CN209923480U - Single crystal cultivation device - Google Patents
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- CN209923480U CN209923480U CN201822274855.XU CN201822274855U CN209923480U CN 209923480 U CN209923480 U CN 209923480U CN 201822274855 U CN201822274855 U CN 201822274855U CN 209923480 U CN209923480 U CN 209923480U
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Abstract
The utility model discloses a single crystal cultivation device, including holding unit and cultivation unit, wherein, the cultivation unit includes first bottle, second bottle and second lid. The part of the peripheral wall surface of the first area of the second bottle body is provided with a required number of through holes; the second cover body comprises a closed part and an extension part which is formed on the closed part and extends vertically; the extension part has a first state that at least part of the through holes are opened and a second state that at least part of the through holes are shielded after the second cover body is arranged at the second opening of the second bottle body. The second bottle and the cooperation of second lid are used, can adjust the through-hole number that the extension sheltered from, also promptly, adjust the percent opening of through-hole on the second bottle. When the second bottle body is filled with the volatile second solvent, the diffusion rate of the solvent is adjusted by adjusting the aperture ratio, so that the quality of the cultured single crystal is improved.
Description
Technical Field
The utility model relates to a single crystal cultivation technical field, concretely relates to single crystal cultivation device.
Background
A crystal is a solid in which particles (molecules, atoms, or ions) inside the substance are periodically and repeatedly arranged in three dimensions, and is the most thermodynamically stable state in which the substance exists. Compared with amorphous materials and thin film materials, the crystalline materials have excellent application prospects in the fields of electricity, optics, magnetism and the like due to high packing density, good crystal quality, low grain boundary and the like. The physical properties of a crystal are often determined by the structure of the crystal, which is determined by the packing relationship of the molecules of the substance. To understand the crystal structure, X-ray single crystal diffraction is performed on the crystal, and the crystal structure is analyzed through the obtained data. In the fields of coordination chemistry, metal organic chemistry, inorganic material chemistry, bio-inorganic chemistry, and the like, particularly scientific research related to crystal engineering and supramolecular chemistry, structural analysis by X-ray single crystal diffraction has become an indispensable research means. Since the prerequisite for analyzing the crystal structure by diffraction using an X-ray single crystal is that a good single crystal must be cultured, the culture of a single crystal is of great significance for the analysis of the compound structure.
The method for single crystal growth is various, and includes a cooling method, a normal temperature volatilization method, a diffusion method, a solvothermal method, a sol-gel method, and the like. Among them, the diffusion method is a synthesis method commonly used in experiments and production. The diffusion method utilizes two solvents a and B which have good intersolubility and a large difference in solubility between the target compounds, for example, the target compound has a high solubility in the solvent a and a low solubility in the solvent B, and the solvent B is a volatile solvent and the solvent a is a non-volatile solvent. In a closed container, a target compound to be crystallized is dissolved in a solvent A, a solvent B is volatilized into the solvent A, the solubility of the compound is continuously reduced, and crystal nuclei are precipitated and grown into a single crystal. The growth rate and quality of the single crystal depend on the rate of formation and growth of the nuclei. If the formation rate of the crystal nucleus is greater than the growth rate, a large number of microcrystals are formed and the phenomenon of crystal agglomeration is easily caused. Conversely, a growth rate that is too fast can also cause defects in the crystal. Therefore, in order to improve the quality of single crystal growth, the formation rate and growth rate of crystal nuclei need to be strictly controlled.
At present, a single crystal is grown by a diffusion method, and generally, a solvent A is contained in a small container, a solvent B is contained in a large container, and the large container is sealed, and then the solvent B is volatilized into the small container. However, in the single crystal growth process, the diffusion rate of the solvent is not controllable, so that effective control of the nucleation and growth rate cannot be realized, and adverse phenomena such as impurity mixing in the crystal, microcrystallization, crystal "agglomeration", generation of amorphous powder and the like occur.
SUMMERY OF THE UTILITY MODEL
Therefore, the technical problem to be solved by the utility model is to overcome the defect that the diffusion rate of the solvent for growing single crystals by diffusion method is not controllable and the growth quality of single crystals is limited in the prior art.
