate is controlled, suitable for preparing the high birefringece crystal of growth difficulty, nonlinear crystal, photorefractive crystal, piezo crystals
Body etc..Wherein, using the available linearly polarized light of the characteristic of birefringece crystal, the displacement etc. to light beam is realized, so that two-fold
Penetrating crystal becomes the pass of the optical elements such as production optoisolator, circulator, pattern displacement device, optical polariser and optical modulator
Key material.Core of the nonlinear crystal as all solid state laser frequency transformation, suitable for preparing laser device, optics, communication,
The fields such as medical treatment, military affairs play increasingly important role.Photorefractive crystal becomes in the light being irradiated on crystalline material
When change, the generation of crystals charge is heterogeneous to be redistributed, so that the refractive index of crystal changes, photorefractive material is in light
Have in many laser such as amplification, high density data storage, phase conjugate, hologram image processing and program interconnection and photoelectron technology
There is important potential using value.Piezo-electric crystal utilizes its piezoelectric effect, occurs in highly selective filter, high-power ultrasonics
Have in the instruments such as device, memory, load cell, underwater acoustic transducer, sound surface delay device, piezoelectric generator and piezoelectric transformer
It is widely used.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is to provide the main view of single crystal cultivation device in the embodiment of the present invention 1；
Fig. 2 is the top view of the support unit provided in the embodiment of the present invention 1；
Fig. 3 is the structural schematic diagram of the second bottle body provided in the embodiment of the present invention 1；
Fig. 4 is the structural schematic diagram after the second bottle body horizontal spreading provided in the embodiment of the present invention 1；
Fig. 5 is the main view of the second lid in the embodiment of the present invention 1；
Fig. 6 is the left view of the second lid in the embodiment of the present invention 1；
Fig. 7 is the top view of the second lid in the embodiment of the present invention 1；
Description of symbols:
1- accommodating unit, 11- culture vessel, 12- sealing element；
2- cultivates unit, the first bottle body of 21-, the second bottle body of 22-, 221- through-hole, the second lid of 23-, 231- envelope
Closing part, 232- extension；
3- temperature conditioning unit；
4- support unit, the first mounting hole of 41-, the second mounting hole of 42-.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
As long as in addition, the non-structure each other of technical characteristic involved in invention described below different embodiments
It can be combined with each other at conflict.
Embodiment 1
The present embodiment provides a kind of single crystal cultivation devices, including accommodating unit 1, culture unit 2, temperature conditioning unit 3 and support
Unit 4.Wherein, accommodating unit 1 has accommodating inner cavity, cultivates unit 2 and support unit 4 is set in accommodating inner cavity, temperature control list
Member 3 is set to the outside of accommodating unit 1.
As shown in Figure 1, accommodating unit 1 includes culture vessel 11 and sealing element 12.Wherein, culture vessel 11 has in accommodating
Chamber and the third opening that accommodating inner cavity is in communication with the outside, for example, culture vessel 11 is hydrostatic column, in hydrostatic column
Inside forms accommodating inner cavity, and third opening is formed on the top of hydrostatic column；Sealing element 12, which is adapted to mount to third opening, to be made to hold
It sets inner cavity and forms seal cavity, for example, sealing element 12 is sealing cover, sealing cover is covered in the third opening of hydrostatic column,
Form the accommodating inner cavity of sealing.
Cultivating unit 2 includes the first bottle body 21, the second bottle body 22 and the second lid 23, wherein the first bottle body 21 and second bottle
Body 22 is installed on the support unit 4 in accommodating inner cavity.As depicted in figs. 1 and 2, support unit 4 is to be embedded at culture vessel 11
Circular base slab in interior sidewall surface, support plate are parallel with the bottom wall of culture vessel 11.It offers on the supporting plate several
The maximum of a first mounting hole 41 and second mounting hole 42, corresponding first bottle body 21 of the aperture size of the first mounting hole 41 is outer
Diameter is arranged in the first bottle body 21 in first mounting hole 41, and corresponding second bottle body 22 of the aperture size of the second mounting hole 42 is most
Big outer diameter is arranged in the second bottle body 22 in second mounting hole 42.Above-mentioned 4 structure setting of support unit is simple, can be simultaneously
Support multiple first bottle bodies 21 and the second bottle body 42.