Therefore, the utility model provides a following technical scheme:
in a first aspect, the present invention provides a single crystal growing apparatus, comprising:
the accommodating unit is provided with an accommodating inner cavity;
the culture unit is arranged in the accommodating inner cavity and comprises a first bottle body, a second bottle body and a second cover body;
the first bottle body is provided with a first inner cavity and a first opening which is communicated with the first inner cavity and the accommodating inner cavity;
the second bottle body is provided with a second inner cavity and a second opening which is communicated with the second inner cavity and the containing inner cavity; the peripheral wall surface of the second bottle body is provided with a first area and a second area which extend vertically, the first area is positioned above the second area, and a part of the peripheral wall surface of the first area is provided with a required number of through holes;
the second cover body comprises a closed part and an extension part which is formed on the closed part and extends vertically; the extension part is arranged on the second opening of the second cover body, is attached to the inner side wall surface of the second bottle body, and has a first state that at least part of the through holes are opened and a second state that at least part of the through holes are shielded.
Preferably, the above single crystal growing apparatus further comprises:
and the temperature control unit is arranged outside the accommodating unit and is used for adjusting the temperature in the accommodating inner cavity.
Further preferably, in the single crystal growth apparatus described above, the temperature control unit is a heat insulating layer disposed on an outer side wall surface of the accommodating unit.
Preferably, the above single crystal growing apparatus further comprises:
the supporting unit is arranged in the accommodating inner cavity, and at least two mounting holes suitable for mounting the first bottle body and the second bottle body are formed in the supporting unit.
Further preferably, in the above single crystal growth apparatus, the support unit is a support plate laterally embedded in the growth vessel.
Preferably, in the above single crystal growing apparatus, the accommodating unit includes:
the culture container is provided with the accommodating inner cavity and a third opening for communicating the accommodating inner cavity with the outside;
and the sealing element is suitable for being arranged on the third opening to enable the containing inner cavity to form a sealed cavity.
Preferably, in the single crystal growing apparatus described above, the extension portion is an annular wall having a notch in a circumferential direction, the notch corresponding to the first region where the through hole is located.
Further preferably, in the above single crystal growing apparatus, a vertical height of the extension portion is greater than or equal to a vertical height of the first region.
Preferably, in the single crystal growing apparatus described above, the circumferential length of the first region where the through hole is located is half of the entire circumferential length of the first region, and the circumferential length of the extension portion is equal to the circumferential length of the first region where the through hole is located.
Preferably, in the above single crystal growing apparatus, the outer diameter of the closing part (231) is larger than the outer diameter of the extending part (232).
In a second aspect, the present invention provides a single crystal cultivation method based on the above apparatus, comprising the following steps:
s1, adding a second solvent into the second bottle body, wherein the liquid level height of the second solvent is lower than that of the first area;
s2, mounting the second cover body on the second opening of the second bottle body, wherein the extension part of the second cover body shields part of through holes on the first area, the rest of the through holes are open, and the opening rate of the through holes is recorded;
s3, dissolving a target material to be crystallized in a first solvent to obtain a saturated solution of the target material, and adding the saturated solution of the target material into the first bottle body;
s4, sealing the containing unit to form a sealed inner cavity; standing and culturing until the target material grows into a single crystal;
s5, judging the quality of the grown single crystal, and finishing the culture if the quality of the single crystal reaches the target quality;
if the quality of the single crystal is lower than the target quality, the process returns to the step of S2, the opening ratio of the through-hole is adjusted, and then the steps of S3 and S4 are continued.
Preferably, the above culture method further comprises: s6, repeating the step S5 until the quality of the single crystal reaches the target quality.
Preferably, in the above culture method, the step S4 includes: the closed accommodating unit (1) enables the accommodating inner cavity to form a closed inner cavity; setting the temperature in the accommodating inner cavity by using the temperature control unit (3), and standing for culture until the target material grows into a single crystal;
preferably, in the above culture method, the step S5 includes:
judging the quality of the grown single crystal, and finishing the culture if the quality of the single crystal reaches the target quality; if the quality of the single crystal is lower than the target quality, the process returns to the step of S2, the opening ratio of the through hole (221) and the temperature in the receiving cavity are adjusted, and then the steps of S3 and S4 are continued.
In a third aspect, the present invention provides a single crystal, which is obtained by culturing the single crystal culture apparatus described above.
In a fourth aspect, the present invention provides the use of a single crystal grown by the above single crystal growing apparatus for the production of optical elements, communication elements, laser devices, optoelectronic elements and/or piezoelectric elements.
The utility model discloses technical scheme has following advantage:
1. the utility model provides a single crystal cultivation device, including holding unit and cultivation unit, the cultivation unit includes first bottle, second bottle and second lid. When the single crystal culture device with the structure is used for culturing a single crystal, the first inner cavity of the first bottle body is filled with the first solvent dissolved with the target compound, the second inner cavity of the second bottle body is filled with the second solvent, and the liquid level of the second solvent is positioned in the second area so as to prevent the second solvent from flowing out of the second bottle body through the through hole. The first solvent has high solubility and is difficult to volatilize to the target compound, and the second solvent has low solubility and is easy to volatilize to the target compound. Because the partial peripheral wall surface of the first area of the second bottle body is provided with the through holes in required quantity, after the second cover body is arranged on the second opening, the second solvent is volatilized and then is diffused outwards through the through holes on the bottle body, the second solvent is diffused into the first bottle body and is mixed with the first solvent, so that the solubility of the target compound is reduced, and further the target compound is crystallized and precipitated.
Because the extending part of the second cover body has a first state that at least part of the through holes are opened and a second state that at least part of the through holes are shielded, the number of the through holes shielded by the extending part and the number of the through holes not shielded by the extending part can be adjusted by adjusting the position of the second cover body on the second opening, namely, the opening rate of the through holes on the second bottle body is adjusted. Through the aperture ratio of control through-hole, can realize the effective regulation to second solvent rate of volatilizing, and then realize the effective control to crystal nucleus formation rate and growth rate, improve the growth condition of single crystal, improve the single crystal quality of growing. Particularly for compounds with unknown growth conditions, the single crystal cultivation device can be used for adjusting the aperture ratio of the through hole, so that the optimal solvent diffusion rate suitable for cultivating the single crystal can be obtained, the formation of crystal agglomeration, microcrystals, crystal defects, amorphous powder and the like can be avoided, and the single crystal with high quality can be obtained.
2. The utility model provides a single crystal cultivation device, still including setting up in the outside control by temperature change unit of holding unit, the control by temperature change unit is used for adjusting temperature in the holding inner chamber realizes the effective control to the temperature environment that the single crystal grows, reduces the influence that the ambient temperature changes the growth of single crystal. The volatilization speed of the second solvent is controlled by adjusting the environmental temperature because the temperature influences the volatilization of the solvent; when the volatilization speed of the second solvent is adjusted, the adjustment of the aperture ratio of the through hole on the second bottle body is adjusted in a matching way, so that the volatilization amount of the second solvent to the accommodating inner cavity is controlled. The temperature regulation and the aperture ratio regulation have synergistic effect, so that the diffusion rate of the second solvent is fully controlled, and the formation and growth rate of crystal nuclei are effectively regulated and controlled. In addition, the probability of co-crystallization of the compound and the solvent can be reduced by controlling the temperature, and the purity of the grown single crystal can be improved.
3. The utility model provides a single crystal cultivation device still includes the support element, sets up in the holding inner chamber, set up two at least mounting holes that are suitable for first bottle of installation and second bottle on the support element. Can set up a plurality of mounting holes on the supporting unit to increase the quantity of first bottle in the single crystal culture apparatus, at the first bottle internal growth single crystal of difference, can develop the parallel experiment of multiunit in single crystal cultivation process, be favorable to improving experimental efficiency, save the experiment cost, and the uniformity of culture condition between the different experimental groups of effective control. In addition, by utilizing the single crystal culture device, the first solvents with different target compounds dissolved in the first bottles are contained in different first bottles, and different single crystals grown by the same second solvent can be cultured in the same containing cavity.
4. The utility model provides a single crystal culture device, the support element transversely inlays the backup pad of establishing in culture container. The structure of the single crystal culture device is simplified by utilizing the supporting plate, and meanwhile, the simultaneous culture of a plurality of groups of single crystals in the same culture environment is realized by arranging the mounting holes on the supporting plate.
5. The utility model provides a single crystal cultivation device, the holding unit includes: the culture container is provided with the accommodating inner cavity and a third opening for communicating the accommodating inner cavity with the outside; and the sealing element is suitable for being arranged on the third opening to enable the containing inner cavity to form a sealed cavity. Utilize the sealing member, make culture vessel's holding inner chamber form sealed inner chamber, for the single crystal growth provides sealed environment, avoid external environment's interference, make in the second solvent can fully get into first bottle after the diffusion, effectively mix with first solvent.