First bottle body 21 has first inner chamber, and connection first inner chamber and the first opening for accommodating inner cavity.Specifically,
One bottle body 21 can be the tapered reaction tube in bottom, and reaction tube utilizes the part with larger outer diameter to be fastened on the first mounting hole
In 41, it is suitable for containing the first solvent for being dissolved with target compound to be crystallized in the first inner chamber of reaction tube, the first solvent is
High to the solubility of target compound and nonvolatile solvent.Second bottle body 22 has second inner chamber, and connection second inner chamber
It is open with the second of accommodating inner cavity, for example, the second bottle body 22 is long-neck solvent bottle.As shown in Figure 3 and Figure 4, second bottle body 22
Periphery wall face has vertically extending first area and second area, and first area is located at the top of second area, first
Required amount of through-hole 221 is offered on the portion perimeter wall surface in region.As shown in figure 4, first area is extended transversely
Direction is divided into third region and the fourth region, opens up on the periphery wall surface in third region respectively transversely (circumferential direction) and vertical
The array through-hole 221 of (axial direction) arrangement, specifically, the circumferential lengths for offering the third region of through-hole 221 are first areas
The half of circumferential lengths.It is suitable for containing the second solvent in the second inner chamber of second bottle body 22, the second solvent is to target compound
The low and volatile solvent of solubility.The liquid level of the second solvent is lower than the vertical height of second area in second inner chamber, prevents
Only the second solvent overflows bottle body by the through-hole 221 on first area.Second solvent is by being provided with 22 periphery wall surface of the second bottle body
On through-hole 221, can volatilize diffuse to accommodating inner cavity in.The volume of first bottle body 21 less than the second bottle body 22 volume, with
The use ratio of first solvent and the second solvent during the suitable single crystal cultivation of offer.
As shown in Figure 5-Figure 7, the second lid 23 include closure 231 and form with it is in closure 231 and vertically extending
Extension 232.For example, the second lid 23 is circular grinding port plug, closure 231 is the round bottom cover of grinding port plug, extension
232 be the annular wall taken shape on bottom cover.Second lid 23 is adapted to mount in the second opening of the second bottle body 22, is being installed to
Behind position, the extension 232 of the second lid 23 and the interior sidewall surface of the second bottle body 22 fit.The outer diameter of extension 232 is less than envelope
The outer diameter of closing part 231, convenient for installation and removal of second lid 23 in the second opening.Extension 232 has notch, extension
232 are presented the annular wall for having excalation in circumferential direction.Second lid 23 is opened in be installed on the second bottle body 22 second
After on mouth, the second lid 23 is made to change the position of annular wall and the corresponding first area of notch by the second lid 23 of rotation
The selectivity of extension 232 block the through-hole 221 in 22 peripheral outer wall of the second bottle body, extension 232 has and makes at least partly to lead to
The open first state in hole 221, and make the second state that at least partly through-hole 221 blocks again.For example, extension 232 is perpendicular
It is equal to the vertical height of first area to height, when the second lid 23 rotation to a certain position, extension 232 can be by correspondence
Through-hole 221 on the first area of position all blocks, and vertically disposed through-hole 221 is avoided to influence due to that can not be blocked pair
The adjusting of 221 percent opening of through-hole.The circumferential lengths of extension 232 are equal to the circumferential lengths in third region, that is, extension 232
Circumferential lengths be first area circumferential lengths half.After the second lid 23 is installed in the second opening, the second lid of rotation
Body 23 makes the position in the corresponding third region of extension 232, then through-hole 221 is extended portion 232 and all blocks；Rotate the second lid
23, make the position of the corresponding the fourth region of extension 232, then through-hole 221 all opens wide, by the second lid 23 in above-mentioned two position
Between rotate, can be realized through-hole 221 by the different percent openings of 0-100%.