6. The utility model provides a single crystal cultivation device, the extension is the annular wall that has the breach in week, the breach corresponds the first region at through-hole place. Because the extension part is an annular wall with a notch in the circumferential direction, the number of through holes shielded by the annular wall and the number of through holes opened by the notch are adjusted by changing the relative position of the second cover body on the second opening, so that a first state that the extension part enables at least part of the through holes to be opened and a second state that the extension part enables at least part of the through holes to be shielded are realized. The aperture ratio of the through hole on the peripheral wall of the second bottle body is adjusted, so that the diffusion rate of the second solvent in the second bottle body is effectively controlled.
7. The utility model provides a single crystal cultivation device, the vertical height of extension is more than or equal to the vertical height of first region makes the extension when being located the position of the first region at through-hole place, and the ring extension can cover the through-hole completely on vertical direction.
8. The utility model provides a single crystal cultivation device, the through-hole place the circumference length of first region is half of the whole circumference length of shown first region, the circumference length of extension equals the through-hole place the circumference length of first region. According to the single crystal culture device with the structure, the opening rate of the through hole can be adjusted from 0-100% by arranging the extension part and the position of the first area corresponding to the notch, so that a wide regulation range of the diffusion rate of the second solvent is obtained, and in actual operation, the optimal culture regulation suitable for the growth of the single crystal of the target compound is obtained by screening.
9. The utility model provides a method is cultivateed to single crystal utilizes foretell single crystal culture apparatus, can realize the effective regulation and control to the solvent diffusion rate of diffusion method cultivation single crystal, and then realizes the effective control to crystal nucleus formation rate and growth rate, cultivates and obtains having high-quality single crystal. By recording the growth quality of the single crystal corresponding to the aperture ratio of the different through holes, the optimum aperture ratio suitable for growing the single crystal can be obtained. By using the above culture method, compounds with unknown single crystal culture conditions can be experimentally screened to obtain the optimal experimental conditions suitable for growing single crystals of the compounds. On the basis of adjusting the aperture ratio, the temperature in the accommodating cavity is further adjusted in a matching manner, so that the optimal second solvent diffusion rate suitable for single crystal growth can be obtained.
10. The utility model provides an application of single crystal that single crystal culture apparatus cultivateed in preparation optical element, communication component, laser device, optoelectronic element and/or piezoelectric element. The single crystal culture and culture device controls the crystal nucleus formation and growth rate, and is suitable for preparing birefringent crystals, nonlinear crystals, photorefractive crystals, piezoelectric crystals and the like with high growth difficulty. The linearly polarized light can be obtained by utilizing the characteristics of the birefringent crystal, the displacement of light beams and the like are realized, and the birefringent crystal becomes a key material for manufacturing optical elements such as an optical isolator, a circulator, a light beam shifter, an optical polarizer, an optical modulator and the like. The nonlinear crystal is used as the core of frequency conversion of the all-solid-state laser, is suitable for preparing laser devices, and plays an increasingly important role in the fields of optics, communication, medical treatment, military and the like. When light irradiated on a crystal material changes, charges in the crystal are unevenly redistributed, so that the refractive index of the crystal changes, and the photorefractive crystal has important potential application value in a plurality of laser and photoelectron technologies such as light amplification, high-density data storage, phase conjugation, holographic image processing, program interconnection and the like. The piezoelectric crystal utilizes the piezoelectric effect thereof and has wide application in instruments such as a high-selectivity filter, a high-power ultrasonic generator, a memory, a load cell, an underwater acoustic transducer, a sound surface delay device, a piezoelectric generator, a piezoelectric transformer and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a front view of a single crystal growing apparatus according to example 1 of the present invention;
fig. 2 is a plan view of a support unit provided in embodiment 1 of the present invention;
fig. 3 is a schematic structural view of a second bottle body provided in embodiment 1 of the present invention;
fig. 4 is a schematic structural view of the second bottle body provided in embodiment 1 of the present invention after being laterally unfolded;
fig. 5 is a front view of a second cover body in embodiment 1 of the present invention;
fig. 6 is a left side view of the second cover in embodiment 1 of the present invention;
fig. 7 is a plan view of a second cover body in embodiment 1 of the present invention;
description of reference numerals:
1-containing unit, 11-culture vessel, 12-sealing member;
2-culture unit, 21-first vial, 22-second vial, 221-through hole, 23-second cap, 231-closure, 232-extension;
3-a temperature control unit;
4-support unit, 41-first mounting hole, 42-second mounting hole.