By being used cooperatively for the second bottle body 22 and the second lid 23, to opening for the through-hole 221 opened up on the second bottle body 22
Porosity is adjusted, and with the diffusion rate of the second solvent contained in Effective Regulation second inner chamber, and then realizes and is formed to nucleus
It to obtain the monocrystalline with high quality is the structure elucidation of the application of subsequent monocrystalline, compound with effective control of growth rate
Etc. providing advantage.The single crystal cultivation device of above-mentioned sovent diffusion controllable-rate is conducive to the growth conditions for improving monocrystalline,
The formation for avoiding crystal reunion, crystallite, crystal defect, amorphous powder etc., realizes the culture of high quality single crystal.
Temperature conditioning unit 3 is set to the outside of culture unit 2, for example, temperature conditioning unit is attached on 11 outer wall of culture vessel
Insulating layer, insulating layer can be set in whole outside wall surfaces of culture vessel 11, or only around the first bottle body 21 and
Position in two bottle bodies 22 more than second solvent liquid level height is coated.It, can be to the temperature in accommodating inner cavity by insulating layer
Degree environment is adjusted, and keeps the isoperibol in single crystal growth process, avoids changing due to ambient temperature to crystal growth
Adverse effect.Since temperature influences the volatilization of solvent, by the adjusting to environment temperature, the evaporation rate of the second solvent is carried out
Control；While adjusting the second solvent evaporation rate, cooperation adjusts the adjusting of vias rate on the second bottle body, to control the
Volatile quantity of two solvents into accommodating inner cavity.Temperature, which is adjusted, adjusts the two synergistic effect with percent opening, realizes and expands the second solvent
The abundant control of rate is dissipated, with the formation and growth rate of Effective Regulation nucleus.In addition, passing through the temperature in control accommodating inner cavity
Degree can reduce the purity of the probability of compound and solvent cocrystallization, the monocrystalline for improving growth, further increase crystal growth
Quality.
First area as first alternative embodiments of the present embodiment, where the through-hole 221 of the second bottle body 22
Circumferential lengths be also less than the circumferential lengths of whole first areas, or greater than the circumferential lengths of whole first areas, only
Through-hole 221 is opened up on the position of first area, enable the second solvent by being diffused by through-hole.As change
Shape, the circumferential lengths of extension 232 are also less than the circumferential lengths of the first area where through-hole, or are greater than where through-hole
First area circumferential lengths, as long as make extension 232 circumferential lengths be less than first area circumferential lengths, pass through change
The position of second lid 23, extension can be made, which to have, to be made at least partly open first state of through-hole 221 and makes at least portion
The second state for dividing through-hole 221 to be blocked.As further deformation, the arrangement of through-hole 221 can also be other arrangements
Mode, for example, cluster arrangement or irregular arrangement etc., it is only necessary under the cooperation of the second bottle body 22 and the second lid 23, make
It is blocked to 221 property of can choose of through-hole, to adjust the percent opening of through-hole 221.
As second alternative embodiments of the present embodiment, the notch of the extension 232 of the second lid 23, which is opened, may be used also
To be located at the inside of annular wall.For example, annular wall horizontal spreading is rectangle, and notch corresponds to inside rectangular annular wall
Lack part.As long as making the first lid 23 after being installed in the second opening, extension 232 is imperfect block through-hole 221 or
It opens wide through-hole 221 all, can be realized the first state and the second state of extension 232.
As the alternative embodiment of third of the present embodiment, the second bottle body 22 and the second lid 23 can also be it
His shape, for example, the second bottle body 22 is polyhedron, then the second lid 23 is the correspondingly-shaped with the second bottle body 22, it is only necessary to be protected
Card opens up through-hole on the periphery wall surface of the second bottle body 22, after the second lid 23 is installed on the second bottle body 22, Neng Goutong
The relative position for crossing the second lid 23 of change makes extension have first state and the second state.As deformation, first bottle
Body 21 can also be other shapes, for example, cylindrical bottle body etc..As deformation, culture vessel 11 can also be other shapes
Container, for example, cuboid, square etc..As further deformation, sealing cover can also be that other are adapted to be mounted to the
Sealing element 12 in three openings, for example, elastic cock body etc. makes to accommodate as long as making sealing element 12 after being installed on third opening
Inner cavity is capable of forming sealing inner cavity.
As the 4th alternative embodiment of the present embodiment, support plate can also be other shapes, the branch of structure
Support unit 4.For example, support unit 4 includes a level board for being parallel to 11 bottom of culture vessel, at two opposite ends of level board
Portion connects vertical plate, and the one end of vertical plate far from level board is set in the bottom wall of culture vessel 11 by fixinig plate etc..