Detailed Description
The technical solution of the present invention will be described clearly and completely with reference to the accompanying drawings, and obviously, the described embodiments are some, but not all embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Furthermore, the technical features mentioned in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other.
Example 1
The embodiment provides a single crystal cultivation apparatus, which comprises a containing unit 1, a cultivation unit 2, a temperature control unit 3 and a supporting unit 4. The accommodating unit 1 is provided with an accommodating inner cavity, the culture unit 2 and the supporting unit 4 are arranged in the accommodating inner cavity, and the temperature control unit 3 is arranged outside the accommodating unit 1.
As shown in fig. 1, the housing unit 1 includes a culture vessel 11 and a sealing member 12. The culture container 11 has an accommodating inner cavity and a third opening for communicating the accommodating inner cavity with the outside, for example, the culture container 11 is a cylindrical container, the accommodating inner cavity is formed in the cylindrical container, and the third opening is formed at the top of the cylindrical container; the sealing member 12 is adapted to be mounted in the third opening to form a sealed cavity, for example, the sealing member 12 is a sealing cover, and the sealing cover is disposed on the third opening of the cylindrical container to form a sealed containing cavity.
The culture unit 2 includes a first bottle 21, a second bottle 22 and a second cover 23, wherein the first bottle 21 and the second bottle 22 are mounted on the supporting unit 4 in the accommodating cavity. As shown in FIGS. 1 and 2, the support unit 4 is a circular support plate which is fitted to the inner wall surface of the culture vessel 11 and is parallel to the bottom wall surface of the culture vessel 11. A plurality of first mounting holes 41 and a second mounting hole 42 are formed in the supporting plate, the size of the opening of each first mounting hole 41 corresponds to the maximum outer diameter of the corresponding first bottle body 21, so that the corresponding first bottle body 21 is clamped in the corresponding first mounting hole 41, and the size of the opening of each second mounting hole 42 corresponds to the maximum outer diameter of the corresponding second bottle body 22, so that the corresponding second bottle body 22 is clamped in the corresponding second mounting hole 42. The support unit 4 has a simple structure and can simultaneously support a plurality of first vials 21 and second vials 42.
The first bottle body 21 has a first inner cavity and a first opening communicating the first inner cavity and the accommodating inner cavity. Specifically, the first bottle 21 may be a reaction tube with a tapered bottom, the reaction tube is clamped in the first mounting hole 41 by a portion with a larger outer diameter, and a first inner cavity of the reaction tube is suitable for containing a first solvent for dissolving a target compound to be crystallized, and the first solvent is a solvent with high solubility to the target compound and non-volatility. The second bottle body 22 has a second inner cavity and a second opening communicating the second inner cavity and the accommodating inner cavity, for example, the second bottle body 22 is a long-neck solvent bottle. As shown in fig. 3 and 4, the outer peripheral wall surface of the second bottle 22 has a first region and a second region extending vertically, the first region is located above the second region, and a part of the outer peripheral wall surface of the first region is provided with a required number of through holes 221. As shown in fig. 4, the first region is divided into a third region and a fourth region along the direction of the transverse extension, the outer peripheral wall surface of the third region is provided with array through holes 221 arranged along the transverse direction (circumferential direction) and the vertical direction (axial direction), respectively, and specifically, the circumferential length of the third region provided with the through holes 221 is half of the circumferential length of the first region. The second bottle 22 has a second interior adapted to contain a second solvent, which is a solvent that is low in solubility and volatile with respect to the target compound. The liquid level of the second solvent in the second inner cavity is lower than the vertical height of the second area, so that the second solvent is prevented from overflowing the bottle body from the through hole 221 on the first area. The second solvent can be volatilized and diffused into the accommodating inner cavity through the through hole 221 formed in the peripheral wall surface of the second bottle body 22. The volume of the first bottle body 21 is smaller than that of the second bottle body 22 to provide a suitable ratio of the first solvent to the second solvent for the single crystal growth process.
As shown in fig. 5 to 7, the second cover 23 includes a closing portion 231 and an extending portion 232 formed on the closing portion 231 and extending in the vertical direction. For example, the second cover body 23 is a round burr plug, the closing portion 231 is a round bottom cover of the burr plug, and the extending portion 232 is an annular wall formed on the bottom cover. The second cover 23 is suitable for being mounted on the second opening of the second bottle 22, and after being mounted in place, the extending portion 232 of the second cover 23 is attached to the inner sidewall of the second bottle 22. The outer diameter of the extension 232 is smaller than that of the closing portion 231, so that the second cover 23 can be easily attached to and detached from the second opening. The extension 232 has a gap, the extension 232 presenting an annular wall with partial absence in the circumferential direction. After the second cover 23 is mounted on the second opening of the second bottle 22, the position of the first area corresponding to the annular wall and the notch is changed by rotating the second cover 23, so that the extending portion 232 of the second cover 23 selectively covers the through hole 221 on the circumferential outer wall of the second bottle 22, and the extending portion 232 has a first state that at least a portion of the through hole 221 is opened and a second state that at least a portion of the through hole 221 is covered. For example, the vertical height of the extension portion 232 is equal to the vertical height of the first area, when the second cover 23 rotates to a certain position, the extension portion 232 can completely shield the through holes 221 on the first area at the corresponding position, and the problem that the through holes 221 arranged vertically cannot be shielded to affect the adjustment of the aperture ratio of the through holes 221 is avoided. The circumferential length of the extension 232 is equal to the circumferential length of the third region, i.e., the circumferential length of the extension 232 is half of the circumferential length of the first region. After the second cover 23 is mounted on the second opening, the second cover 23 is rotated to make the extending portion 232 correspond to the third area, so that the through hole 221 is completely shielded by the extending portion 232; when the second cover 23 is rotated to a position corresponding to the fourth region of the extension 232, the through-holes 221 are all opened, and the second cover 23 is rotated between the two positions, thereby achieving different opening ratios of the through-holes 221 from 0% to 100%.
Through the cooperation use of second bottle 22 and second lid 23, adjust the aperture ratio of the through-hole 221 of seting up on the second bottle 22 to the diffusion rate of the second solvent of effective regulation and control splendid attire in the second inner chamber, and then realize the effective control to crystal nucleus formation and growth rate, in order to obtain the single crystal that has high-quality, provide the advantage for the application of follow-up single crystal, the structure of compound is analyzed etc.. The single crystal culture device with the controllable solvent diffusion rate is beneficial to improving the growth condition of single crystals, avoids the formation of crystal agglomeration, microcrystals, crystal defects, amorphous powder and the like, and realizes the culture of high-quality single crystals.
The temperature control unit 3 is disposed outside the incubation unit 2, and for example, the temperature control unit is a heat insulating layer attached to the outer wall of the incubation container 11, and the heat insulating layer may be disposed on the entire outer wall surface of the incubation container 11 or may be wrapped around only the first bottle 21 and the second bottle 22 at a position higher than the liquid level of the second solvent. Through the heat preservation, can adjust the temperature environment in the holding inner chamber, keep the constant temperature environment among the single crystal growth process, avoid because the harmful effects of ambient temperature change to single crystal growth. The volatilization speed of the second solvent is controlled by adjusting the environmental temperature because the temperature influences the volatilization of the solvent; when the volatilization speed of the second solvent is adjusted, the adjustment of the aperture ratio of the through hole on the second bottle body is adjusted in a matching way, so that the volatilization amount of the second solvent to the accommodating inner cavity is controlled. The temperature regulation and the aperture ratio regulation have synergistic effect, so that the diffusion rate of the second solvent is fully controlled, and the formation and growth rate of crystal nuclei are effectively regulated and controlled. In addition, by controlling the temperature in the accommodating cavity, the probability of co-crystallization of the compound and the solvent can be reduced, the purity of the grown single crystal can be improved, and the growth quality of the single crystal can be further improved.