By starting the first mounting hole 41 and the second mounting hole 42 on level board, equally can be realized to the first bottle body 21 and second bottle
Body 22 supports.As deformation, it can also be not provided with support unit 4 in accommodating inner cavity, by the first bottle body 21 and the second bottle body
22 are placed directly in the bottom wall of culture vessel 11, can equally be entered by the second solvent volatilization in the second bottle body 22
First bottle body 21, realizes the culture of monocrystalline.
As the 5th alternative embodiment of the present embodiment, temperature conditioning unit 3 can also be insulating box etc., will accommodate
Unit 1 is placed in insulating box, realizes the control to temperature in accommodating inner cavity.As deformation, temperature conditioning unit can also be not provided with
3。
Embodiment 2
The present embodiment provides a kind of monocrystal cultivation methods, for example, the target material of monocrystalline to be grown is feux rouges material of main part
The chemical structure of NPAFN, NPAFN are as follows:
Using embodiment 1 provide any single crystal cultivation device cultivated, cultural method the following steps are included:
S1 is added the second solvent (such as: n-hexane) into the second bottle body 22, and the liquid level of the second solvent is lower than first
The height in region；
Second lid 23 is installed in the second opening of second bottle body 22, the extension 232 of the second lid 22 by S2
The partial through holes on first area are blocked, the through-hole of remainder opens wide, and records the percent opening of through-hole；
S3 takes the target material of about 5mg in test tube with clean spoon, be added in test tube the first solvent (such as: two
Chloromethanes) about 3ml, ultrasound dissolves target material sufficiently；
After target material is completely dissolved, a small amount of material and ultrasound are continuously added, until be trained supersaturated solution, to the
The supersaturated solution of target material is added in one bottle body 21；Wherein, about 5 times of the amount for the second solvent being added in the second bottle body 22
The amount for the supersaturated solution that (volume) is added in the first bottle body 21；
S4 closes accommodating unit 1, makes to accommodate inner cavity formation closing inner chamber；It is arranged in accommodating inner cavity using temperature conditioning unit (3)
Temperature be 20 DEG C, stationary culture, until target material is grown to monocrystalline.
S5 judges the monocrystalline quality of growth, if monocrystalline quality reaches aimed quality, culture terminates；
If monocrystalline quality is lower than aimed quality, S2 step is returned, adjusts the percent opening of through-hole, and in selective control accommodating
Temperature in chamber then proceedes to S3 and S4 step.
S6 repeats S5 step, until monocrystalline quality reaches aimed quality.
Using above-mentioned single crystal cultivation device, effective tune of the sovent diffusion rate to diffusion method culture monocrystalline can be realized
Control, and then realize effective control to nucleation rate and growth rate, culture obtains the monocrystalline with high quality.Pass through note
The corresponding crystal growth quality of percent opening for recording different through-holes can obtain the optimum opening porosity for being suitable for growing monocrystalline, by opening
Porosity adjusts cooperation temperature and adjusts, and obtains the best diffusion rate of the second solvent suitable for crystal growth.Utilize above-mentioned culture
Method, compound that can be unknown to single crystal cultivation condition carry out experiment screening, obtain suitable for the best of compound growth monocrystalline
Experiment condition.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (15)
1. a kind of single crystal cultivation device characterized by comprising
Accommodating unit (1) has accommodating inner cavity；
It cultivates unit (2), is set in the accommodating inner cavity, including the first bottle body (21), the second bottle body (22) and the second lid
(23)；
First bottle body (21) has first inner chamber, and the connection first inner chamber is opened with the first of the accommodating inner cavity
Mouthful；
Second bottle body (22) has second inner chamber, and the second opening of connection second inner chamber and the accommodating inner cavity；Institute
The periphery wall face for stating the second bottle body (22) has vertically extending first area and second area, and the first area is located at institute
The top of second area is stated, required amount of through-hole (221) are offered on the portion perimeter wall surface of the first area；
Second lid (23) includes closure (231), and takes shape on the closure (231) and vertically extending prolong
Extending portion (232)；The extension (232) is installed on second opening in second lid (23), with second bottle body
(22) interior sidewall surface fits, and having makes at least partly open first state of the through-hole (221), and makes at least portion
The second state for dividing the through-hole (221) to be blocked.