As a first alternative embodiment of the present embodiment, the circumferential length of the first region where the through holes 221 of the second bottle 22 are located may also be smaller than the circumferential length of all the first regions, or larger than the circumferential length of all the first regions, as long as the through holes 221 are opened at the positions of the first regions, so that the second solvent can diffuse through the through holes. As a modification, the circumferential length of the extension 232 may be smaller than the circumferential length of the first region where the through hole is located, or larger than the circumferential length of the first region where the through hole is located, as long as the circumferential length of the extension 232 is smaller than the circumferential length of the first region, and the extension can have a first state where at least part of the through hole 221 is opened and a second state where at least part of the through hole 221 is blocked by changing the position of the second cover 23. As a further variation, the through holes 221 may be arranged in other manners, such as in a cluster, or irregularly, and the like, and only under the cooperation of the second bottle 22 and the second cover 23, the through holes 221 may be selectively blocked to adjust the aperture ratio of the through holes 221.
As a second alternative of this embodiment, the notch opening of the extension 232 of the second cover 23 may also be provided inside the annular wall. For example, the annular wall may be rectangular in transverse extent, with the gap corresponding to a missing portion of the interior of the rectangular annular wall. After the first cover 23 is attached to the second opening, the first state and the second state of the extension 232 may be achieved by leaving the extension 232 in an incomplete state to cover the through hole 221 or leaving the through hole 221 completely open.
As a third alternative embodiment of this embodiment, the second bottle 22 and the second cover 23 may have other shapes, for example, if the second bottle 22 is a polyhedron, and the second cover 23 has a shape corresponding to the second bottle 22, it is only necessary to ensure that a through hole is formed on the outer peripheral wall surface of the second bottle 22, and after the second cover 23 is mounted on the second bottle 22, the extending portion can have the first state and the second state by changing the relative position of the second cover 23. As a variant, the first body 21 may also have other shapes, for example a cylindrical body or the like. As a modification, the culture vessel 11 may also be a vessel of other shape, for example, a rectangular parallelepiped, a cube, or the like. As a further modification, the sealing cover may be another sealing member 12 adapted to be mounted on the third opening, for example, an elastic plug body, etc., as long as the sealing member 12 is mounted on the third opening, and then the accommodating cavity is formed into a sealing cavity.
As a fourth alternative embodiment of the present embodiment, the supporting plate may also be a supporting unit 4 with other shapes and structures. For example, the support unit 4 includes a horizontal plate parallel to the bottom of the culture vessel 11, and vertical plates are attached to opposite ends of the horizontal plate, and one ends of the vertical plates remote from the horizontal plate are provided on the bottom wall surface of the culture vessel 11 by fixing pieces or the like. By starting the first mounting hole 41 and the second mounting hole 42 on the horizontal plate, the first vial 21 and the second vial 22 can be similarly carried. As a modification, the supporting unit 4 may not be disposed in the accommodating chamber, and the first flask 21 and the second flask 22 may be directly placed on the bottom wall surface of the culture container 11, and the second solvent in the second flask 22 may be volatilized to enter the first flask 21, thereby culturing the single crystal.
As a fifth alternative embodiment of this embodiment, the temperature control unit 3 may also be an incubator, and the accommodating unit 1 is placed in the incubator to control the temperature in the accommodating cavity. As a modification, the temperature control unit 3 may not be provided.
Example 2
This example provides a single crystal growing method, for example, the target material to grow single crystal is red light host material NPAFN, and the chemical structure of NPAFN is as follows:
the single crystal growth apparatus according to any one of embodiments 1, wherein the method comprises the steps of:
s1, adding a second solvent (such as n-hexane) into the second bottle 22, wherein the liquid level of the second solvent is lower than that of the first area;
s2, mounting the second cover 23 on the second opening of the second bottle 22, wherein the extension 232 of the second cover 22 blocks part of the through holes in the first area, and the remaining part of the through holes are open, and recording the opening ratio of the through holes;
s3, taking about 5mg of the target material with a clean spoon, adding about 3ml of the first solvent (such as dichloromethane) into the test tube, and performing ultrasonic treatment to dissolve the target material sufficiently;
after the target material is completely dissolved, continuously adding a small amount of material and performing ultrasonic treatment until the material is cultured to form a supersaturated solution, and adding the supersaturated solution of the target material into the first bottle body 21; wherein the amount of the second solvent added in the second bottle 22 is about 5 times (volume) the amount of the supersaturated solution added in the first bottle 21;
s4, sealing the accommodating unit 1 to form an enclosed inner cavity; the temperature in the accommodating inner cavity is set to be 20 ℃ by utilizing the temperature control unit (3), and standing culture is carried out until the target material grows into a single crystal.