2. single crystal cultivation device according to claim 1, which is characterized in that further include:
It is set to the external temperature conditioning unit (3) of the accommodating unit (1), the temperature conditioning unit (3) is for adjusting in the accommodating
Temperature in chamber.
3. single crystal cultivation device according to claim 2, which is characterized in that the temperature conditioning unit (3) is to be set to accommodating
Insulating layer on unit (1) outer side surface.
4. single crystal cultivation device according to claim 1-3, which is characterized in that further include:
Support unit (4) is arranged in the accommodating inner cavity, offers on the support unit (4) and is suitable for installation described first
At least two mounting holes of bottle body (21) and second bottle body (22).
5. single crystal cultivation device according to claim 4, which is characterized in that the support unit (4) is laterally to be embedded
Support plate in the culture vessel (11).
6. single crystal cultivation device according to claim 1-5, which is characterized in that accommodating unit (1) packet
It includes:
Culture vessel (11), the culture vessel (11) have the accommodating inner cavity and the accommodating inner cavity are in communication with the outside
Third opening；
Sealing element (12), being adapted to be mounted to the third opening makes the accommodating inner cavity form seal cavity.
7. single crystal cultivation device according to claim 1-6, which is characterized in that the extension (232) be
There is the annular wall of notch, the notch corresponds to the first area where the through-hole (221) in circumferential direction.
8. single crystal cultivation device according to claim 7, which is characterized in that the vertical height of the extension (232) is big
In or equal to the first area vertical height.
9. single crystal cultivation device according to claim 1-8, which is characterized in where the through-hole (221)
The circumferential lengths of the first area are the half of shown first area whole circumferential lengths, the circumferential direction of the extension (232)
Length is equal to the circumferential lengths of the first area where the through-hole (221).
10. a kind of monocrystal cultivation method based on any one of claim 1-9 described device, which is characterized in that including following step
It is rapid:
S1, to the second solvent is added in the second bottle body (22), the liquid level of the second solvent is lower than the height of first area；
Second lid (23) is installed in the second opening of second bottle body (22), the extension of the second lid (23) by S2
(232) partial through holes (221) on first area are blocked, the through-hole (221) of remainder opens wide, and record through-hole (221) is opened
Porosity；
The target material of crystallization to be grown is dissolved in the first solvent, obtains the saturated solution of target material by S3, to the first bottle body
(21) saturated solution of target material is added in；
S4 is closed accommodating unit (1), makes to accommodate inner cavity formation closing inner chamber；Stationary culture, until target material is grown to monocrystalline；
S5 judges the monocrystalline quality of growth, if monocrystalline quality reaches aimed quality, culture terminates；
If monocrystalline quality is lower than aimed quality, S2 step is returned, adjusts the percent opening of through-hole (221), then proceedes to S3 and S4 step
Suddenly.
11. cultural method according to claim 10, which is characterized in that further include: S6 repeats S5 step, until monocrystalline
Amount reaches aimed quality.
12. cultural method described in 0 or 11 according to claim 1, which is characterized in that the S4 step includes: that closing accommodating is single
First (1) makes to accommodate inner cavity formation closing inner chamber；Using temperature conditioning unit (3) be arranged accommodating inner cavity in temperature, stationary culture, until
Target material is grown to monocrystalline.
13. the described in any item cultural methods of 0-12 according to claim 1, which is characterized in that the S5 step includes:
Judge the monocrystalline quality of growth, if monocrystalline quality reaches aimed quality, culture terminates；If monocrystalline quality is lower than target matter
Amount returns to S2 step, adjusts the temperature in the percent opening and accommodating inner cavity of through-hole (221), then proceedes to S3 and S4 step.
14. a kind of monocrystalline, which is characterized in that the monocrystalline is by the described in any item single crystal cultivation device cultures of claim 1-9
It obtains.
15. the monocrystalline by the described in any item single crystal cultivation device cultures of claim 1-9 is preparing optical element, communication member
Application in part, laser device, optoelectronic component and/or piezoelectric element.
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