S5, judging the quality of the grown single crystal, and finishing the culture if the quality of the single crystal reaches the target quality;
if the quality of the single crystal is lower than the target quality, the process returns to the step of S2, the opening rate of the through hole is adjusted, and the temperature in the accommodating cavity is selectively adjusted, and then the steps of S3 and S4 are continued.
S6, repeating the step S5 until the quality of the single crystal reaches the target quality.
By utilizing the single crystal culture device, the solvent diffusion rate of the single crystal cultured by the diffusion method can be effectively regulated, so that the crystal nucleus formation rate and the growth rate can be effectively controlled, and the single crystal with high quality can be obtained by culture. The optimal aperture ratio suitable for growing the single crystal can be obtained by recording the growth quality of the single crystal corresponding to the aperture ratio of different through holes, and the optimal diffusion rate of the second solvent suitable for growing the single crystal is obtained by adjusting the aperture ratio and matching with temperature adjustment. By using the above culture method, compounds with unknown single crystal culture conditions can be experimentally screened to obtain the optimal experimental conditions suitable for growing single crystals of the compounds.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications can be made without departing from the scope of the invention.
Claims (9)
1. A single crystal growing apparatus comprising:
the accommodating unit (1) is provided with an accommodating inner cavity;
the culture unit (2) is arranged in the accommodating inner cavity and comprises a first bottle body (21), a second bottle body (22) and a second cover body (23);
the first bottle body (21) is provided with a first inner cavity and a first opening which is communicated with the first inner cavity and the containing inner cavity;
the second bottle body (22) is provided with a second inner cavity and a second opening which is communicated with the second inner cavity and the containing inner cavity; the peripheral wall surface of the second bottle body (22) is provided with a first area and a second area which extend along the vertical direction, the first area is positioned above the second area, and a part of the peripheral wall surface of the first area is provided with through holes (221) with required quantity;
the second cover body (23) comprises a closed part (231) and an extending part (232) which is formed on the closed part (231) and extends along the vertical direction; the extension part (232) is mounted on the second opening at the second cover body (23), is attached to the inner side wall surface of the second bottle body (22), and has a first state in which at least a part of the through hole (221) is opened and a second state in which at least a part of the through hole (221) is blocked.
2. The single crystal growing apparatus of claim 1, further comprising:
the temperature control unit (3) is arranged outside the accommodating unit (1), and the temperature control unit (3) is used for adjusting the temperature in the accommodating inner cavity.
3. The single crystal growth apparatus according to claim 2, wherein the temperature control unit (3) is a heat insulating layer provided on the outer side wall surface of the housing unit (1).
4. Single crystal growing device according to claim 1, characterized in that said containing unit (1) comprises:
a culture container (11), wherein the culture container (11) is provided with the accommodating inner cavity and a third opening for communicating the accommodating inner cavity with the outside;
a sealing element (12) which is suitable for being arranged at the third opening to enable the containing inner cavity to form a sealed cavity,
the supporting unit (4) is arranged in the accommodating inner cavity, and at least two mounting holes suitable for mounting the first bottle body (21) and the second bottle body (22) are formed in the supporting unit (4).
5. Single crystal growing device according to claim 4, characterized in that said supporting unit (4) is a supporting plate laterally embedded in said growing container (11).
6. The single crystal growth apparatus according to claim 1, characterized in that the extension (232) is an annular wall having a notch in the circumferential direction, the notch corresponding to the first region where the through hole (221) is located.
7. Single crystal growing device according to claim 6, characterized in that the vertical height of said extension (232) is greater than or equal to the vertical height of said first region.
8. The single crystal growth apparatus according to claim 1, wherein the first region in which the through-hole (221) is located has a circumferential length half of the entire circumferential length of the first region, and the extension portion (232) has a circumferential length equal to the circumferential length of the first region in which the through-hole (221) is located.
9. A single crystal growing device according to claim 1, characterized in that the outer diameter of the closing part (231) is larger than the outer diameter of the extension part (232).
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| CN109652854A (en) * | 2018-12-29 | 2019-04-19 | 宁波卢米蓝新材料有限公司 | A kind of single crystal cultivation device and monocrystal cultivation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109652854A (en) * | 2018-12-29 | 2019-04-19 | 宁波卢米蓝新材料有限公司 | A kind of single crystal cultivation device and monocrystal cultivation method |
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